United States
  Environmental Protection
  Agency
Office of Air Quality
Planning and Standards
Research Triangle Park. NC27711
EPA - 454/R-00-008
March 2000
   Air
 &EPA
Final Report of Lime Manufacturing Industry
Fourier Transform Infrared Spectroscopy
Austin White Lime Company
Austin, Texas

-------
Lime  Kiln  Source Characterization
                 Final Report
                 Contract No. 68-D7-0001
                  Work Assignment 2-03
                Austin White Lime Company
                     Austin, 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

-------
                                Table of Contents
                                                                              Page
1.0    INTRODUCTION	1-1
      1.1     Objectives  	1-1
      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
      1.4     Test Report	1-4

2.0    SUMMARY OF RESULTS  	2-1
      2.1     Emissions Test Log 	2-1
      2.2     FTIR Results 	2-2
             2.2.1   Overview  	2-2
             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 Fourier
             Transform Infrared Spectroscopy (FTIR)  	3-1
             3.1.1   FTIR Sampling Equipment  	3-1
             3.1.2  Preparation for Sampling	3-5
             3.1.3  Sampling and Analysis	3-7
             3.1.4  FTIR Method Data Review Procedures	3-10
             3.1.5  FTIR QA/QC Procedures	3-13

4.0    QUALITY ASSURANCE/QUALITY CONTROL	4-1
      4.1     FTIR Analytical Quality Control	4-1

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
K \0091-02\002\003\WHITELIM\WHTL1ME RPT
                                         11

-------
                                   List of Figures

                                                                                 Page

2-1.  HC1 Inlet Run - Austin White Baghouse - Kiln #3  	2-5

2-2.  HC1 Outlet Run - Austin White Baghouse - Kiln #3	2-6

2-3.  HC1 Inlet Run - Austin White Wet Scrubber - Kiln #2	2-7

2-4.  HC1 Outlet Run - Austin White Wet Scrubber - Kiln #2	2-8

3-1.  FTIR Sampling and Measurement System 	3-3
                                    List of Tables

                                                                                  Page

 2-1.   Emissions Test Log 	2-1
 2-2.   Wet Scrubber Kiln #2, FTIR HC1 Results, ppmv 	2-4
 2-3.   Baghouse Kiln #3, FTIR HC1 Results, ppmv	2-4
 2-4   Other Species Detected by FTIR - Wet Scrubber - Kiln #2, Inlet	2-10
 2-5.   Other Species Detected by FTIR - Wet Scrubber - Kiln #2, Outlet	2-11
 2-6.   Other Species Detected by FTIR - Baghouse - Kiln #3, Inlet 	2-12
 2-7.   Other Species Detected by FTIR - Baghouse - Kiln #3, Outlet	2-13
 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.   QC Spiking Results 	4-3
 4-2.   Gas Standard Analysis Results  	4-4
 4-3.   HC1 QA Spike Run 1 Results - Baghouse	4-5
 4-4   HC1 QA Spike Run 2 Results - Baghouse	4-6
 4-5   Gas Standard Analysis	4-7
  K,V0091-02\002\003\WHITEUM\WHTLIME,RPT

-------
1.0    INTRODUCTION

       The purpose of this testing program is to: (1) 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, respectively. 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, 25A, and 322 testing. For this test, screening means a measurement to
determine approximate levels of species other than HO.

       The lime kiln facility and sampling locations tested in this program are detailed in the
report prepared by PES.

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.
K \009l.02\002\OOi\\VHITELIM\WHTLIME RPT
                                          1-1

-------
1.2    Brief Site Discussion

       Testing was conducted at the Austin White Lime Company located in Austin, Texas.
Testing was performed on the inlet and outlet on Kiln #2 and #3, wet scrubber and a baghouse,
respectively. 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 Austin White Lime Company, located in Austin, Texas.  Included in this section are
summaries of the test matrix, test schedule, and authorized deviations from the test plan.
Additional detail on these topics are provided in the sections that follow.

1.3.1  Test Matrix

       The complete sampling and analytical matrix that was performed is 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 also, in
a screening capacity, to measure other HAPs that can be detected by FTIR.

       FTER measurements were conducted in two sets:

       •      Unconditioned; and
       •      Conditioned.

       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 one-hour period to screen for
 aromatic species such as benzene, toluene, etc.
 K \OOTI.02\002\003\WHrTELIM\WHTI_IME RPT
                                           I-2

-------
       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 no less than a total of

90 minutes.  Some data points (typically, 5 minutes) 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.


7.3.3  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 20 at the outlet, then 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 one hour total sample collection
              of the conditioned samples, l/2 hour each on inlet and outlet. If detection of other
              HAPs was determined, then the run would extend to the full 2 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
              these sampling system 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.
K \0091-02\002\003\WHrrEUM\WHTLIME RPT
                                           1-3

-------
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 I provides an introduction to the testing effort and includes a brief
              description of the test site and an overview of the emissions measurements
              program;

       •      Section 2 gives a summary of the test results for the FTIR results for HCl and
              other detected species;

       •      Section 3 presents detailed descriptions of the sampling and analysis procedures;
              and;

       •      Section 4 provides details of the 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.
 K \0091 -02\002\003\WHrrELIM\WHTLIME RPT                 1-4

-------
2.0    SUMMARY OF RESULTS

       This section provides the FTIR results of the emissions test program conducted at the
Austin White Lime Company in Austin, Texas from June 30 to July 1, 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 from Kiln #2 and the Baghouse from Kiln #3.

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
6/30/98
6/30/98
6/30/98
7/0 1 /98
7/01/98
7/01/98
Location
Baghouse Kiln #3
(inlet/outlet)
Baghouse Kiln #3
(inlet/outlet)
Baghouse Kiln #3
(inlet/outlet)
Wet Scrubber Kiln #2
(inlet/outlet)
Wet Scrubber Kiln #2
(inlet/outlet)
Wet Scrubber Kiln #2
(inlet/outlet)
Run
Number
Spike 1
Run 1
Spike 2
Spike 1
Run 1
Spike 2
Test Type
FTIR HCl Spike (inlet)/
System QC (outlet)
FTIR (Unconditioned)
FTIR (Conditioned)
FTIR HCl Spike (inlet)/
System QC (outlet)
FTIR HCl Spike (inlet)/
System QC (outlet)
FTIR (Unconditioned)
FTIR (Conditioned)
FTIR HCl Spike (inlet)/
System QC (outlet)
Run Time
10:15- 11:56
12:45-16:22
17:36- 18:31
16:27- 17:21
11:51 - 13:57
14:15- 17:35
19:26-20:26
17:58- 19:04
K \0091-02\002\001\WHITEUM\WHTLIME RPT
2-1

-------
2.2    FTIR Results

2.2.1  Overview

       FTER data for HCI and other species were collected at the inlet and outlet of the wet
scrubber and baghouse. FTIR data collection of unconditioned samples was synchronized with
EPA Method 23 manual dioxin/furan testing and EPA Method 322 GFC-ER HCI measurements.
Conditioned samples were measured by FTIR for other HAP species.

       FTER data were collected by alternating sample analysis between inlet and outlet every
30 minutes for Kiln #2 and every 35 minutes for Kiln #3.  Inlet and outlet samples were drawn
on a continuous basis; only the FTER sample analysis was alternated between inlet and outlet.
The first five data points from each 30 (Kiln #2) and 35 (Kiln #3) minute inlet/outlet
measurement period were discarded to eliminate data for samples containing both inlet and outlet
sample gas. Five data points correspond to the measured response time of the complete FTER
sampling and analysis system (details on measurement of system response time are given below).
The measurement run contained a total of 74 (Kiln #2) and 79 (Kiln #3) 1-minute average data
points for both inlet and outlet measurements, after discarding the transient data points. A
 1-minute average data point is generated by analysis of a composite spectrum consisting of an
average of 43 FTER spectra collected over the 1 minute period.

       Section 2.1  gives the schedule  of the tests performed at the Austin White Lime Company
 in Austin, 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 FTER spectra collected over the 1-minute period. These results are reported in
 Section 2.2.2.2.
 K \0091-02\002tt03\WHITELIM\WHTLIME RPT
                                            2-2

-------
       The west scrubber and baghouse removal efficiency for HC1 was measured from the
inlet/outlet data from each location and is reported in Section 2.2.2.1.

2.2.2  FTIR Emission Results

       This section contains the FTIR HC1 test results for the wet scrubber and baghouse inlet
and outlet.

       2.2.2.1  FTIR HCI Test Results.  The estimated FTIR HCl detection limit for this
study was between 0.13 and 0.14 ppmv.  Approximately half the FTIR instrument analysis time
was split equally between inlet and outlet. Results given below are organized by location. HCl
removal efficiency was also calculated for each run. Raw data is presented in Appendix C listing
each compounds run values every minute.  All HCl emission runs were collected during the
unconditioned tests.

       Wet Scrubber - Kiln #2, Outlet/Inlet HCl Results—Table 2-2 gives a summary of
the wet scrubber outlet/inlet FTIR HCl results.  Appendix C provides 1-minute averages for all
target species.  The measured HCl removal efficiency due to the baghouse was not statistically
significant, 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.

       Baghouse - Kiln  #3, Outlet/Inlet HCl Results—Table 2-3 gives a summary of the
Baghouse outlet/inlet FTIR HCl results.  The measured HCl removal efficiency due to the
Baghouse was 71.0 percent, assuming that the  sample gas composition to the inlet of the scrubber
did not change significantly during the outlet testing. Figures 2-3 and 2-4 show a real-time graph
for the  inlet and outlet runs, respectively.
K \OOTI-02\002\OOWVHITELIM\WHTLIME RPT                2-3

-------
                               Table 2-2. Wet Scrubber
                            Kiln #2, FTIR HCI Results, ppmv

Date
Time
Location
Average
SD
Maximum
Minimum
NDP
RE
Runl
7/01/98
14:15 - 17:35
Inlet
3.30
2.14
9.53
0.83
74
Outlet
5.19
4.23
17.07
0.90
89
NC
SD    =      Standard Deviation
NDP   =      Number of data points measured
RE    =      Removal Efficiency in percent: 100 X (Avg. inlet-Avg. outlet)/Avg. inlet
NC    =      Not Calculated due to the outlet being greater than the inlet value, however inlet and outlet
              levels are statistically equivalent, due to the level of standard deviation.
Note:   =      Raw data presented in Appendix C.
                                  Table 2-3.  Baghouse
                            Kiln #3, FTIR HCI Results, ppmv

Date
Time
Location
Average
SD
Maximum
Minimum
NDP
RE
Run 1
6/30/98
12:45 - 16:22
Inlet
1.76
3.97
15.08
<0.15
80
Outlet
0.51
1.27
6.86
<0.15
110
71.0
 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.
 K \0091.02\002\Q01\WHITEUM\WHTUME RPT
                                            2-4

-------
   12.00
                         Figure 2-1. HCI Inlet Run - Austin White Wet Scrubber - Kiln #2
   10.00
    8.00
   6.00
   4.00
I
o

o
O
   2.00
   0.00
                                                         Time

-------
                     Figure 2-2.  HCI Outlet Run - Austin White Wet Scrubber - Kiln #2
18.00
16.00
 0.00 r—i—i i i i i  i i i i i i i i—i i i i i i i i i i—i i i  i i i i i i i—i
                                                    Time

-------
                           Figure 2-3. HCI Inlet Run - Austin White Baghouse - Kiln #3
   16.00
   14.00
   12.00
_ 10.00

g; 8.00

o
o
0  6.00
   0.00 I i  i i i i  i i i  i—i i i—i i i  i i—i
                                                          Time

-------
                                 Figure 2-4. HCI Outlet Run - Austin White Baghouse - Kiln #3
     8.00
     7.00
     6.00
  ^ 5.00
  •**
   o






^ g. 4.00
oo o.
   o


   O
   O
     3.00
     2.00
     1.00
     0.00
          co co  o>  CM  m  oo
          in m  in  o  o  o
                              i-  -  CM  m
O  T-  T-
                                                                                                                             CO
                                                                    Time

-------
       2.2.2.2  Other Species Detected by FTIR. Other species were detected during the
unconditioned and conditioned FTIR test runs.  Species in Table 2-4 thorugh 2-7 indicated with a
"U" were measured concurrently with HC1. Species in Table 2-4 through 2-7 indicated with a
"C" were measured during the conditioned sample test run. Results given below were are
organized by location.

       Wet Scrubber - Kiln #2, Outlet/Inlet for Other Species Results—Table 2-4 and
2-5 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.

       Baghouse - Kiln #3, Outlet/Inlet for Other Species Results—Table 2-6 and 2-7
respectively gives the summary of the baghouse for the inlet and outlet FTIR results for other
species found during the standard Draft Method 320 extractive analysis.
 K \009I-02M302\003\WHITEUM\WHTLIME RPT
                                          2-9

-------
                                Table 2-4. Other Species Detected by FTIR - Wet Scrubber - Kiln #2, Inlet

                                                 (all values are ppmv, except CO2 and H2O in percent)
Parameter
U/C
Average
Std. Dev.
Max.
Min.
NDP
EDL
C.H,
C
0.89
0.07
1.09
0.76
25
0.16
C2H4
C
2.68
0.12
2.85
2.27
25
0.11
C3HA
C
1.66
0.24
2.07
1.05
25
0.32
C02
u
13.3
1.65
16.0
11.7
89
0.057
NH,
U
2.17
2.22
7.04
<0.32
89
0.32
CO
U
131
5.79
141
119
89
0.66
NO
U
133
14.4
159
104
89
7.6
H2CO
U
2.03
0.13
2.39
1.66
89
0.10
C *
*~4
U
1.73
0.11
1.91
1.46
89
0.30
H2O
U
21.5
2.46
25.6
19.3
89
0.13
to
o
U/C - Unconditioned (U) or Conditioned (C) Sample
C4+ - Total aliphatic hydrocarbons larger than 3 carbons (ppmv hexane equivalent)
NDP - Number of data points; the total number for the inlet was 7 5-minute intervals, not the standard 1-minute intervals used during the unconditioned sampling.
EDL - Estimated detection limit for spectral region used for analysis
Stcl. Dev. - Standard Deviation
Max. - Maximum
Min. = Minimum
Note:  Raw data presented  in Appendix C.
        K V009I-02VD02VXH\WHm-l.lM\WHTLIMt RPT

-------
                            Table 2-5.  Other Species Detected by FTIR - Wet Scrubber - Kiln #2, Outlet

                                          (All values are ppmv, except CO2 and H2O in percent)
Parameter
U/C
Average
Std. Dev.
Max.
Min.
NDP
EDL
C6H6
C
0.44
0.09
0.63
0.31
25
0.16
C2H4
C
1.64
0.07
1.82
1.46
25
0.11
C3H6
C
0.94
0.22
1.43
0.56
25
0.32
CO2
u
12.4
1.31
14.3
11.0
89
0.085
CO
u
66.1
2.78
71.0
62.2
89
0.79
NO
U
125
15.7
152
95.3
89
7.2
NH3
U
0.59
1.05
4.72
<0.47
89
0.47
H2O
U
35.1
3.73
39.6
30.7
89
0.22
N>
       U/C - Unconditioned (U) or Conditioned (C) Sample
       NDP - Number of data points; the total number for the inlet was 7 5-minute intervals, not the standard 1-minute intervals used during
       the unconditioned sampling.
       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.
       KVKWI 02V002W)nWHITi;i.lM\Wini.lMliRI'l

-------
                                   Table 2-6. Other Species Detected by FTIR - Baghouse - Kiln #3, Inlet

                                                (All values are ppmv, except CO2 and H2O in percent)
Parameter
U/C
Average
Std. Dev.
Max.
Min.
NDP
EDL
C.H4
C
0.77
0.07
0.94
0.65
20
0.14
C2H4
C
2.05
0.11
2.22
1.79
20
0.12
QH2
C
023
0.03
0.27
0.16
20
0.07
CO,
u
14.8
1.85
15.8
5.86
80
0.0657
NH3
U
7.40
5.28
13.4
<0.36
80
0.36
CO
U
<9.36
0.02
0.21
< 9.36
80
9.36
NO
U
243
66.6
400
114
80
2.52
H,CO
U
118
20.5
148
42.8
80
8.64
C 4
*-4
U
1.54
0.31
1.87
< 0.96
80
0.96
H2O
U
4.23
0.54
4.88
<2.06
80
2.06
to
        U/C - Unconditioned (U) or Conditioned (C) Sample
        C,+ - Total aliphatic hydrocarbons larger than 3 carbons (ppmv hcxane equivalent)
        NDP - Number of data points; the total number for the inlet was 7 5-minutc intervals, not the standard I-minute intervals used during the unconditioned sampling.
        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.
        K \009I-02V002WOWVHI IL1JMWHTIIMI KIT

-------
                          Table 2-7. Other Species Detected by FTIR - Baghouse - Kiln #3, Outlet

                                         All values are ppmv, except CO2 and H,O in percent
Parameter
U/C
Average
Std. Dev.
Max.
Min.
NDP
EDL
C6H4
C
0.72
0.12
0.97
0.48
25
0.14
C2H4
C
1.69
0.28
2.04
1.08
25
0.12
C2H2
C
0.22
0.04
0.26
0.13
25
0.07
CO,
u
<0.59
0.13
0.64
<0.59
25
0.59
CO
u
<0.36
0.17
0.67
<0.36
25
0.36
NO
U
3.37
040
4.26
2.77
25
0.64
NH,
U
1.06
0.18
1.55
0.77
25
0.51
H2CO
U
148
1.86
16.1
5.48
110
0.0658
C *
*-4
U
<9.36
4.72
34.4
<9.36
no
9.36
H2O
U
218
97.4
468
52.6
110
2.52
U/C - Unconditioned (U) or Conditioned (C) Sample
C4+ - Total aliphatic hydrocarbons larger than 3 carbons (ppmv hexane equivalent)
NDP - Number of data points; the total number for the inlet was 7 5-minute intervals, not the standard 1-minute intervals used during the unconditioned sampling.
EDL - Estimated detection limit for spectral region used lor analysis
Std. Dev. = Standard Deviation
Max. = Maximum
Min. = Minimum
K:\0091 -02tt02W0.1WHITr;UM\WHTI.IMB RPT

-------
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
      Fourier Transform Infrared Spectroscopy (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;

K.«09l-02\002\003\WHITELIM\WHTUMERPT               3-1

-------
       •      FTIR spectrometer;
       •      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 paniculate 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
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.
 K \0091 -02\002W).i\WHrrEUM\WHTUME RPT
                                           3-2

-------
                                         Heat-traced line
     Sample
     Gas In
                     Spike or QA/QC Gas
-L
                                                                Vaporization
                                                                  block
               Main Sample Pump
                                                        QA/QC Gas Standard Manifold
                                       Heat-traced line
                                       (up to 100 feet)
                                                                      QA/QC Gas Standards
                                                                                               Spiking Solution
OJ
              Heated Flow Meter
               Legend
         Bold text and lines = Heated

       Normal text and lines = Unheated
          Sample Distribution Manifold
FTIR
Sample
Pump/
Flowmeter
                 I         I         \
                   To Other Instruments
                   FTIR Sample Cell
                                                         Excess sample to
                                                         atmosphere
                                                            Exhaust to atmosphere
                                     Figure 3-1. FTIR Sampling and Measurement System

-------
       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:
 K.«09l-02\002\00.1\WHrTELIM\WHTLIME.RPT               3-4

-------
              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 frequency calibration. Carbon monoxide is
              directly injected into the sample cell to measure photometric accuracy, validity of
              the non-linear 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



K \009I-02\002\003\WHITELIM\WHTLIMERPT                3-5

-------
      •      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
 K WWI-02>002\00:i\WHITELIM\WHTUME RPT
                                          3-6

-------
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

K:\009I-02\002\OCH\WH1TELIM\WHTLIME RPT                 3-7

-------
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 FTER 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
5 minute cell purge and 25
minute sample collection
2 minute cell purge and 28
minute sample collection
Outlet
5 minute cell purge and 15
or 25 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 three-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
 K «09l-02\002V003\WHrrELIM\WHTLIME RPT
                                            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.
K ro9!.02\002\00.1\WHITEL!M\WHTLIME RPT                3-9

-------
            Table 3-2. Compounds for Which Reference FTIR Spectra Are
                        Available in the ERG Spectral Library"
1-butene
1,3-butadiene
2-methylpropane
2-propanol
2-methoxyethanol
2-methyl-2-propanol
2-methylbutane
4-vinylcyclohexane
acetaldehyde
acetic acid
acetone
acetylene
acrolein
ammonia
benzene
carbon monoxide
carbon dioxide
carbonyl sulfide
chlorobenzene
c/.s-2-butene
cyclohexane
cyclopentane
cyclopropane
ethane
ethylbenzene
ethylene
formaldehyde
hydrogen fluoride
hydrogen chloride
isobutylene
m-xylene
/rz-cresol
methane
methanol
methyl ethyl ketone
methylene chloride
n-butanol
/i-butane
n-pentane
nitric oxide
nitrogen dioxide
nitrous oxide
o-cresol
o-xylene
p-cresol
p-xylene
phenol
propane
propylene
styrene
sulfur dioxide
toluene
rrart.y-2-butene
water vapor
 Spectra were collected at a cell temperature of 185° C.
K \009I-02\002\OOWVHITELIMWHTLIME RPT
                                         3-10

-------
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 m  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.\DOT|.02V002\003\WHITEUM\WHTLIMERPT                3-1 1

-------
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 \009l.02\002\003\WHrrEUMWHTLIME RPT
                                            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 pa;.rs 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.
K W}(»-02\00:\OOWVHITELIM\WHTLIME RPT
                                           3-13

-------
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 course of 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 FTER 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 «»1-02VX)2\00.1\WHITELIM\WHTLIME RPT               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;
       •      Direct measurement of a CO gas standard;
       •      Direct measurement of a methane (CH4), nitrous oxide (NO:), and carbon
              dioxides (CO2) standard; and
       •      Pathlength calibration using halocarbon 22 (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. Table 4-1
through 4-4 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 HC1, 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 HC1 standard was obtained at a
 ±5 percent analytical tolerance, the acceptance criteria was set at ±10 percent.  FTIR NOX is
 measured as NO + NO:. Examination of Table 4-5 shows that all QC checks met the above
 criteria.
 K \009I -OiWCmiWHITELIMWHTUME RPT
                                           4-2

-------
              Table 4-1.  HCI QA Spike Run 1 Results - Wet Scrubber
                             Austin White Lime Company
Outlet
Spike Run
Number
I
2
3
4
5
6
Average
Lowest
Unspiked
Value (ppmv)
6.54
6.4 1
6.37
6.40
6.60
6.94
6.54
Spiked
(ppmv)
153.63
164.74
167.84
176.16
214.76
172.64
174.96
Corrected
Difference
(ppmv)
147.74
158.97
162.11
170.40
208.82
166.39
169.07
Spike
Level
(ppmv)
149.00
149.00
149.00
149.00
149.00
149.00
149.00
% Recovery
WMMi.





113.47
SF6
Cone.
(ppmv)
0.048
0.048
0.048
0.048
0.048
0.048
0.048
Dilution
Ratio
0.100
0.100
0.100
0.100
0.100
0.100
0.100
Inlet
Spike
Run
Number
I
2
3
4
5
6
Average
Lowest
Unspiked
Value (ppmv)
64.44
58.23
53.16
48.44
54.97
71.11
58.39
Spiked
(ppmv)
180.38
183.70
185.71
188.18
229.33
164.38
188.61
Corrected
Difference
(ppmv)
121.42
130.42
137.07
143.86
179.03
99.31
135.18
Spike
Level
(ppmv)
126.65
126.65
126.65
126.65
126.65
126.65
126.65
%
Recovery
'WMKs





106.74
SF6
Cone.
(ppmv)
0.041
0.041
0.041
0.041
0.041
0.041
0.041
Dilution
Ratio
0.085
0.085
0.085
0.085
0.085
0.085
0.085
NOTE:  The spike runs were conducted before and after the test runs, therefore the minimum and
maximum values listed here may be different than 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 \0091-O:\002\00.1\WHITELIM\WHTL1ME RPT
                                            4-3

-------
              Table 4-2. HCI QA Spike Run 2 Results - Wet Scrubber
                             Austin White Lime Company

Spike Run
Number
1
2
3
4
5
6
Average

Spike
Run
Number
1
2
3
4
5
6
Average

Lowest
Unspiked
Value (ppmv)
3.15
3.00
3.03
3.04
2.87
3.38
3.08

Lowest
Unspiked
Value (ppmv)
163.62
164.47
144.88
145.78
140.24
150.37
151.61

Spiked
(ppmv)
140.24
150.37
154.83
159.17
164.67
165.42
155.78

Spiked
(ppmv)
203.47
207.26
223.18
223.95
170.32
169.33
199.59
Outlet
Corrected
Difference
(ppmv)
137.41
147.67
152.10
156.43
162.09
162.38
153.01
Inlet
Corrected
Difference
(ppmv)
46.11
49.37
84.10
84.00
35.69
24.97
54.04

Spike
Level
(ppmv)
148.00
148.00
148.00
148.00
148.00
148.00
148.00

Spike
Level
(ppmv)
59.20
59.20
59.20
59.20
59.20
59.20
59.20

% Recovery
'9%^



WK^/

103.39

%
Recovery
W^&





91.28

SF6
Cone.
(ppmv)
0.209
0.209
0.209
0.209
0.209
0.209
0.209

SF6
Cone.
(ppmv)
0.084
0.084
0.084
0.084
0.084
0.084
0.084

Dilution
Ratio
0.100
0.100
0.100
0.100
0.100
0.100
0.100

Dilution
Ratio
0.040
0.040
0.040
0.040
0.040
0.040
0.040
NOTE:  The spike runs were conducted before and after the test runs, therefore the minimum and
maximum values listed here may be different than 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 \Q09I-02\002\OO.WHITELIM\WHTLIME RPT
                                            4-4

-------
                Table 4-3. HCI QA Spike Run 1 Results - Baghouse
                             Austin White Lime Company
Outlet
Spike Run
Number
I
2
3
4
5
6
Average
Lowest
Unspiked
Value (ppmv)
6.53
6.56
6.32
5.88
5.55
5.27
6.02
Spiked
(ppmv)
35.90
39.89
42.64
43.45
45.12
45.70
42.12
Corrected
Difference
(ppmv)
29.75
33.72
36.69
37.92
39.90
40.74
36.45
Spike
Level
(ppmv)
30.41
30.41
30.41
30.41
30.41
30.41
30.41
% Recovery
WM9,.





119.86
SF6
Cone.
(ppmv)
0.300
0.340
0.350
0.360
0.370
0.370
0.348
Dilution
Ratio
0.059
0.059
0.059
0.059
0.059
0.059
0.059
Inlet
Spike
Run
Number
I
2
3
4
5
6
Average
Lowest
Unspiked
Value (ppmv)
9.56
9.07
9.29
8.50
7.88
7.29
8.60
Spiked
(ppmv)
14.46
15.63
17.93
19.60
20.95
21.02
18.27
Corrected
Difference
(ppmv)
6.96
8.51
10.64
12.93
14.77
15.30
11.52
Spike
Level
(ppmv)
11.69
11.69
11.69
11.69
11.69
11.69
11.69
%
Recovery
'WM^/s





98.52
SF6
Cone.
(ppmv)
0.450
0.450
0.440
0.440
0.430
0.430
0.440
Dilution
Ratio
0.215
0.215
0.215
0.215
0.215
0.215
0.215
NOTE:  The spike runs were conducted before and after the test runs, therefore the minimum and
maximum values listed here may be different than 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
    -02<002\00.1\WHrrEUM\WHTUME RPT
                                           4-5

-------
                Table 4-4. HCI QA Spike Run 2 Results - Baghouse
                             Austin White Lime Company

Spike Run
Number
1
2
3
4
5
6
Average

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

Lowest
Unspiked
Value (ppmv)
17.50
18.79
19.81
20.59
21.24
21.12
19.84

Spiked
(ppmv)
17.34
17.97
18.06
18.25
18.31
18.59
18.09

Spiked
(ppmv)
40.32
43.54
45.06
46.50
46.98
48.13
45.09
Outlet
Corrected
Difference
(ppmv)
13.37
13.97
14.10
14.14
14.53
14.16
14.04
Inlet
Corrected
Difference
(ppmv)
24.58
26.64
27.24
27.98
27.87
29.13
27.24

Spike
Level
(ppmv)
15.94
15.94
15.94
15.94
15.94
15.94
15.94

Spike
Level
(ppmv)
25.40
25.40
25.40
25.40
25.40
25.40
25.40

% Recovery
WMX.





88.12

%
Recovery

WMS',




107.24

SF6
Cone.
(ppmv)
0.320
0.320
0.320
0.310
0.310
0.310
0.315

SF6
Cone.
(ppmv)
0.510
0.510
0.520
0.520
0.520
0.520
0.517

Dilution
Ratio
0.063
0.063
0.063
0.063
0.063
0.063
0.063

Dilution
Ratio
0.100
0.100
0.100
0.100
0.100
0.100
0.100
NOTE:  The spike runs were conducted before and after the test runs, therefore the minimum and
maximum values listed here may be different than 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 \0091-02\002\CXWWHrTELIM\WHTLIME RPT
                                            4-6

-------
                      Table 4-5. Gas Standard Analysis Results

Date
6/30/98





6/30/98





7/01/98





7/01/98






Time
08:35 AM





06:36 PM





08:28 AM





08:33 PM






Compound
HC1
CO
CH4
NO
C02
H22
HC1
CO
CH4
NO
CO,
H22
HC1
CO
CH4
NO
CO:

HC1
CO
CH4
NO
CO,
H22
True
(ppm)*
253
102.3
491
503
4.99 %

253
102.3
491
503
4.99 %

253
102.3
491
503
4.99 %
3.40m
253
102.3
491
503
4.99 %

Result
(ppm)*
248.2
102.3
489.4
501.9
4.95 %
3.40m
245.4
102.4
491.2
503.2
4.97 %
3.38m
251.1
100.2
490.4
505.4
5.07 %
3.41 m
249.1
100.4
493.3
493.2
4.99 %
3.28m
%
Recovery
98.1
100
99.7
99.8
99.2

97.0
100.1
100
100
99.6

99.2
100.2
99.9
100.5
101.6

98.4
98.1
100.5
98.0
100

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 NO, and CO2 Gas Standard Accuracy; ±1 percent; Acceptance Criteria: ±6 percent of target.
* All compounds are recorded in ppm except for CO, in percent (%), and H22 in meters (m).
The Halocarbon 22 (H22) is used to calibrate the pathlength.
K \009l-02\002\001\WHrTELIM\WHTLIME RPT
                                          4-7

-------
                        APPENDIX A

            FTIR DATA SPREADSHEET CALCULATION
                       QA/QC SHEETS
K \0091-02V002V003WHITELIM\WHTLIME RPT

-------
                                  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)
                                       0/acr
                                                                               TIME:
Run Description
Reviewer:
                                                                               Date:
         entnes match, referencesvafut
         ''---s^
                             e
1.  Pollutants matches pollutants in both the
   original and QA/QC data     	 	
                                        I/
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.  Verily that the QA/QC value is zero. This
   indicated that both the original and the
   QA/QC values are identical.
  ^Check that calculations are cor
                                        l/
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
 Facilit  Name:
                                              DATE:
 Source Location (INLET or OUTLET
ET)   ,
TIME:
 Run Description
Reviewer:

          entries match references valu
      jrSJir-*-- «*~- «-!*«'i •''•-.-i- -^i*1*-'
      me following by comparing tficprm
1.  Pollutants matches pollutants in both the
   original and QA/QC data
I.  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.
!. No mathematical errors
    fo 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:

             I.  Excel QA/QC workbook

             2.  Inlet and Outlet QA/QC information
Facilit  Name:
UU*.
                                      DATE:
Source Location (INLET or OUTLET!
'•amgf^g-ofttfT
                                              TIME:
Run Description
                                M
Reviewer:
                                              Date:
   )A/QC entries match references valui
   K>«^»^;i-.i---.->i^'V—-••-<• -•"--'.•"••'•%j*j»*v '•
    : the following by comparing thepnnf
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.
   Check that calculations are co
!. 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
 Reviewer:
                                                                                Date:
    A/QC entriesjnafch references values?
                 '' •- t'.vS'«v»iV'4
                   comparmg the.
1.  Pollutants matches pollutants in both the
   original and QA/QC data
                                         t/
2.  Times for Inlet/Outlet samples match.
                                         v/
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.
t. 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
 Facility Name:
i   ,/  *\
LAMK
DATE:
 Source Location (INLET or OUTLET)
                  ^^
                                                   TIME:
 Run Description
 Review
                                                   Date:
   iecklist

£&QA/QC entries match, references values
^W*f«<^>«l->'ti?5^i'*'-i'-tJ"/-'< ••^'•"••i./'^-V'Wajn'i. i»-'
      me iollowmg by comparing the prmtourof tne
 I.  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.
 !. 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:

               I.   Excel QA/QC workbook

              2.   Inlet and Outlet QA/QC information
FadlityName:
                                        DATE:
Source Location (INLET or OUTLET)
                                        TIME:
Reviwer:
                                        Date:
 1. Pollutants matches pollutants in both the
   original and QA/QC data
J
2. Times for Inlet/Outlet samples match.
I/
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.	
   ChecK that calculations'are co
   M'M.* » +^Jrt--\*M ~ '—-'•	J^.*	-^.-- -^.->—
 i.  No mathematical errors
2. No errors in the data macro

                  l\>^Mc   is

-------
                         APPENDIX B




             GAS CYLINDER CERTIFICATION SHEETS
K «09l-02\002\OOWVHITELiM\WHTL!ME RPT

-------
                                                                       REC'O AUG 141998
                SPECTRR GHSES
          ^^J 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
     COMPONENT
                                                  ANALYTICAL ACCURACY: + / - 5%
                  REQUESTED GAS
                      CONC
                                                                           ANALYSIS
 Hydrogen Chloride
 Sulfur Hexafluoride
                      50 0 ppm
                      2.00 ppm
54.3 ppm
2.01 ppm
 Nitrogen
                      Balance
                                                                             Balance
Sulfur Hexafluoride is +/- 2%
ANALYST:
                 Tefd Neeme
                                           DATE:
                                                                            8/10/98
                            USA • United Kingdom • Germany • Japan
                                       130  3003

-------
              SPECTBfl 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
                                     isa  a a a s

-------
              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
Morrisville, 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:
                                                +/- 2%
    COMPONENT
  Hydrogen Chloride-
  Sulfur Hexafluoride
                  REQUESTED GAS
                      CONC
                     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 Kingdom • Germany • Japan

-------
                                                                       1^1998
              SPECTRfl GflSES

              277 Coit Street • Irvington, NJ 07111 USA  Tel: (973) 372-2060 • (800) 929-2427 • Fax: (973) 372-855 •

 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
                   CONC

                  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
               Mike Deyle
                          USA • United Kingdom • Germany • Japan
                                    ISO 9002

-------
                SPECTRfl  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 # :
ITEM# :
CERTIFICATION DATE:
P.O.*:
BLEND TYPE:
                     134942
                     2
                     8/10/98
                     9101008011-R132
                     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:
                                                                 DATE:      8/10/98
                 Ted Neeme
                            USA • United Kinnrlnm • ftarmanu • .lanan

-------
              SPECTRfl GflSES

              277 Coit Street • Irvington, NJ 07111 USA   Tel: (973) 372-2060 • (800) 929-2427 • Fax: (973) 372-855<

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
ITEMS:             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
                   CONC

                   500 ppm
                   5.00 ppm

                   Balance
                                                                    ANALYSIS
516 ppm
5.09 ppm

Balance
* Analytical Accuracy of Hydrogen Chloride is +/- 5%
ANALYST:
                                         DATE:     5/11/98
                          USA • United Kingdom • Germany • Japan
                                    iso  s o a a

-------
                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
 Momsville , NC 27560
                                        CERTIFICATE
                                             OF
                                         ANALYSIS
 SGI ORDER # :        134942
 ITEM*:              3
 CERTIFICATION DATE:  8/10/98
 P.OJ:               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 Hexafluonde
                      1,000 ppm
                      2.00 ppm
1,030 ppm
2.02 ppm
 Nitrogen
                       Balance
 Balance
Sulfur Hexafluonde is +/- 2%
ANALYST:
H-
                                             DATE:
                                                                            8/10/98
                 Ted Neeme
                            USA • United Kingdom • Germany • Japan
                                      iso  Baas

-------
          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 #:   G1
CUSTOMER:
SGI ORDER #
ITEM*:
P.O.*:
                   Eastern Research Group Inc.
                   126876
                   3
                   7904004005-R562
CERTIFICATION DATE: 8/26/97
EXPIRATION DATE:    8/26/2000
                                  CYLINDER # :
                                  CYLINDER PRES:
                                  CGA OUTLET:
                                                             CC80890
                                                             2000 PSIG
                                                             350
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
Honba-VIA-510



SERIAL *
570423011



DETECTOR
NDIR



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:
-Pol
                                                        DATE:
                                                                 8/26/97
               TED NEEME

-------
               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
Morrisville, NC 27560
                                      CERTIFICATE
                                            OF
                                        ANALYSIS
 SGI ORDER*:        128118
 ITEM*:              2
 CERTIFICATION DATE: 10/16/97
 BLEND TYPE:         CERTIFIED
                                CYLINDER #:    CC82244
                                CYLINDER PRES: 2000 psig
                                P.O.*:          7904004005-R690
                                         ANALYTICAL ACCURACY:     +/- 2%
    COMPONENT
 Chlorodifluoromethane
                  REQUESTED GAS
                      CONG
                     40.0 ppm
                                                                       ANALYSIS
40.3 ppm
       Nitrogen
                     Balance
 Balance
ANALYST:
                Ted Neeme
                                         DATE:
                                                                        10/16/97
                           USA • United Kingdom • Germany • Japan
                                     ISO 3002

-------
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, NJ. 08865
   CERTIFICATE OF ANALYSIS
                                  EPA PROTOCOL MIXTURE
                                  PROCEDURE #:  G1
   CUSTOMER:
   SGI ORDER #:
   ITEM*:
   P.O.*:
        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
Nicolet-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

-------
                             APPENDIX C




                           RAW FTIR DATA
K \009I -02\00:\OOWVHITELIM\WHTUME RPT

-------
                                        a a'lisa

                                                                                             »*s*
                                                                                             Is
                                                                                                                                                   Sf.S
                                                                                                 g C Sl2 g S 'S
                                                                                                 s sisisio s S|s oisii'siajs^aio'gJiiiijiiiiBl'g
   I
i
iSi* SiSISiaiSii
                                      38jllIS3
                                                  Ol[— *|M U> Ul .— ,W^*i W Q\ «n(,^i5l«'K>I5

                                                  S-a|al8l8.8iS,;iaigi8l«i8|aiftl8!8
   B
       ill
              35 Si
                                              X wlw SlujHiulB u 2:5 a 8 8
                                              £ 8|8|ti g|a!i|3|S g|!a S 8 8
                                                                         __,
                                                                         88 §18 • * S
                                                                                                                                                   •I—
       SS
       38
              8 8|S 8 8|S % b!
                          B
                          si
                          sja
                                lsias
                                               SiSSISiSSS
                        sltlic al
                                                                                                 ml
                                                                                                     8ISS"
                                                                                                          M
     eg
     s o
                    IMII
                    ""
                           83818
SIS t[2
                S5I55
oSSI£|S3!2|t S5S88
                                                                          site
2J5SS1*
                                                                                         = 8
                                                                                                      sass
                                                                                                                         !=ic:= Sla Sit SIS S'S S:S:S Si
                              s g 8ia s s s
                                                  3|8|8 | Sif=i§j| s g |i Slllf 21 ^s § siSTls g S S 2 § s.S.i 5 5'S S g S 3 S;§ 15 5 § g ; s g s § s|2 «
              fas
                        383-SSSBS:
                                        88|g
                                                s s is 8 s Kisisislis s g

                                                              sIS
                                                                                                                      =1=1;
                     SSt!
                                        atialsiaais
                                                                    SKS2I.SSS888
                                                           i^aisia a sis s.sia 8 s
                                                                                     8183
                                                                                                                                          .S £ S.S
                                      l»|«lvi« « •>{«

                                      SlsjS'S 2 Si's
                                                   • l<0 VlVIBj-tflu*|« «!• • 0» • t»lo» 0> « 0»
                                                   g|8 s|s|al«|sla|8|s s g s aia sis a
                                                                                                                                       l'S8i8!3;s1|
                       s       ss       lsiasssi   ii   I     lli     ii.i     i       ;::!       lji  g
                                      zas Kiciss^ic
rsa s:s:Ki=:si
   '
                                                                                             a Kis-Kisis:: =IK S:K,K.S   s s s   s:     s a,
                                                                                                                   '

                                                                                                       f,t!K'S!S:S!8!S 8 8:8 S 8^8 S 8 8 S'S 8 g 888 8 S
                                      Is s,s Ij.is!8iai.!±ili8^,s!ai^.'^^aiS!.i.!£|sJ»!.!aia!8!aia!a'a!si^                                     s s s s si
                                       :,,::!;;       —i  i i  !  , I  ,  ,  I i  !  I  ; |  ! ,  !  i  i '  !  I  ' I  I  ;  ,—i—-—,  I  . '  ,  i ,  :  ,	2_
      islg sisi
                                                                                                                                           a s s s i

                                                                                                                         ^^^.^*!*^.^ • » « « »:
                                                                                                                         '(O -«J eg  fi
                                                                                                                         — i^i<0) PO '^i -J A t/i • Ln Cn — Ot ir> X
                                                        rs s s ^ a'i::

       S,= ::;; r:S r,= S S £:SiS;5,5 ='^ = S S C 5; = 5'Z'S S S 2 E,3 5 S S : S £ S S:S S 8 S S.S.g^^ £,I = = S S:S S S I K S S:: = S^S S 55 S 5 S ii I C,S B o
  _^  —,__, —l-l —,_ —_ __ — ^(o--o - -. — o -i- ->- --.-- ~>o O'O -to'-- oo'o-ooo- -o---o   —               	
 .:B Sis^'i sis iiS'S.s'iii 5 s g;ii^= s;^i j's:a s.J:s 8 ;^!g,s,a s 3 s s i s s!s^'s I ;!s'5:3 sij:s s s i:s i ii =:$ 5 ; a|= ; 8 s^.s's'a zs-ss r.s's s a a 5 g
                                                      ..,,                   ,
                                                      ^ S 2it:S S:S S S S S,2!S S S S S'S:3:rS;S;S S-3^S S 3        S S'S S S 3 3 S 3 S-S S 5 2 I S 2:2 K S S §
                                                                                                                                  S £ So " 3> 5 »5 «
                                                                                                                                            22=1
                                                                                                                                            .--„
  B-.IOI—'—i-*i—i— — -*,-*! — '— —,—;— ^;^ — _* — —!_. —,_.—,— _.,— ~ ^,— -. —'— —I— -...
  j*,,| —j^j —j —|Ol— — Ol-*| —[•*( —t —I —| —1 — |O| — | —i—'-*|O|-*i-*iO|o O|Oj —[ — lOiO^'Oi —1 — 1*
  S8S
                                                                                                             =:8:8 S S = S'i S;S:8:8 S S,8 8 8 g g g'g 2'
         l I
                                                                                     w!» j
                                                                                     jut.w

                                                                                      I  I
                                                                                                      :S:S'i: SiSiX E S S
                                                                                                           .  .    , .
                                                                                                                            iS^^^.S S 3 ^ S:2 S S!
                                                                                                                            .  i

   i
           s s is o eieisg    s aa   sis
                                       ajsjs aisiai?!? Iili? sis|i|i|B S i Ili|I ijIls|s|I|2is!S i Sis si? g 2Sg!gtlgj8Jaja|s!g|8|8j8!aiajaigjgis
                                                                                                                           -l-,-;-i
                                                   SlS S SS
  SS88388
                siiiliiiiiili
                                   8SSSSS88S8SS833!i:
                                                              5SES!SS£ISSSS.5«33SIs!sSS5Ii3BIiSS!l5 S 5 S S|£|£|8|S!S|S
                                                                     i  i
                                                                                                                                               ;'=!,
 O = W^OOOOOOB^O^|

 8liS388l888888|gg
                         o o o o o
                         88888
                                8 8 8,8 8 8 8 8 8 8 8 8 8 j 8 8|8l8,8 88 8 8 8|8 8 8 8 8 8 8 8 8 8 8 8 8 8 8|8 8 8|8 8,8 8 8 g|s S 8,8 8 8lt!,g|g SJS 8 8i5ia!S;3iP!
                                °	I	1—t	1 I  I	1	1  I I	1	1	1	-H	1	1	I I  I	1—t	1—-I	1	1	•—!	I	   I	1	    '	1	1	'	
    25
 III I i III I,! i
                818888 818 88888 SISiSlSlSisIS 8 sIS^ISISlS SlSiilJIsIS 8 8!8l8 818 8 8,8
 82
      22
              22222222222222
                                          22122
                                                           2181212 2 2 Si
                                                                        22|22J22|22
                                                                                       122
                                                                                             222
                                                                                                        228
                                                                                                               2|2 2|2|2|2 212J2I2J2I2I2 2|2!2:2!2i2:21'§!
                                8,888
                                        8.818 8 8.81818 S 818 8|8|8|8 8,8 818 Sjglsls 8^888 818.8 8J8I8 818 8 818 818 818 8 8l8i8!8i8!8l8l8i8l8!8,8i8:8!8;8 8,S:
             i«
                     83338
                                                      B8SSI2
                                                               SISaS
                                                                                        ssst
                                                                                                ia s a K x s S|B g|s s s,s sisis tiais.s a sis:s;s s s:s:
 ISI8
         SS33
                                     8SSS
                  Si*
                                                                8BS1:
                                                                      Slu
                                                                          sssssss
                                                                                                      iSjS sislslsjajs i SiSsSiSSiSissssssislSg:
                                                                                                      i'X 8 "!«!8,tl8 8..!Sia;SISia'SiS:t!3,»'BlS'£lSiS,><
    -3SS
                      SESS88
                                  8.888
                                                                    SlS S S S 3 K S
                                                                                  -IX St

-------
 -           _;_ i  j    i .  j  i  : i    | .  i  i i     i  i  | .    |  | |  |  j |  ;jj  i  | ii    ij  |j !  i  M i  i

'•II j'lis aiiii*.i«i.i.!.l.!.iitli|.!.:.:.ilaf Illlll II is! i'si.iii aillils al -ills siiljsiSs 11s
                                                         ^&^msimwM&
                                                                                                       as sis
                                                                                                       is s
                       .|.l.;.|iig;5;;5a^

                            .j.i.j.j:i.j.i.|.j.|.j.;.i.!.!^^

                                                                             lilt ft fill

                                                                             ilflawlaij
                                                       ^

                                                                                                                                                                                      stiessajsk; !
                                                                                                                                                                                      TrrrTiTi;  i
                   	       -   .        	,,,-,,.   ,  .,   -,      -,-
  s J3*l.c»;a'1j'jii|7:|i3!a!5;«5-.sa;a:3^i;:3:!:-3;r:c;«,e;»ii;i:»ie"j:5 g3J«|cW|gi:!c!x|:|>i3!«ijia xjnc »!» x!< «|xI«jsj*j*ljJ8JsjxixJ8:gigj.':8j.jc|i ajj.f'sitio^s^iti.pljiciiitjaiSiXjt !lsj»:«|S'ci: ajeB;
^	;     I     '  I  ; 'i    i !    |;-—--,--   ;-,--.  -;  ,  ,      ,            '  !  !   !    i   L     i  '   I  M I       I  r  i  ' r   '  '  :   i    I   :         i     '   I     .  I    , i    !   i  I       I  '   Zi

 j::s:s.:'j;«,j«:t!s;3:i'81«l»|Jia:8,ji;s!«i»iai«i::=s:=!s!=:BiBi;ia,Jisi«i>|fl;«iRi:^l*|la:aiS:«sj:lsl';=:=]S|=.»l=:=:=W!::qi«i.:8:iS!Si=;^

•.:'•'"~~'~rr--'f'rr\--""'-r~~'~r\~~~'^^^^                                                                                                                                 PTi f!*!
                                                                                                     itia.aiaisialsiaislajaieltii.tblireKiiltia.itnwitjgltlTltiaitnitigialwil.itN^wi-^nftMwlvtwiiasi
                                                                                                     .|.|.BI..|5|....|.i.|.|.l.|.i....i.ia..l.|..|.pa..|.|..|.l.|.|.l.l.|...i.a|.i...i.p|~'.i^.BB.i


                                                                                                     |B!B|siBS«i:qixx)a>;sia|B;a:|:|K£:sj<|2l:an!;i:!a»glswia*|3l:ia!aielc'lce!ai8la|ilaL»acala':
                                                                                                     I...,-..l.|.i-.2,.lala. .1-'-!...!-!-,-,.00- .f.-|-.1.1. . .l3.t.lo!a.«la>a!elaalalo!aa at lo at.M.iat
 f—:    ; "   i  •  i '  '  i  " i  !  ' ;  •  • ;  !  I i  i  ! M  • I    '  i '  '  i I  i  '  i !  I  i I  i  I  ; i  i  I I  I  .  I !  i  I   I  .  111 P  !' t'.  ' I  '  i 1  1  i  ! I  I   I  I   !  11!
,g;s s J,« K t ju a a s s::;,s i j:s;i,ji. s i: >i»!s!ji:3'S J,3;3 XiXixiaia'.iaia alawsjsix aigf* 3 alaiaiaiaialaiaia.iai.'ixlxja ax:x siala sia'aiXiaix ijaixlaisials aia a i:a aia a;
'j^e'a a oa a ajalaialaytalalaLe aiaiaioraiataia oia;a|aja[« e,e|a|aiaia aiaiaiato.aialaiaieielelalo.aiaialaieiBiaja^iaialala aia|aiB|a>aK.a a e e.e e>eio 0,0 eloioaiaiaiO>aia]aala>a|a|-|.i.rj»|>|»» ^r,»,»|-rrr|a, »;»»|»|- :p.|»p|»l»i>|.|-l»l»-.-.iP"H-|"j»-|->|'-<-.-|..»|P.i»l»-!»,•• ;»l»|»|P--.|>|»|»|«|«;«i

                                                                 5,;:s:nR jss'Si^E'tisssii'j.sirs1: s'BJis's.Js.jst ss.s'S.i.jsS'S.sis^^.i^aii^iiTEijisi^a^^lsi.s'a'i'C.)!1",.!:!^!:!*:1*.
                                                                                                                                                                                                   ;*;  *:
                                                                                                                                                                                                   | -*'  f '
J a "a"* :~.ia>lix>'S;'g;i:alaig!«8,<3'3'*!Ka:'Xislx!aK3i8;i:.ig!i:a,;;a;B'aixi88l'':^>s|*:g<8^lS!:<>iajXlsix:»'!:3:a!s^:i8iB«
U'-j -tun •>!->« .n -> «,m »nn.«iin Mia'*'.«iaiiA «i«i«i«ii« n -f • •n»iml*i«|iff)«il*'*i*i-».»»'n' *>.m -f ami'a m » in * n>iin|uii-t'«iliol-f «i,«nn1->t*|«|ti> *nB|« » «>«<« «iai«t*i«,«»t«»'.''*^-»'^i»l-*'^<-»^'*;
It j *..,* » * » ; s s:s,xp x S:»'» » S » XiSiX.XIX X «*.«:» Xn{X.X,X,X;X|X:XiX S:S.5 XjXA.
... a,a,a a a.aia.a,. a,, al.;. . . a . o . ... . ........a;. a|. a ..... . ....a;. » . . . .,,
                                                                                              'S.s « R « n x.s.*i«,s s *u.r s K'ft^.a.
                                                                                              o eieiaaaieiaia.a ajaia eaalai
                                                                                                                              .a.AiftjX.aiAcisi^^Xiftwxjwxjiiivixiff^iviAi;;;^!; ;|o,9|9 s^.s^iwa.B'Jis
                                                                                                                              iajaja a|a|a!ala|a|a(«i»laja a • «|a a a •iejeiaia |ele|*>|aie|ai0 alaiajojW* *ta|*l
  8 8 s 8,8 giaiaia51'a;t!8.a>aia:aaiRa:wii«ia!iiaia|«|il*!*IBi*W<8|i!fmwi"'3S;«;ip«ra«E,a>a B !^|a;8:8l=:a!:laisj.'.iatgjg,?;8;ai)iji?5;»B'?l8igi.iS!aiSiai8iS!8j||n|8i8i«'»i»|g|a E<8lEixMi£,a|3'*!
  a e ^e^e'aia.aiaialoaiaiaiopo.aia-aiototoiajaia^loSagigppgjgppfflgglgiglB'BJBCIg B|B|S|g Bjg|g SlS BIB B[SiBJBBg|B B|8ia|^|r|sis|; ; "'"I"r |''l*|gjSi^ig^!=!=g!g8!8gl8^iJ*l''|'"rr- !*
                                                                                                                                                           88|
                                                                                                                                                           Bja|
                                                                                                                                                             8|888!glg|g888|g|.a«»UUl
                                                                                                                                                             ja|» olSiato OJ5 5 »loj    I !  I  I  I

                                                                                                                                                                I'll!1!    Ill'
ge s 8'8'S s^aaasaia.sgiBiSiSiSiSS'aisn.Bg^S'Sis g BIS
it a eia a p elO|a[aiaia|alaia'alO|Bia»aiataialO|B|aiatB'aia}a a ala^
                                                                      gl8lg!glg|gg|gg!g8>8g|8lgig;gig|g|g|glg
                                                                      • [•ieloia;aia|a a.aieialeialotaieieialaiaia
                                                                        '
                                                                      si
                                                                      ja
                                                                     ssp'JiSI^SE ! 5 -S*! J'SSi* S J! SI'S * *
                                                                                                                                                                             gis. -isisna a
                                                                                                                                                                             rrj    lri-|-
                                                                                                               I'J'I:! s'S'S'.'.'.'si'Siiis?! iI:!';2:J:;.ij.i:S £!J'!!i!!: SlSsbiSS'biSSc'SS'aSlS.S.iS!
                                                                                                               i  !  i 1  '  I •    •     I '       I  .  : .  i  I  ' !  .  I t  I  I I  .  I I .    I  i I  i  i  I I      .ill'
  fja'J^'B'a JlB;8-s!8:8ii=;tl.i«i«lt:s:S'a!«:«>:s8:«Tisi8!.;»;»:il:iS:sisl8;»is;t,;^lB!!!:*;;iSis:a;s.sJi
  « •,at«wl*taia|«i*lal»>|a|a,*|aU|aiaiaia!aja}«i)a|alaU
-------
    1
        SSISjSISiX!
        8388 8 8
                  ! !  !  i  i
         sis s as
         318SSI88!
                                                         Ill    I
                                    SSSSSS3SSS8S 3:8:8,3,
                                                              8188,888
                                                                                      iS2
                                                   o» I en tut A,!***
                                                 8S28|8|-]!5
                                                   8 8 3 Sis 8 8 8:2i2i2
         S
         i
8 S;S|Sia|g 8
                           a,s
                                       S
                                       us
                                                   ,88s sis
                                                            8,8
                                                             JSB
                                                               isss
                                                                      ilili
                                                                      w =**?*»
                                                                                                           ss:?
 ii
   S«C
   S88S
                    S2SS
                             sal"
                             8.5IBI8
                            S3 Si
                          SiS 888
  M
  1618
                                                 §55
                                                 $13
                                                                    SSI
                                                              SslS
                                                                                       88:
                                                        b*!bllb»>*'*
                                                        SISISIB'B
                                                            ls[
                                                     ssis^s'lfsl  :
                                                        S'saiS'SSg!  :
             s a s si
                     MM 11*
                                    S
                                  SIS
                             42
  I
ill
SSIB
illElS
S|B|o|8
sift®
                                                                                            ss
                                                                                            ss
                                                                                                              ...
                                                                                                         m,v a 01
                                                                                                        — MI —.81—
                                                                                                                    iiill
                                                                                                                           i'SiSM.iii's
«r'wo-*M-j'^*
s|S 8 8JS &|.|S S
                  SS,8
                         sslalst
                                    sslsisia
                                                                                  s sis sis
                                                                                        5SSSS
                                                                                                                       £§!§
            ..88
            S83S
                                   B!M|. Blti
                   siBls gjsis^Sislslsis.s'a
                                                          S81
                                                                                   Kit!
                                                                                   se
                                                                                                              sss
       S'2l8 8
               88889
                                                                         232SS
                                                                                     a a    a a a|g s a sis a  s-sl    aaja ssi
    asiii.isislaSSiM.s
                                    sislls
                                            t
                                            fa»|MlO|lo
  8 8 81818 8 8,8l8!8l8:8|8i8 8 8
                         §l§§l§l§!§ll§l§!il§i§l§i§l|§!§8i§|8lii8|§|l|§i§!§i§!§i§j§|§i§8i§i§l§:§§§liii|88|8:8:
                         -H—i	1—i—'—1—i—!—I—i—'—i—TTT—~i—i M .	'     i i    ' i  r1   I     i       1          r;    i !  '     i         «
                            tim V!
                            )i- a,
            oio!o|p{o
   8l8l8lSi8|8;8l8i8i8
                                                      i o.oiei oo o|o'oioloopiejoiojo.olojo|oioio|o,e'oiO|0|o|o|o|o|
                 OO O OiOIO^^IO.W^^'^t^^^l*S|^'*p'l»p'fcJ|^'fc*i'^|«rflfc*'>rf*p* **fcrf ^rfitaiv**^*^*-*-'*-'^'**]'-''——•»-•—••—•!—• — —I— — I —.  <    ~ ~ ~ ~  :i -. ..L • ...i .,, « 1-1 mi* r* M
                 sss&siBisis.ssisissisisiasssssisi&s^aissigiSiSsslsiisiasiSiBSiSisslsisiSiSisiasi&sisisiSisiSiSisisiSiSiss'S'^
                 —•	.	1—i—i	1——i—i—i—i—i—i—t—i—i—i—i .  t  j—i—•—,—« ...     i i—t—.—  '  i—— •	1—t~i     •  :  n         '                  ~—.
                                                                                                                 o.o.oioio ooo
                                                                                                          .i-i-,-i-
     S 8 2 2 8 8|8 818 2lg|8 S{8 SiSIS S
                                                                                                !ii! ss siaisi
3:2
                      '
                        gsi8iag!8s!5
                                                                                                           i'O O O O '
                                                          lsisiS's!:; a!Bls;8ai-;Misi8si8 si
                                                                                                                                     :8
s 8 i s s'K;sis!5!5iKbis;s!sisio!ii!ois s s!~i~i3:3!3;aisiBiis s:sl2isis;8isi8i8sa!Bia|S!S|a!s!aiSisiaiaia!s!aiK!s!S|a!2|sia aiaiai
 i     i  :  '       , '  .     ,    '   ,   ,  '    ,   '    ,  ,   '  ' '     i  ,   ,     i       !  !     , i  ,  '  i ,  *  i  i i  ,  '   ,  ;
                                                                                                                               > o o o o i
                                     '—I—loi  n'mioiloloioio o'o oio o oioiolelo o o oioiojoioio o|oiplo|o|o o|O|O oio.op,o oTo ojo>M.K>,U u * w M t-» u
                                                                                                          C>N> CD U £ M * CD W -* K> — O O O ^
^sls!,;si2:siMl;;s!2!2ia!aisig;ai8:a!s!2!s!o!8islsig|a:5i.;s:5:a'oi^                                            Sisis's 5 951 S.5.5 5'5 S15 5 S
                                                                            :2:a 2[a!Si2i2i2ia:aiaa,a:a!alai2;2:a.8.a 2'a,a:a a s,2.a a a s 2,8
as  sia  a   asi   aiSissgsis aais
                                                                                          is saiaasjsjs ssjs^'S s'sis^
                                                                                                                              g.ssg
            2 S HlHlSlolSlH IS KIBJtilS SigiSl
                                                                            HOlOIO|0 OIO O;o|oi0|0t0|0lojoio[0lo|0'0 O'O O O'O O O 0000 O O O •;
                                                                            ,,_.:—,— —i-*!—'—,.*,-*— ._»]_*,_*;_* — [_.,.*,.* '.* — -• -* — rt'rt.-t ^'rti^'rt;^ rt rt r; '
                                    !8;gi8 Sils s2.S S S 3S:S'23:S;S'B:3 y;S,S
                                                                                                                        2 S S,g,2 SSS g.
                 — o o
                 o!S S
                                    ila
                                               gcriiui
                                              l^JM.
                   ssssss
                                               ssaasss
                                                            a aiaia 2 a
                                                                    sa;a-s;sa
                                                                                                            oooo|oc
                                                                                                                                  alo oS
       sss
                       sl^saass
                                                -I-
                                                SIS
                                                        SIS Silt SB
    8838
                       888
                                 832
                                                  aa
                                                        ,!olo
                                                       aaaa
                                                                       a SIB s a s ft s a
                                                                               p o
                                                                           aaaa
                                                                                                       w w w -viis) u AII
                                                                                                       £1       '
                                                                                                                                      ''
                                                                                                            oioiolo'olo o'oloio
                                                                                                                      III
                                                                                                                                     >W
                                                                                                                             OIOIO'O O
 sa
              sis s als
                       seas
                              2,8863
                                                                      aa
                                                                               812,818 8 »
                              sssssss
                                                      w wI Oi|
                                                             SSSl
                                                                        ss;
                                                                                    s|s
 8288,8818
            8i8i8l8ISl8
                          888888881818188
                                               S8!88,88|8{88i8i8i8
                                                        8188181818 8 888 §818,8 8 8,8-8 8|8i8'8:8:8 88 8
  22SS222
              S22SSSSSSSSS8S8SSSSSS
                                                                                                 O o!oiolO!0'0'0'
                                                                                                 O|O'OlO!o|O|OlO|

                                                                                                 —i—I—t
                                                                                                                   O oiojolojp O*O'O O O|O-lt'
                                                                                                                   o oioioio o oioioio o'oiw
 88888888 818888888 8 888
                                 8888888 818 8 8 8 8 818 8J8J8 88888888
                                   isssss
                                             g 8 a a s s s
                                                                                             SBS
                                                                                                  Sid
                                                                                                         ^i^.^i^j^j-j.^i^^^i
                                                                                                          Sl*l^|a,^,«.u< ain.ot'
                                                                                                          ,v,OiS,Ci— Jk ui 0» — ,
                                                                                                          ,
                  83
                            8832
                                   I
                                      sss
                                                       S.
                                                       S3 SiS
                                                               SSi5
                                                                          	SiS
                                                                          S 8,8 S 8 8,
                                                                                    SS3S5I33
                                                                                          SSS
 .
                          S3SSS8
                                          s M S 8 8 S
                                                                                         sgasaas

-------
   !!*S.5;S8!5i2 "l&ftMjj^^
                                                              x*|3 sss R a a|8 R a 8 s sn ss ft 3 8 Rl«R as scsfc sse as): »8jess6B8SKS«88c abasia xlsld
                 ™::i8 *:S S|g- — >-«-(Mfii Min
      S;S, JiJ.BISiajS 8^[SiSI8!S!SiS|SiSIS'8 SiS 3:S!S JIS S'JIJ 8IS S 8888888
                                                                                                                                     88883888 8181
    8 8 8:818 8:8 8 8|8l8!8ISI8{8!8 88 Slsla 8 818 8!8!8 8 8!8l8 8 8|8 8 8 81818 888888888 =Uls SlilR S
    8 8 S S:8 Si8:8.S S'S:»i8,S,S:J S SlSISISiSlSISlEiSlSiSls 8 SiS S'S 8 81818 J J
SJSSI&s ssl8iS!8J8ls;si8 S ttlWJiS!
                                                                                                         6 S'£ 8888 SiS bfiss 8 &
                                                                                                         o olo o o o o eje o o|o o o ti
                               O|O|OJO|O|o|o!O|OIO|O O|O O O O>O|O o OJO o
  O 0:0,0,0,0 0,0,0,- OiOI-'ol-lo'..!- -'0'-.-i- - -i- -'o - -.-l-i- -,-
                                                           3 feigls 8 Sisis 818'S fe'sls
  G Z S I i i:ff!S S S.E;
  £ i.iiii §!§! oill'l !i i iil'i'i 8:8.8:8 8 8.8,8 8 8 8 8:8,8 8.8 8,8:8.8:8'8 8 888 8:8 8'8 8 8 8 8 8:8,8,818 8'8 8 gj8ig!g|8|8 8,8;8 8 8 8,8 g 8 8^818 g gigigiglglSiS 818)8 S:8:a:S

                                                                  I
                                                        jslalsigiiisia S'a R Ri»;8 s
  «2
                                                                             0|0.0|G
  i I !||;lll!8:8;8'8 8 8 8,8.818,8^8:8:8,8:8:88:8 SiSiSig'S^'SlS'SIS 8,8 8 8 8'8I8!8!8 8 8:E!» S^^;!;sjsig;i|S:a S'e'SISRJiE:8!ai™Sc:s:ai8S
  ; 8 8,S S,8 S S:S:S 8 S:5'S S'S S:8ia;SiS!8ISI8 Si*
                             '!^5!5iin^
:3 S:« R X'S s i J:C'
                                                                                                                            8!8:8:8,8.8.8:818:8 g^s'S'SigiagiS'SftS:?
                                                                                                                              :.8|R
                                                                                KIR SiZiE S
-------
Inlet
All data in ppmv wet basis 1
rule conditioned outlet/Intel kin 2
Description Austin White
Method line Sac Al cond |




Starting Dale/Time- Wed Jul 01 19 26.02 1998
Time
2001:57
20:0257
2003.56
200456
20.05.56
2006.57
20-07 57
2008.57
20-09 57
201057
201158
20.12 58
20-1358
20.14.58
20:15-59
201659
20:17:58
20:18:58
20.19.58
2020.58
20:21:58
2022:59
2023:59
20.24:59
20-25.58
Average
Standard deviation
Maximum value
Minimum value
C6H6
0.76
082
084
0.82
088
091
093
090
091
096
096
0.87
091
099
090
089
083
085
065
076
0.85
093
0.93
093
109
089
007
109
0.76
(«-)C6H6
033
032
041
043
045
052
053
059
0.56
055
055
062
058
0.59
0.59
058
057
056
0<1
0.63
061
0.66
0.68
071
0.78
0.56
Oil
0.78
0.32
C7H8
000
0.00
0.00
000
000
000
ooc
000
000
0.00
000
000
0.00
000
000
000
000
000
0.00
000
0.00
000
000
0.00
000
0.00
000
000
000





[+OC7H8
105
101
128
1.36
141
164
167
187
178
1 75
1 74
195
183
185
1.87
184
1.79
1.77
194
198
193
207
2.15
223
247
1 77
034
247
101





OXYL
0.00
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
o.oo
0.00
000
000
000
000
000
000
000
000
000
000
000





[»-)OXYL
067
OSS'
082
087
090
1.05
107
120
1.14
12
.11
25
17
.18
20
18
1.15
1 13
124
127
124
133
137
143
158
1 13
022
158
065





MXYL
000
000
000
000
000
000
000
000
000
000
000
0.00
000
000
000
000
000
000
0.00
0.00
000
000
0.00
000
000
000
000
000
000





[*-)MXYL
1 41
136
1 72
183
189
220
225
251
239
235
234
262
245
248
251
247
2.41
237
260
266
260
278
288
300
331
238
045
331
136





PXYL
198
184
211
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
024
066
211
000





[*-)PXYL
153
1 47
1 87
199
205
239"
I 244
273
259
255
254
285
266
270
273
269
262
258
282
290
282
303
313
3.26
360
258
050
360
1 47





STYR
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
ooo
000
000
000


- - --
Bt-)STYR
r 1 22
1 18
150
1 59
1 64
191
|_ 195
2 18
207
204
203
228
213
216
2 18
215
209
206
226
231
226
242
250
260
288
206
040
288
1 18




13BUT
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
018
018
0 18
000
034
000
000
028
000
000
005
010
034
000




(+-J13BU1
020
019
019
018
018
018
018
017
0 18
018
017
016
019
020
018
017
017
016
015
015
016
017
018
019
021
018
001
021
015
CO2
000
000
000
000
000
000
000
ooo
000
000
000
000
000
000
000
r 000
000
000
000
000
000
000
000
000
000
000
ooo"
1 000
000





(+-£02
059
057
072
076
079
092
094
1 05
1 00
098
097
109
102
104
1 05
1 03
101
099
108
1 11
1 08
1 16
120
125
138
099
0 19
1 38
057





H2O
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000





(»-)H20
12696
12204
15498
16491
17012
19839
20244
22603
21477
211 51
21027
23612
22066
22363
22621
22249
21698
21374
233.95
23988
23378
25066
25963
26970
29809
21392
4098
298 09
12204





C2H4
227
249
253
261
262
256
272
271
271
275
271
265
278
271
274
278
265
273
272
264
268
2.69
282
269
277
268
012
285
227





(«-fC2H4
012
011
Oil
Oil
010
011
Oil
010
011
011
010
oto
Oil
012
010
010
010
009
009
009
010
010
010
011
012
010
001
012
009





C2H2
018
020
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
0.00
0.00
000
000
000
000
000
002
005
020
000





(+-E2H2
018
0.17
022
023
024
028
029
032
031
030
030
034
031
032
032
032
0.31
030
033
0.34
033
036
037
038
042
030
0.08
042
017





C3H6
1 54
105
1 73
1 41
1 74
1 51
131
1 57
1 55
1 70
153
165
1.75
1.75
1.78
164
1.68
1.88
1.29
174
197
2.07
2.02
200
191
1.66
0.24
207
105





[+-JC3H6
035
032
032
031
030
031
031
030
031
0.31
030
030
033
034
030
030
029
027
026
026
0.28
030
030
032
0.36
031
002
036
026





CH3OH
000
000
0.00
000
000
000
000
000
000
000
000
000
000
000
000
000
0.00
0.00
000
000
000
000
000
000
0.00
000
000
0.00
000





»CH3OK
014
013
013
012
012
012
012
012
012
012
012
012
0.13
013
012
012
012
0.11
010
010
011
0.12
012
0.13
014
0.12
001
0.14
oto

-------
Outlet
AH data m ppmv wet basts
Title- conditioned outlet/Mel kiln 2
Description. Austin White
Method title- Sec Al.cond




Starting Date/Time Wed Jul 01 19 26-02 199f
Time
193156
193256
193357
193455
193556
19-36-56
193756
193856
193957
19*055
19.41:56
19-42.56
19-.43.S6
1944.S6
19:4558
19-4657
19 47.57
19.48 57
19 49.57
19 50:57
19:51 57
1952.58
19.53.58
195457
19.55 57
Average
Standard deviation
Maximum value
Minimum value
C6H6
043
049
046
035
054
0.43
052
047
0.44
033
041
036
039
039
036
040
031
031
040
044
049
059
059
063
054
0.44
009
063
031
<«-)C6H6
Oil
013
012
012
015
012
013
015
021
017
0.17
019
017
0.19
018
018
0.15
010
011
013
0.14
0.17
021
0.25
026
016
0.04
026
010





C7H6
O.OC
000
000
000
000
000
000
000
0.00
0.00
0.00
000
000
0.00
0.00
0.00
000
0.00
000
000
000
000
000
0.00
000
000
000
000
0.00





(*-)C7H>
036
040
038
039
047
037
041
049
065
055
055
080
052
061
056
058
046
030
0.35
0.42
044
055
065
0.80
084
051
014
084
030





OXYL
000
000
000
000
0.00
000
000
000
000
000
000
000
0.00
000
000
000
000
000
000
0.00
000
000
000
000
000
000
000
000
000





(+-JOXYL
023
026
024
025
030
024
026
031
042
035
0.35
039
0.33
039
036
037
0.29
0.19
022
027
028
035
042
051
053
032
009
053
019





MXYL
000
000
ooo
000
000
000
000
000
000
000
0.00
0.00
000
000
000
000
0.00
000
000
000
000
000
000
000
000
000
000
0.00
0.00





[+JMXYL
048
054
051
052
064
050
055
065
088
073
074
081
0.70
082
076
077
062
0.41
047
057
060
074
087
108
1 12
068
018
1 12
041





PXYL
122
1 42
1 50
144
1 44
126
1 58
147
145
137
1.22
1 39
1 18
137
1 10
136
1 02
107
128
167
194
1 75
188
188
219
146
029
219
102





[+JPXYL
052
058
056
057
069
055
059
071
095
0.80
081
088
076
089
082
084
067
044
051
062
065
080
095
1 17
1.22
074
020
1 22
044




STYR
000
000
ooo
000
000
000
ooo
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
	



[tJSTYB
042
0.47
045
045
055
044
047
057
1,76
064
064
n'o
061
071
066
067
054
035
041
049
052
064
076
094
097
059
0 16
097
035





13BUT
000
000
000
000
000
000
000
000
000
000
000
0.00
000
000
000
000
000
000
000
000
ooo
000
000
000
000
000
000
000
000





(tJISBUT
0 18
6 18
019
019
019
020
018
019
0 19
019
019
018
018
018
018
019
016
016
017
018
018
019
019
020
020
018
001
020
016





CO2
' 000
000
1 42
1 51
351
000
000
^_ 329
579
425
481
498
529
528
625
574
312
000
000
000
000
000
000
000
000
221
244
625
000





(+-JC02
020
022
021
022
027
021
023
027
037
031
031
034
029
034
032
032
026
017
020
024
025
031
036
045
047
029
008
047
017





H2O
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000





;+-|H2O
4329
4836
4617
4697
5732
4524
4916
5869
7879
6588
6673
7306
6298
7397
6822
6964
5563
3677
4239
5098
5368
6665
7869
9710
10096
61 49
1642
10096
3677





C2H4
146
163
1 54
163
1.58
165
1 55
1 61
162
166
1 73
180
160
182
161
164
163
160
174
162
1 72
166
171
168
159
164
007
182
1 46





>-)C2H«
010
010
Oil
011
Oil
012
Oil
011
011
Oil
Oil
Oil
Oil
Oil
011
Oil
009
0.09
010
0.11
Oil
O.tl
Ott
012
0.12
Oil
001
012
009





C2H2
0.19
017
017
019
0.13
016
017
018
016
0.15
0.18
01«
020
015
0.18
017
019
014
018
017
0.16
018
020
018
016
017
002
020
013





(t-)C2H2
006
007
007
007
OOB
006
007
008
Oil
009
0.10
0.10
009
Oil
010
010
008
005
006
0.07
008
009
Oil
0.14
014
009
002
0.14
0.05





C3H6
124
076
082
078
124
076
056
105
063
1.27
069
1.12
106
074
086
103
1 12
079
082
1.43
0.79
077
too
104
109
094
022
143
056





VJC3H6
031
030
032
032
033
034
031
033
033
033
0.32
031
031
031
031
0.32
027
027
030
031
031
032
033
034
035
032
0.02
0.35
027





CH3OH
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
000
0.00
000
000
000





V)CH3OH
012
012
013
013
013
013
012
013
013
0.13
013
0.12
0.12
012
012
013
Oil
011
0.12
012
012
013
0.13
013
0.14
0.12
001
0.14
0.11

-------
                          APPENDIX D




                    FTIR FIELD DATA SHEETS
K 'O»1-0:\002\OOWHITEUM\WHTLIME RPT

-------
Facility
Stack ID
 KlU
                 FTIR Temperature Readout Sheet
       Outlet Stack
          \10
                  '3(7
                              3)
       Inlet Probe
                                     33?
                                                                     77 ^
       Outlet Probe
                                                 3V2
       Inlet Filter
       Outlet Filter
        Inlet HT
                    3/2.
        Outlet HT
       Inlet Pump
                                           266
                                              7.70
  10
 Outlet Pump
                            516
                                   3/2.
  11
       FTIR Pump
                 '7
                                                    Z??
  12
 Pump Box
            \-L~l
/ze
/Z5"
I'M
  13
  Extra HT
  14
       FTIR Jumper
                                     72?
                                        120
                 77
                             7/7
 15
Pump Jumper
                                        '321
  16
  Hot Box
                       35" /
  17
        Hot Box
  18
  Extra HT
32.7
311
     30?
     7*2.
  19
Electronics Box
                             9
      9$
 20
                                                                           Al

-------
 Facility
 Stack ID
  Date
Run Number

                                FTIR Temperature Readout Sheet
 Channel
Description
\yx'\l'»
                                                                                               Ml 5
        Inlet Stack
                    42.?
        Outlet Stack
        Inlet Probe
                                                                        3*8
        Outlet Probe
         Inlet Filter
        Outlet Filter
                                    S2
                                                             3VV
         Inlet HT
         Outlet HT
                                                                        7V
                                                                       3V7
                                                                       g~7*f
        Inlet Pump
              ^77
                               27
           •25^
                                                                     2.11
   10
Outlet Pump
                                                                                            33*
   11
 FTIR Pump
                                          •Z7/
                                                               27
                                                                      30*
   12
 Pump Box
                                                /t
   13
 Extra HT
                         zee
                                        2-1*2-
                                         2.7?
27?
27V
277
17*7
   14
FTIR Jumper
                               717
                            3/7
                                                     721
   15
Pump Jumper
3*
                                                      12. V
                                                                     lit
   16
         Hot Box
                                                                        3^7
   17
 Hot Box
                                                                                    2,5"
   18
         Extra HT
                               1*7
19
20
       Electronics Box
                                                                               99

-------
  Facility
 Stack ID
  Date
Run Number
                                           FTIR Temperature Readout Sheet
Recorded By
 Channel
         Description
          Inlet Stack
         Outlet Stack
          Inlet Probe
         Outlet Probe
          Inlet Filter
          Outlet Filter
           Inlet HT
          Outlet HT
                                     V}!
          Inlet Pump
   10
      Outlet Pump
   11
       FTIR Pump
   12
       Pump Box
IX
   13
       Extra HT
   14
      FTIR Jumper
   15
      Pump Jumper
   16
        Hot Box
   17
        Hot Box
   18
       Extra HT
19
20
        Electronics Box

-------
FTIR Temperature Readout Sheet

-------
                          APPENDIX E




                    PRE-TEST CALCULATIONS
K 'ttW|.02\00:\001\WHITELiM\WHTLIME RPT

-------
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
  CO-, (potential interferant)
    20%
 0.000002
0.0036
 H,CO (potential interferant)
   1  ppmv
0.0002100
 0.386
 CH, (potential interferant)
                  0.0105
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.


Appendix D

Estimating Minimum Concentration Measurement Uncertainties (MAU)

The result for HCI is:

MAU (HCi) = 0.4 ppmv.
K \OWI-02\00:\(XHWHITEL!M\WHTLIME RPT
                                          E-l

-------
This value is computed using the formula given in Appendix D. However, this value is derived
using band area calculations.  The FTER spectral data in this field study are analyzed by classical
least squares (CLS), not band areas. CLS derived minimum measurement uncertainties for HC1
are on the order of 0.1-0.2 ppmv for this test program.

Appendix E

Determining Fractional Reproducibility Uncertainties (FRU1

This calculation estimates the uncertainty in analysis, using band areas, of two sequentially
measured CTS spectra collected immediately before and after the HC1 reference spectrum.  The
calculation is performed in the analysis region used for HC1. The result is:

FRU(HC1 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 HC1 analysis region.
The table below gives the results.


                         TABLE 2. FCU DETERMINATION
Analyte
H,O
HC1
CH,
ASC (ppm)
113000
253
491
ISC (H2O)
115000
-22.5
-23.0
ISC (HC1)
0.000
254
0.000
ISC (CH4)
0.000
0.000
493
FCU
-1.7%
-0.4%
-0.2%
AU
-
30%
-
Appendix G

Measuring Noise Levels

The result of this calculation is given under the Appendix C heading.
K.\0091-02\002\001\WHITELIM\WHTLIME RFT
                                          E-2

-------
Appendix H

Determining Sample Absorption Pathlength CLst 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.
 K \009I-0:\002V001\WHITELIM\WHTLIME RPT
                                            E-3

-------
                          APPENDIX F




                   POST-TEST CALCULATIONS
K \009l.02\002\001\WHITELIM\WHTLIME RPT

-------
Below are the results of the Method 320 post-test calculations for this test program. The
calculations are organized by appendix as found in the FTDR 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 Uncertain!
These calculations determine the fraction
HC1). The results for HC1 are given in th
outlet test. In order to achieve results that
equivalent of the calculation was perform
by the HC1 concentration.

             TABLE 1. FMU CALCU
                                       1 error in the analysis for the analytes of interest (i.e..
                                       table below for 1 spectrum selected from the inlet and
                                       are consistent with the CLS analysis approach, the CLS
                                        . This is simply the reported analysis error divided
                                       ATION FOR HCL -AUSTIN WHITE
Spectral File Name
RN010007.spa
RN010042.spa
RN010007.spa
RN010042.spa
Inlet/Outlet
Outlet (#3)
Inlet (#3)
Outlet (#2)
Inlet (#2)





irror (ppm)
0.23
0.17
0.16
0.15
Concentration (ppm)
17.1
9.53
6.86
4.78
FMU
0.013
0.018
0.023
0.031
Error is 95% confidence interval reported by CLS software.


Appendix J

Overall  Concentration Uncertainty
The CLS equivalent of overall concentrat
software.  The results for this test program
                                      on uncertainty is simply the error reported by the CLS
                                       are found in Table 1, above.
                             i ">•>,.» • >••/ .  :   .  1^'-.  ... ,
                                        f,  .  .     .,.* ;• :
                             r%.; 1 .v*.   v n<, ••  -      . - .*,
K \OOTI-02VX)2\001\WHrrELIM\WHTLIME RPT
                                           F-l

-------
TECHNICAL REPORT DATA
(Please read Instructions on reverse before completing)
1. REPORT NO. 2.
EPA- 454/R-00-008
4. TITLE AND SUBTITLE
Final Report of Lime Manufacturing Industry
Fourier Transform Infrared Spectroscopy
Austin White Lime Company, Austin Texas
7. AUTHOR®
EMAD
9. PERFORMING ORGANIZATION NAME AND ADDRESS
U.S. Environmental Protection Agency
Office of Air Quality Planning and Standards
Research Triangle Park, NC 2771 1
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
3. RECIPIENT'S ACCESSION NO.
5. REPORT DATE
May 2000
6. PERFORMING ORGANIZATION CODE
8. PERFORMING ORGANIZATION REPORT NO.
10. PROGRAM ELEMENT NO.
1 1 . CONTRACT/GRANT NO.
68-D7-0001
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 nrotectinn Apenr.v i«t invpRtioatina thp limp munnfartiirinff
  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.
                                      KEY WORDS AND DOCUMENT ANALYSIS
! a. DESCRIPTORS
Hydrogen Chloride (HCL)
Hazardous Air Pollutants
18. DISTRIBUTION STATEMENT
. Release Unlimited
-« -•". *.*•••.' f •
b IDENTIFIERS/OPEN ENDED TERMS
Air Pollution control
Fabric Filter Baghouse
Wet Scrubber
19. SECURITY CLASS (Report)
Unclassified
20. SECURITY CLASS fPage)
Unclassified
c. COSATI Field/Group

21. NO. OF PAGES
120 t
22: PRICE
EPA Form 2220-1 (Rev. 4-77)   PREVIOUS EDITION IS OBSOLETE

-------