United States
Environmental Protection
Agency
Office of Air Quality EPA - 454/R-99-018
Planning and Standards June 1999
Research Triangle Park, NC 27711
Air
&EPA
Secondary Aluminum Industry
Final Emissions Test Report
Gulp Aluminum Alloys
Steele, Alabama
-------
Table of Contents
Page
1.0 INTRODUCTION 1-1
1.1 Objectives 1-2
1.2 Brief Site Discussion 1-3
1.3 Emissions. Measurements Program 1-3
1.3.1 Test Matrix 1-3
1.3.2 Test Schedule 1-5
1.4 Test Report 1-5
2.0 SUMMARY OF RESULTS 2-1
2.1 Emissions Test Log 2-1
2.2 Dioxin/Furan Results . 2-5
2.2.1 Overview .\ 2-5
2.2.2 Dioxin/Furan Emission Results 2-5
2.3 HC1 Results ':....,.. 2-18
2.3.1 Overview 2-18
' 2.3.2 HC1 Emission Results ; 2-19
2.4 Particulate Results 2-23
2.4.1 Overview 2-23
2.5 FTIR Results . . 2-26
2.5.1 Overview . . . ;. . 2-26
2.5.2 FTIR Emission Results 2-27
2.5.2.1 EPA Method 301 FTIR Validation Results for HC1 2-28
2.5.2.2 FTIR HC1 Test Results 2-28
2.5.2.3 FTIR Process Optimization 2-32
2.5.2.4 FTIR Screening Results .. 2-33
2.5.2.5 FTIR Sampling and Measurement System Response
Time Measurement 2-39
2.5.2.6 Comparison of FTIR and Method 26A Results for HC1 2-41
3.0 DESCRIPTION OF FACILITY 3-1
4.0 SAMPLING LOCATIONS 4-1
5.0 SAMPLING AND ANALYTICAL PROCEDURES BY ANALYTE . 5-1
5.1 Chlorinated Dibenzo-^-Dioxin and Chlorinated Dibenzofuran Emissions Testing
Using EPA Method 23 5-1
5.1.1 Method 23 Sampling Equipment 5-1
5.1.2 Method 23 Equipment Preparation 5-1
iii
-------
Table of Contents (Continued)
Page
5.1.2.1 Glassware Preparation 5-3
5.1.2,2 XAD-2® Resin and Filter Preparation , 5-3
5.1.2.3 Method 23 Sampling Train Preparation '..' 5-5
5.1.3 Method 23 Sampling Operations • 5-6
5.1.3.1 Preliminary Measurements ..........\.' 5-6
5.1.3.2 Assembling the Train 5-6
5.1.3.3 Sampling Procedures 5-7
5.1.4 CDD/CDF Sample Recovery .'........ 5-12
5.1.5 CDD/CDF Analytical Procedures ..:....'. 5-15
5.1.5.1 Preparation of Samples for Extraction ...:-.... 5-18
5.1.5.2 Calibration of GC/MS System 5-18
5.1.6 CDD/CDF Analytical Quality Control..-.." 5-18
5.1.6.1 CDD/CDF Quality Control Blanks, 5-19
5.1.6.2 Quality Control Standards and Duplicates . 5-20
5.1.7 Analytes and Detection Limits for Method 23 .V 5-21
5.2 Hydrochloric Acid/Particulate Matter Emissions Testing Using EPA
Method 26A 5-23
5.2.1 Method 26A Sampling Equipment .".. • '5-23
5.2.2 Method 26A Sampling Equipment Preparation 5-25
5.2.2.1 Glassware Preparation 5-25
5.2.2.2 Reagent Preparation 5-25
5.2.2.3 Equipment Preparation 5-26
5.2.3 Method 26A Sampling Operations 5-28
5.2.3.1 Preliminary Measurements 5-28
5.2.3.2 Assembling the Train 5-28
5.2.3.3 Sampling Procedures 5-29
5.2.4 Method 26A Sample Recovery 5-30
5.2.5 HC1 Analytical Procedures . 5-37
5.2.6 HC1 Analytical Quality Control 5-38
5.2.7 Particulate Analysis 5-38
5.2.8 Quality Control for Gravimetric Procedures 5-40
5.3 FTIR EPA Method 320 5-40
5.3.1 FTIR Sampling Equipment 5-40
5.3.2 Preparation for Sampling 5-43
5.3.3 Sampling. '. 5-45
5.3.4 FTIR Method Data Review, Validation, and Verification
Requirements 5-48
5.3.5 QC for the FTIR 5-51
IV
-------
Table of Contents (Continued)
Page
6.0 QUALITY ASSURANCE/QUALITY CONTROL 6-1
6.1 Sampling QC Results 6-1
6.1.1 .Leak Checks '.". '. ...6-1
6.1.2 Percent Isokinetics ..6-4
6.1.3 Meter Box Calibrations 6-5
6.1,4 Field Blank Results 6-5
6.1.5 FTIR Sampling Quality Control 6-7
6.2 Analytical Quality Control Results 6-9
6.2,1 D/F Analytical Quality Control 6-9
6.2.1.1 D/F Quality Control Blanks 6-9
6.2.1.2 Quality Control Standards 6-10
6.2.2 HC1 Analytical Quality Control 6-10
6.2.3 Quality Control for Gravimetric Procedures 6-11
6.2.4 FTIR Analytical Quality Control 6-11
-------
List of Figures
Page
2-1 FTIR System Response Profile (Measured on 7 December 1997) 2-40
4-1 El, Chip Dryer Baghouse Inlet 4-2
4-2 E2, Chip Dryer Baghouse Outlet 4-3
4-3 E3, Reverberatory Furnace #1 Baghouse Inlet 4-4
4-4 E4, Reverberatory Furnace #1 Baghouse Outlet 4-5
4-5 Chip Dryer Baghouse Inlet, Traverse Points 4-6.
4-6 Chip Dryer Baghouse Outlet, Traverse Points 4-7
4-7 Reverberatory Furnace #1 Baghouse Inlet Traverse Points 4-8
4-8 Reverberatory Furnace #1 Baghouse Outlet Traverse Points 4-9
5-1 Method 23 Sampling Train Configuration 5-2
5-2 Method 23 Field Recovery Scheme 5-13
5-3 Extraction and Analysis Schematic for Method 23 Samples- 5-17
5-4 Schematic of Method 26A Sampling Train 5-24
5-5 Method 26A Sample Recovery Scheme 5-34
5-6 Method 5 Preparation and Analysis Scheme (Integral Part of Method 26A) 5-39
5-7 FTIR Sampling and Measurement System 5-42
VI
-------
List of Tables (Continued)
Page
2-21 Summary of EPA Method 301 FTIR Validation Results for HC1 2-28
2-22 Chip Dryer FTIR HC1 Results, ppmv 2-30
2-23 Reverberatory Furnace #1 Baghouse FTIR HC1 Results During Charging, ppmv ... 2-30
2-24 Reverberatory Furnace #1 Baghouse FTIR HC1 Results During Tapping, ppmv .... 2-31
2-25 Combined Charging and Tapping Reverberatory Furnace #1 Baghouse FTIRHC1 .
Results, ppmv 2-32
2-26 Reverberatory Furnace #1 Baghouse FTIR HC1 Results - Grand Average, ppmv . . .2-32
2-27 Reverberatory Furnace #1 Hood Baghouse Outlet HC1 Results - Overnight, ppmv ... 2-33
2-28 Other Species Detected by FTIR - Chip Dryer Inlet 2-34
2-29 Other Species Detected by FTIR - Chip Dryer Outlet 2-35
2-30 Other Species Detected by FTIR - Reverberatory Furnace #1 Inlet 2-36
2-31 Other Species Detected by FTIR - Reverberatory Furnace #1 Outlet 2-38
2-32 Comparison of FTIR and Method 26A results for HC1, ppm 2-41
5-1 Method 23 Glassware Cleaning Procedure (Train Components, Sample Containers
and Laboratory Glassware) 5-4
5-2 CDD/CDF Sampling Checklist 5-9
5-3 Method 23 Sample Fractions Shipped To Analytical Laboratory 5-15
5-4 CDD/CDF Congeners To Be Analyzed 5-16
5-5 Method 23 Blanks Collected 5-19
5-6 Analytical Detection Limits For Dioxins/Furans 5-22
vm
-------
List of Tables (Continued)
Page
5-7 CDD/CDF Method Detection Limits 5-22
f
5-8 Glassware Cleaning Procedure (Method 26A Train Components) 5-26.
5-9 Sampling Checklist for EPA Method 26A 5-31
5-10. Typical FTIR Operating Parameters .5-45
5-11 Compounds for Which Reference FTIR Spectra Are Available in the ERG Spectral
Library 5-49
6-1 Summary of Dioxin/Furan Test Leak Check Results : 6-2
6-2 Summary of HC1/PM Test Leak Check Results 6-3
6-3 Summary of Isokinetic Percentages 6-4
6-4 Dry Gas Meter Post-Test Calibration Results 6-5
6-5 Method 26A Field Blank Analysis Results, ug Detected 6-6
6-6 Method 23 Field Blank Analysis Results, ng Detected 6-7
6-6 QC Spiking Results 6-13
6-7 HC1 Gas Standard Analysis Results 6-14
6-8 CO Gas Standard Analysis Results : 6-15
6-9 CH4, NOX, and CO2 Gas Standard Analysis Results 6-16
-------
1.0 INTRODUCTION
The purpose of this testing program was to obtain emissions data for uncontrolled and
controlled hydrochloric acid (HCl), paniculate matter (PM) and speciated hydrocarbon
Hazardous Air Pollutants (HAPs) from a secondary aluminum processing plant to support a
national emission standard for hazardous air pollutants (NESHAP).
The Gulp Aluminum Alloys facility in Steele, Alabama, is a secondary aluminum
reclamation facility. The Gulp facility accepts many different forms of scrap aluminum
feedstock, and operates a chip dryer to volatilize oils and lubricants from scrap aluminum chips
prior to the remelting operation. The chip dryer emissions are captured by closed hoods and are
ducted to a lime injected baghouse. There is a side-well reverberatory furnace that is used to
remelt, flux, and alloy aluminum scrap that has been pre-processed in the chip dryer operation in
addition to non-processed purchased aluminum scrap. The side-well reverberatory furnace
emissions are captured by a canopy hood located above the charging and refluxing side-well and
ducted to a lime injected baghouse. Emissions from the hearth stack are uncontrolled.
The existing total hydrocarbons (THC) emissions test data from secondary aluminum
smelting plants had not been speciated to determine HAP content. Additional data were needed
to identify HAPs emitted and their respective emission rates from melting furnace and chip
drying operations at secondary aluminum smelting plants. Also, information on the HCl, PM,
and dioxin/furan (D/F) removal efficiency of baghouses with dry lime injection was needed.
Source tests were required to quantify and characterize the HCl, PM, D/F, and HAP
emissions and to assess control device performance from chip drying and side-well reverberatory
furnace #1 operations, and to identify, quantify, and assess the performance of a lime injected
baghouse at two lime injection rates for HCl from the side-well reverberatory furnace #1
operations. Application of the following stationary source test methods was required to
adequately characterize these processes:
1-1
-------
• Determination of D/F using EPA Method 23;
Determination of HC1 and PM using EPA Method 26A and EPA Method 320; and
Screening for speciated hydrocarbon HAPs using EPA Method 320.
The objective of this work assignment was to perform all activities necessary to
characterize specified point sources for the parameters listed above. The facility selected for
testing, the Gulp Aluminum Alloys Plant located in Steele, Alabama, has lime injected baghouses
as control technology.
1.1 Objectives
The objective of the testing at the Gulp Aluminum Alloys facility, in Steele, Alabama,
was to perform all activities necessary to characterize the lime injected baghouses for the
following emission components:
• Determination of D/F using EPA Method 23;
Determination of HC1/PM using EPA Method 26A and EPA Method 320; and
• Screening for speciated hydrocarbon HAPs using EPA Method 320.
For the manual methods, testing was performed simultaneously at the inlet and outlet of
the chip dryer lime injected baghouse and simultaneously at the reverberatory furnace #1 lime
injected baghouse. FTIR testing was not simultaneous at inlet/outlet; the FTIR alternated
between inlet/outlet (for example, ten minutes inlet/ten minutes outlet). In addition, a day of
testing was performed using EPA Method 320 to identify, quantify, and assess the performance
of the lime injected baghouse associated with the reverberatory furnace #1 for HC1 removal at
two injection rates of lime. Two additional days were required to perform a Method 301
validation of FTIR for HC1: one day each for the two baghouses.
1-2
-------
1.2 Brief Site Discussion
The Gulp Aluminum Alloys Plant is located in Steele, Alabama, approximately 4 miles
south of Gadsden, Alabama. The plant is a secondary aluminum plant, primarily smelting
recycled aluminum. Gulp Aluminum Alloys primarily recycles aluminum parts to create a
secondary aluminum alloy which is used in cast aluminum. The plant operates 24 hours per day,
but the chip dryer process is down Monday from 7 AM to 4 PM, except for the furnaces.
The Gulp Aluminum Alloys Plant has two baghouses associated with the furnaces as
control devices: the first baghouse is the original one while the second is newer. The exhaust
stacks on both are approximately the same size. Furnace #1 and Furnace #2 differ in that
Furnace #2 has an additional exhaust from the sweat furnace. The sweat furnace is used to
separate plastic parts and metals of higher melting points from the aluminum prior to placing the
aluminum into the furnace.
1.3 Emissions Measurements Program
This section provides an overview of the emissions measurement program conducted at
the Gulp Aluminum Alloys Plant in Steele, Alabama. Included in this section are summaries of
the test matrix, sampling locations,.sampling methods, and laboratory analysis. Additional detail
on these topics are provided in the sections that follow.
1.3.1 Test Matrix
The sampling and analytical matrix that was performed at Gulp Aluminum Alloys is
presented in Table l-l, with the schedule that was followed in the field. Manual and Fourier
Transform Infrared (FTIR) instrumental emissions tests were performed, with detailed
descriptions of these sampling and analytical procedures provided in Section 5.0 of this
document.
1-3
-------
Table 1-1. Gulp Aluminum Alloys Facility (Steele, Alabama) Test Matrix
Industry: Secondary Aluminum
Process: Aluminum Chip Drying and Smelting
Sampling
Location
E2
Chip Dryer
Lime Injected
Baghouse
Outlet
E1/E2
Chip Dryer
Lime Injected
Baghouse
Inlet/Outlet
E3/E4
Reverberatory
Furnace #l
Lime Injected
Baghouse
E3/E4
Reverberatory
Furnace # 1
Lime Injected
Baghouse
E3/E4
Reverberatory
Furnace #1
Lime Injected
Baghouse
Inlet/Outlet
Runs/
Date
1 day
12/03/97
3
Run 1
12/05/97
Runs 2,3
12/06/97
1 day
12/07/97
1 day
12/07/97
6:
Run 1
12/08/97
Run 2
12/09/97
Run 3
12/10/97
Run 4
12/11/97
Sample Type
HC1 Validation
HC1/PM
Dioxins/Furans
All species
detected by FTIR1
HC1 Removal
efficiency study
HC1 Validation
HC1/PM
Dioxins/Furans
All species
detected by FTIR1
Reference
Method
Method 320
Method 26A
Method 23
Method 320
Method 320
Method 320
Method 26A
Method 23
Method 320
Sampling
Duration
4-8 hours
4 hours
4-8 hours
8-10
hours
4 hours
Analysis
Method
FTIR
Method 26A
Method 8290
Method 320
FTIR
FTIR
Method 26A
Method 8290
Method 320
Laboratory
ERG
Triangle Labs
Triangle Labs
ERG
ERG
ERG
Triangle Labs
Triangle Labs
ERG
' All species detected by FTIR includes all gaseous HAPs (i.e.. HC1), as well as criteria pollutants (i.e., NO,,
S0:, CO).
2Work Assignment Manager elected to perform four test runs in the field.
1-4
-------
1.3.2 Test Schedule
The daily test schedule is shown in Table 1-1. The test required one day of set-up at the
chip dryer lime injected baghouse, two test days at the inlet/outlet of the chip dryer lime injected
baghouse, one day of process operating parameter optimization using FTIR, and five test days at
the inlet/outlet of the reverberatory furnace #1 lime injected baghouse. One day was allowed as
contingency/tear-down. The facility did not operate on Mondays from 7 AM to 4 PM, except for
the furnaces; allowance was made for the plant schedule in the test schedule. Each test day was
12 to 16 hours in length. Set-up and tear-down days were 8 to 10 hours in length.
1.4 Test Report
This final report, presenting all data collected and the results of the analyses, has been
prepared in six sections and two volumes, as described below:
Section 1 provides an introduction to the testing effort and includes a brief
description of the test site and an overview of the emissions measurements
program;
Section 2 gives a summary of the test results for the PM, HC1, D/F tests, and the
FTIR results for HC1 and selected HAPs;
Section 3 provides a description of the process and plant operation during the field
test. These data are to be supplied by EPA through Research Triangle Institute to
be included at a later date;
Section 4 gives a discussion of the sampling locations;
Section 5 presents detailed descriptions of the sampling and analysis procedures;
and
Section 6 provides details of the quality assurance/quality control procedures used
on this program and the QC results.
The appendices containing copies of the actual field data sheets and the results of the
laboratory analyses are contained in Volume 2.
1-5
-------
2.0 SUMMARY OF RESULTS
This section provides the results of the emissions test program conducted at the Gulp
Aluminum Alloys plant from December 2 to December 11, 1997. Included in this section are the
results for the manual tests conducted for PM, HC1, CU, dioxin and furan and for the extractive
FTIR test conducted for HC1 and screening for selected HAPs. Testing was performed at the
inlet and outlet of the baghouse associated with the chip dryer and at the inlet and outlet of the
baghouse associated with the reverberatory furnace number 1.
2.1 Emissions Test Log
Twenty eight manual tests were performed over a nine day period (14 D/F and 14
HC1/PM). Table 2-1 presents the emissions test log which shows the test date, location, run
number, test type and run times for each method. Concurrent with the manual testing at each
location were extractive FTBR measurements for HC1.
Table 2-2 shows the volume of stack gas sampled for each run in dry standard cubic
meters (dscm) and Table 2-3 shows the stack gas volumetric flow rate during each run in dry
standard cubic meters per minute (dscmm). The percent relative standard deviation (%RSD)
calculated for the stack flow rates (shown in Table 2-3) was less than 10 % indicating that each
process flow was maintained at a fairly constant rate over the respective test days. All related
field data sheets are given in Appendix A.
2-1
-------
2.2 Dioxin/Furan Results
2.2.7 Overview
Three 4-hour D/F tests were performed at the inlet and outlet of the baghouse associated
with the chip dryer operation (total of 6) and four 6-hour tests were performed at the inlet and
outlet of the baghouse associated with the reverberatory furnace number 1 (total of 8). The
sampling and analysis procedures followed EPA Method 23 protocol. All results except for the
2,3,7,8-tetrachlorodibenzofuran (2,3,7,8-TCDF) were determined by high resolution gas
chromatography (HRGC)/high resolution mass spectrometry (HRMS) using a DB-5 capillary gas
chromatographic column. The 2,3,7,8-TCDF was determined by HRGC/HRMS using a DB-225
column which gives improved chromatographic resolution for this compound over the DB-5 and
thus a more accurate quantitation. Any compound that was not detected is reported as a "less
than" value with this value being the instrument detection limit. A "less than" value rather than a
"0" is used in all appropriate calculations. All D/F raw data can be found in Appendix B of this
report.
2.2.2 Dioxin/Furan Emission Results
Chip Drver
Tables 2-4 and 2-5 present the concentration, in nanograms per dry standard cubic meter
(ng/dscm), of the selected D/F congeners by run number, the average concentration over the three
runs and the %RSD for the chip dryer inlet and outlet, respectively. These values were
calculated by dividing the reported analytical results, in ng, by the appropriate sample volume
collected, in dscm, from Table 2-2. As indicated in Table 2-4 (dryer inlet), the concentration
values of several congeners in Runs 1 and 2 are presented as "greater than" values and should be
considered estimates. The amount of these analytes detected in the sample extracts exceeded the
calibration curve. The observed concentrations for Run 3 are generally lower by a factor of two
than those observed for Runs 1 and 2, causing the %RSDs for most analytes to be in the 40 to
2-5
-------
50 range. The fact that different feed stocks or combinations of feed stocks were used for each of
the runs is the most probable explanation for this. The feed stock for Run 1 was continuous
during the run. The feed stock for Run 2 was the remainder of the feed stock used during Run 1
(depleted after approximately the first half of Run 2) plus a portion of a new feed stock of
different material and different oily coating. The feed stock for Run 3 was a combination of the
remainder of the second feed stock from Run 2 plus a third feed stock material with yet another
different oily coating. Each lot of feed stock material used during the testing was added to the
loading hopper as needed until it was depleted, followed by the next lot until it was depleted and
so on. Each lot of material was processed as a discrete material type and oily coating with no
mixing or blending of the three lots. Table 2-5 (dryer outlet) shows concentrations considerably
lower than the inlet for Runs 1 and 2, whereas for Run 3 the inlet and outlet values are similar.
The %RSDs generally in the 20 to 30 range still reflect the use of three different lots of feed
stock.
Table 2-6 shows the D/F stack emission rate from the chip dryer outlet in micrograms of
analyte per megagram (jag/Mg) of feed stock for each of the three runs, the average and the
%RSD. These values were calculated using standard conversion factors (i.e., pounds to grams)
and from the concentrations given in Table 2-5, the stack flow rates given in Table 2-3 and the
number of pounds of each feed stock consumed during the test period as supplied by the facility.
The latter data set (pounds of feed stock consumed) for each of the three runs was not a
straightforward calculation. Mitigating factors included:
• Each lot of feed was processed at a different rate;
• Combinations of feed stock were used during two of the runs; and
• Two of the feed stocks were processed beginning on one day, finishing on the
next day with the process shut down over night.
For run number one a single lot of feed stock was used, but it was processed over a two day
period (32,000 pounds in 8 hours on the first day during Run 1 and 4,740 pounds in 3.5 hours on
the next day during the first part of Run 2). The feed rate of feed stock consumed during Run 1
2-8
-------
was therefore calculated by dividing 32,000 by 8. The same logic was followed for Runs 2 and
3, except that two different lots were used during each run and the average feed rate was
therefore determined. The feed rate calculations are summarized below:
Run No.
1
2
2
3
3
Lot
1
1
2
2
3
Feed Time-Date
8 hrs- 12/5/97
3. 5 hrs- 12/6/97
8 hrs- 12/6/97
8 hrs- 12/6/97
2 hrs- 12/6/97
Pounds of Feed
32,000
4,740
20,500
20,500
7,000
Feed Rate
4,000 Ibs/hr
1,354
2,563
2,563
3,500
Avg. Feed Rate. Ibs/hr
4,000
1,959
3,032
Table 2-7 shows the D/F congener concentrations in ng/dscm converted to 2,3,7,8-TCDD
toxicity equivalents as well as a summation of the values presented as total chlorinated dioxins
and total chlorinated furans.
Reverberatorv Furnace #1
A total of four tests was performed collecting samples simultaneously at the inlet and
outlet of the baghouse associated with furnace number 1. Each test was performed over the
duration of a batch cycle starting at the time of the first furnace charge and ending at the time of
the last tap out, a period ranging from approximately five and one-half hours to six and one-half
hours. The same product was produced during each of the four tests. Each batch followed a
three stage process: charging, mixing and tap-out. Charging required approximately four hours
to complete, mixing one hour and tap-out one hour. The highest emissions were observed during
the charging process (as observed from the real time FTIR data for HC1). A "front-end loader"
Caterpillar tractor was used to charge feed stock or flux to the furnace approximately every ten
minutes during the charging stage. As each load was added emissions were visible in the form of
clouds of black smoke/soot which were captured by an overhead hood and directed to the
baghouse.
2-10
-------
Table 2-7. (Continued)
Congener
OCDD
Total PCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1. 2.3.4,6.7. 8-HpCDF
1.2.3,4,7,8,9-HpCDF
OCDF
Total PCDF
2,3,7,8
TCDD
TEF1
0.001
0.1
0.05
0.5
0.1
0.1
0.1
0.1
0.01
0.01
0.001
ng/dscm
Runl
0.00114
1.76
0.94
12.1
1.53
0.701
0.438
0.0242
0.0416
0.00498
0.000605
Run 2
0.000493
0.862
0.538
7.22
0.954
0.421
0.273
0.0122
0.0237
0.00257
0.000270
Run 3
0.000455
0.993
0.656
8.90
1.23
0.573
0.332
0.0161
0.0287
0.00266
0.000255
Average
0.000696
2.44
1.20
. 0.710
9.40
1.24
0.565
0.348
0.0175
0.0313
0.00340
0.000377
13.5
'Toxicity Equivalence Factor
Tables 2-8 and 2-9 present the concentration, in ng/dscm, of the selected D/F congeners
by run number, the average concentration over the three runs and the %RSD for the reverberatory
furnace No. 1 inlet and outlet, respectively. These values were calculated by dividing the
reported analytical results, in ng, by the appropriate sample volume collected, in dscm, from
Table 2-2. As indicated in Table 2-8 (furnace inlet) the concentration value of the
octachlorofuran in Run 2 is presented as a "greater than" value and should be considered an
estimate. The amount of this analyte detected in the sample extract exceeded the calibration
curve.
2-12
-------
The observed concentrations for the four runs at the inlet are generally of the same
magnitude as indicated by the low %RSDs. Table 2-9 (furnace outlet) shows the concentrations
to be considerably lower than those at the inlet by a factor of 10 to 100. Several of the analytes
exhibited a concentration level below the calibration curve, less than 5 times the detection limit
or not detected. These factors contribute to the high %RSD observed, not unusual in this
situation.
Table 2-10 shows the D/F stack emission rate from the furnace number 2 outlet in
jnicrograms of analyte per megagram (ug/Mg) of feed stock for each of the four runs, the average
and the %RSD. These values were calculated using standard conversion factors (i.e., pounds to
grams), the concentrations given in Table 2-9, the stack flow rates given in Table 2-3 and the
number of pounds of feed stock consumed during the test period as supplied by the facility.
Although the feed stock was added only during the first four hours of each batch, the feed rate
was calculated using the total pounds consumed divided by the length of the total batch process.
This calculation process was necessary to correspond with the emissions collected by the
integrated sample over the duration of the entire batch process including charging, mixing and
tap-out. The latter data set (pounds of feed stock consumed) for each of the four runs is given
below:
Run No.
1
2
3
4
Lot
Batch Time-Date
1 6 hrs-12/8/97
2 6.5 hrs-12/9/97
3 5.75 hrs-12/10/97
4 6.5 hrs-12/11/98
Feed Consumed. Ibs.
70,200
70,200
75,600
81,000
Feed Rate. lbs./hr
11,700
10,800
13,148
12,462
Table 2-11 shows the congener concentrations in ng/dscm converted to 2,3,7,8-TCDD
toxicity equivalents as well as a summation of the values presented as total chlorinated dioxins
and total chlorinated furans.
2-15
-------
Table 2-11. (Continued)
Congener
1,2,3,4,6,7,8-HpCDD
OCDD
Total PCDD
2,3,7.8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7, 8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1, 2,3.7, 8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1.2,3,4,7,8.9-HpCDF
OCDF
Total PCDF
2,3,7,8-
T/T\rfc
1CUU
TEF1
0.01
0.001
0.1
0.05
0.5
0.1
0.1
0.1
0.1
0.01
0.01
0.001
Run 1
0.00166
0.000249
0.0115
0.00630
0.111
0.0485
0.0180
0.0235
0.00125
0.00665
0.00120
0.000554
Run 2
0.000228
0.000038
0.00811
0.00206
0.0284
0.00768
0.00299
0.00327
0.000142
0.000967
0.000156
0.000171
ng/dscm
Run 3
0.000173
0.000023
0100993
0.00273
0.0367
0.00806
0.00302
0.003' 17
0.000144
0.000590
0.000072
0.000035
Run 4
0.000198
0.000032
0.00356
0.000989
0.0145
0.00580
0.00198
0.00264
0.000264
0.000818
0.000106
0.000061
Average
0.000565
0.0000856
0.0146
0.00827
0.00302
0.0476
0.0175
0.00650
0.00816
0.000449
0.00226
0.000385
0.000205
0.0944
'Toxicity Equivalence Factor
2.3 HCI Results
2.3.7 Overview
Three 4-hour HC1/C1-, tests were performed at the inlet and outlet of the baghouse
associated with the chip dryer operation (total of 6) and four 6-feour tests were performed at the
inlet and outlet of the baghouse associated with the reverberatory furnace number 1 (total of 8).
The sampling and analysis procedures followed EPA Method 26A protocol Prior to testing, the
plant personnel replaced all fabric filters in the baghouse with new ones and performed the
appropriate leak checks. All analyses were performed by ion chromatography using the samples
as received from the field. Any compound that was not detected is reported as a "less than"
2-18
-------
value with this value being the instrument detection limit. A "less than" value rather than a "0" is
used in all appropriate calculations. All HC1/C1, raw data can be found in Appendix C of this
report.
2.3.2 HCI Emission Results
Chip Dryer
The baghouse associated with the chip dryer is injected with lime (hydrated calcium
hydroxide) for the purpose of reducing HCI emissions. The reaction between the two compounds
forms calcium chloride and water. The lime injection to the baghouse was continuous at a feed
rate of approximately 50 pounds per hour. Table 2-12 gives the concentration, in micrograms per
dry standard cubic meters (^g/dscm), the average concentration over the three runs and the
%RSD for the inlet and outlet, respectively. The results for Run 3 inlet are invalid as the sample
was compromised during sample recovery in the field. Chlorine was not detected (at the
instrument detection limit) in any samples at either the inlet or the outlet. The HCI results for
Runs 1 and 2 inlet and Runs 1 and 2 outlet are very consistent among themselves with the outlet
concentrations representing about 3% of the amount entering the baghouse. Table 2-13 gives the
concentrations in parts per million (ppm) in order to provide an easy comparison to the FTIR
results which are also presented in ppm and provided in Section 2.5 of this report.
The emission rate of HC1/C12, in pounds/hour (Ibs/hr), was calculated using the
concentration results from Table 2-12 and the stack flow rate data from Table 2-3 and is
presented in Table 2-14. Using the average emission rates calculated for the inlet and the outlet,
a baghouse percent removal efficiency for HCI was determined to be 96.9%, as shown in
Table 2-15. The emission rate of HC1/CU was also determined as pounds per ton of feed stock
using the data given in Table 2-14 and the feed stock feed rates for the chip dryer given in
Section 2.2.2 above. These results are given in Table 2-16.
2-19
-------
Table 2-12. HCI and CI2 Concentration, |jg/dscm
Location
Chip Dryer Inlet1
Chip Dryer Outlet
Furnace 1 Inlet
Furnace 1 Outlet
Parameter
HCI
Cl,
HCI
Cl,
HCI
Cl,
HCI
Cl,
Runl
43704
<191
1367
<123
119887
188*
689
<66.2
Run 2
37254
<198
1899
<137
119768
4305
764
129*
Run 3
6102
<179
202
<168
66034
783
2379
<62.4
Run 4
NA
NA
NA
NA
109455
231*
1262
<45.6
*Less than 5 x MDL
'Run 3 compromised during sample recovery
Table 2-13. HCI and CI2 Concentration, ppm
Location
Chip Dryer Inlet1
Chip Dryer Outlet
Furnace 1 Inlet
Furnace 1 Outlet
Parameter
HCI
Cl:
HCI
C!2
HCI
Cl,
HCI
Cl,
Runl
29.6
<0.067
0.927
<0.043
81.3
0.066*
0.467
<0.023
Run 2
25.3
<0.069
1.288
<0.048
81.2
1.50
0.518
0.045*
Run 3
4.14
0.062
0.137
<0.058
44.8
0.273
1.61
<0.022
Run 4
NA
NA
NA
NA
74.2
0.081*
0.856
<0.016
*Less than 5 x MDL
'Run 3 compromised during sample recovery
2-20
-------
Table 2-14. HCI and Cl, Emission Rate, Ibs/hour
Location
Chip Dryer Inlet'
Chip Dryer Outlet
Furnace 1 Inlet
Furnace 1 Outlet
Parameter
HCI
C12
HCI
C12
HCI
C12
HCI
Cl,
Runl
0.820
<0.00359
0.0276
<0.00249
11.4
0.0179*
0.0760
<0.00731
Run 2
0.798
<0.00423
0.0429
<0.00310
10.5
0.379
0.0760
0.0128*
Run 3
0.115
<0.00338
0.00424
<0.00352
5.88
0.0698
0.227
<0.00596
Run 4
NA2
NA
NA
NA
8.38
0.0177*
0.112
<0.00407
Average
0.809
0.00391
0.0249
0.00304
9.05
0.121
0.123
0.00754
%RSD
NA
NA
78.1
17.1
27.3
143.4
58.3
50.0
*Less than 5 x MDL; should be considered an estimate
'Run 3 compromised during sample collection; Runs 1 and 2 used to calculate average
2NA=Not Applicable
Table 2-15. HCI Removal Efficiency
Location
Chip Dryer
Furnace #1, Cond. l'
Furnace #l,Cond. 22
Average Emission Rate, Ibs/hour
Inlet
0.809
10.97
7.13
Outlet
0.0249
0.0760
0.170
Removal
Efficiency, %3
96.9
99.3
97.6
Condition 1 = continuous lime feed, Runs 1 and 2
Condition 2 = 50 Ibs. lime every 2 hours, Runs 3 and 4
'Average of runs 1 and 2
2Average of runs 3 and 4
3Removal Efficiency = (inlet-outlet/inlet) x 100
2-21
-------
Table 2-16. HCI and CI2 Emission Rate, Ibs/Ton of Feed
Location
Chip Dryer Inlet'
Chip Dryer Outlet
-urnace 1 Inlet
Furnace 1 Outlet
Parameter
HCI
C12
HCI
C12
HCI
C12
HCI
Clr
Runl
0.410
0.00180
0.0138
0.00124
1.95
0.00305
0.0130
0.00125
Run 2
0.814
0.00432
0.0438
0.00317
1.95
0.0702
0.0141
0.00238
Run 3
0.0759
0.00222
0.00279
0.00232
0.895
0.0106
0.0346
0.000908
Run 4
NA2
• NA
NA
NA
1.34
0.00284
0.0180
0.000653
Average
0.612
0.00306
0.0201
0.00224
1.54
0.0217
0.0199
0.00130
%RSD
NA
NA
105
42.9
33.5
150
50.3
58.7
'Run 3 compromised during sample collection, Runs 1 and 2 used to calculate average
2NA, Not Applicable
Reverberatorv Furnace Number 1
The results for the reverberatory furnace #1 are given in Tables 2-12 through 2-16
following the same sequence as the chip dryer. During Test Runs 1 and 2, lime was fed
continuously to the baghouse (Condition 1). During Test Runs 3 and 4, lime was added to the
lime feed hopper at the rate of one 50 Ib bag every two hours (Condition 2). Lime was consumed
at the rate of approximately 50 pounds per 30 minutes during the test period. The concentration
results presented in Tables 2-12 and 2-13 for HCI for Runs 1 and 2 are consistent among
themselves for both the inlet and outlet. Run 4 inlet results were consistent with Runs 1 and 2.
However, the outlet results were approximately a factor of 2 higher than for Runs 1 and 2. The
fact that one of the four baghouse modules (module 4) had developed a leak and was off-line
could be a possible explanation for this observation. The Run 3 inlet HCI concentration was
observed to be approximately half that for the other runs, possibly because furnace C12 flow
supply was not turned on until at least an hour into the test.
2-22
-------
The baghouse removal efficiency for HC1 was determined for Condition 1 using the
average of the emission rate results from Runs 1 and 2 and for Condition 2 using the average of
Runs 3 and 4. The results are presented in Table 2-15. The removal efficiency for Condition 2
was slightly less than that for Condition 1, with both well above 95%. The emission rate of
HC1/C12 was also determined as pounds per ton of feed stock using the data given in Table 2-14
and the feed stock feed rates for the furnace given in Section 2.2.2, above. These results are
given in Table 2-16.
2.4 Participate Results
2.4.7 Overview
Paniculate matter emissions were determined from the same sampling trains used for the
determination of HC1 emissions. PM collected on the filter and in the front half acetone rinse
(nozzle, probe, front-half filter holder) was analyzed gravimetrically. PM stack concentrations in
grains per dry standard cubic meter (gr/dscm), PM emission rate in pounds per ton of feed
(Ibs/Ton) and pounds per hour (Ibs/Hr), and the PM removal efficiency of each baghouse as a
percent (%) for the chip dryer and furnace number 1 operations are presented below. The results
of the PM testing are presented in Tables 2-17 through 2-20. All raw data for the PM
determinations can be found in Appendix D.
2.4.2 Particulate Emission Results
Chip Dryer
Table 2-17 gives the concentration, in gr/dscm, the average concentration over the three
runs and the %RSD for the inlet and outlet. The average of the three runs was 20.3 and 0.778 for
the inlet and outlet, respectively.
2-23
-------
Table 2-20. Particulate Matter Emission Rate, Ibs/Ton of Feed
Baghouse Location
Chip Dryer Inlet
Chip Dryer Outlet
*urnace 1 Inlet
•urnace 1 Outlet
Ibs/ton of Feed
Run 1
16.9
1.35
7.73
0.173
Run 2
27.3
0.791
5.35
0.0289
Run 3
11.190
0.982
2.82
0.00970
Run 4
NA
NA
3.07
0.00555
Average
18.5
1.04
4.74
0.0543
%RSD
44.3
27.5
48.3
147
The emission rate of PM, in Ibs/hr, was calculated using the concentration results from
Table 2-17 and the stack flow rate data from Table 2-3 and is presented in Table 2-18. Using the
average emission rates calculated for the inlet and the outlet, a baghouse percent removal
efficiency for PM was determined to be 93.6%, as shown in Table 2-19. The emission rate of
PM was also determined as pounds per ton of feed stock using the data given in Table 2-18 and
the feed stock feed rates for the chip dryer given in Section 2.2.2 above. These results are given
in Table 2-20.
Reverberatorv Furnace Number 1
Table 2-17 gives the concentration, in gr/dscm, the average concentration over the four
runs and the %RSD for the inlet and outlet. The average of the four runs was 4.68 and 0.0455 for
the inlet and outlet respectively. The inlet PM concentrations for Runs 1 and 2 (condition 1) are
noticeably higher than for Runs 3 and 4 (condition 2), possibly due to the lower lime injection
rate that occurred during Runs 3 and 4. The high variability between the outlet results is due to
the low mass of PM present on the filters. Values near the limit of detection have inherent
increased variability.
The emission rate of PM, in Ibs/hr, was calculated using the concentration results from
Table 2-17 and the stack flow rate data from Table 2-3 and is presented in Table 2-18. Using the
2-25
-------
average emission rates calculated for the inlet and the outlet, a baghouse percent removal
efficiency for PM was determined to be 98.9%, as shown in Table 2-19. The emission rate of
PM was also determined as pounds per ton of feed stock using the data given in Table 2-18 and
the feed stock feed rates for furnace number 2 given in Section 2.2.2 above. These results are
given in Table 2-20.
2.5 FTIR Results
2.5.1 Overview
FTIR data for HCl and other species were collected at the inlet and outlet of the
.baghouses associated with the chip dryer and reverberatory furnace 1. FTIR data collection was
synchronized with manual HCl and dioxin/furan testing to allow semi-quantitative comparison of
the FTIR and manual HCl results. Due to partitioning of FTIR analysis time between
unconditioned and conditioned inlet/outlet samples, only 25% of FTIR data during a given run on
the chip dryer and 38% on the furnace were collected simultaneously with the corresponding
inlet or outlet manual train sampling.
FTIR data were collected at each location by alternating sample analysis between inlet
and outlet every 10 minutes. Both inlet and outlet sampling systems continuously withdrew
sample from their respective location. Each 10 minute measurement period contained ten 1
minute average data points. The first two data points from each period were discarded to
eliminate data for samples containing both inlet and outlet sample gas. Two data points
correspond to the measured response time of the complete FTIR sampling and analysis system
(see below for details on measurement of system response time) A 1 minute average data point
is generated by analysis of a composite spectrum consisting of an average of 43 FTIR spectra
collected over the 1 minute time period.
Section 2.1 gives the schedule of the tests performed at the Gulp facility. Both
unconditioned samples and conditioned samples were analyzed. Conditioned samples were
2-26
-------
generated by passing the raw sample gas through a water vapor/carbon dioxide scrubbing system
(See Section 5.3 for details). Unconditioned and conditioned samples extracted from the chip
dryer baghouse were measured during the first and last two-hour periods for each four hour run,
respectively. At the reverberatory furnace #1, the sampling order went as follows: 2 hours
unconditioned, 1 hour conditioned, and 2 hours unconditioned. Two unattended unconditioned
overnight runs were also conducted to look continuously at reverberatory furnace #1 hood
baghouse outlet emissions. Those results are reported in Section 2.5.2.2.
Baghouse removal efficiency for HC1 was measured from the inlet/outlet data from each
location and is reported in Section 2.5.2.2. Optimization of the reverberatory furnace 1 baghouse
for HC1 removal was also carried out. The removal efficiency was found to exceed 90% for all
tests at all lime injection rates tested.
EPA Method 301 validation tests for HC1 were carried out on the chip dryer baghouse
outlet, and reverberatory furnace #1 baghouse inlet and outlet. In all three tests, the Method 301
statistical calculations showed that the FTIR method demonstrated acceptable precision and no
statistically significant bias for HC1. Details of the validation results can be found in
Section 2.5.2.1.
A comparison of the FTIR and Method 26A results for both the chip dryer and furnace
tests are presented in Section 2.5.2.6
2.5.2 FTIR Emission Results
This section contains the FTIR EPA Method 301 HC1 validation results, HC1 test results,
and screening results for the chip dryer and reverberatory furnace #1 hood baghouse inlet and
outlet. Also included are results for the reverberatory furnace #1 hood baghouse HC1 removal
efficiency optimization tests.
2-27
-------
2.5.2.1 EPA Method 301 FTIR Validation Results for HCI
EPA Method 301 validation testing for HCI was performed on the chip dryer outlet, and
reverberatory furnace #1 hood inlet/outlet. The spiking procedure is given in Section 5.3.2. Five-
minute measurement periods were used for the chip dryer outlet, while 1-minute measurement
periods for both inlet and outlet of the reverberatory furnace #1 were used. The 1-minute periods
were used because of the rapidly fluctuating nature of the furnace emissions. Table 2-21
summarizes the validation results.
Table 2-21. Summary of EPA Method 301 FTIR Validation Results for HCI
Location
Chip Dryer Outlet
Furnace 1 Inlet
Furnace 1 Outlet
Date
12/03/97
12/07/97
12/07/97
Spiked/Unspiked
Precision
Acceptable?
Yes/Yes
Yes/Yes
Yes/Yes
Statistically
Significant
Bias?
No
No
No
Note: Acceptable precision is equal to or less than 50% RSD.
Detailed results of the validation testing can be found in Appendix E.
2.5.2.2 FTIR HCI Test Results
The estimated FTIR HCI detection limit for this study is 0.05 ppmv.
While it is instructive to compare HCI results from both FTIR and manual methods, care
must be taken in interpreting the two sets of results. The FTIR system measured HCI at a given
inlet or outlet only 25 % of the time; the corresponding manual method was integrated over the
entire sampling period. Half of the FTIR instrument analysis time was split equally between inlet
and outlet as unconditioned and conditioned samples. Since HCI was measured only in
2-28
-------
unconditioned samples, this sampling scheme results in a 25% duty cycle for the total run for
HC1 measurement at a given inlet or outlet. The potential difference between FTIR and manual
results will increase with greater fluctuations in the HC1 concentration during the run, since the
FTIR captures 25% of the manual method sample for a given inlet or outlet run. Greatest
fluctuation in HG1 was observed during charging operations on the furnace #1 inlet to the
baghouse.
Results given below are organized by location. HC1 removal efficiency was also
calculated for each run.
Chip Dryer Baghouse Outlet/Inlet HC1 Results—Table 2-22 gives a summary of the
chip dryer baghouse outlet/inlet FTIR HC1 results. The average inlet concentrations were
consistent between runs, but the outlet concentrations varied by a factor of 10.
During Run 1, a large slug of particulate matter filled the FTIR inlet heated filter
assembly which prevented sampling of the inlet gas. The FTIR system was allowed to measure
the outlet while the inlet filter system was cleaned; thirty more data points were therefore
measured on the outlet versus the inlet. These extra 30 data points were reported in the
preliminary data, but they are not included in the results presented in Table 2-22. The removal of
the extra 30 data points does not cause any significant changes in the Run 1 results, however.
Reverberatory Furnace 1 Baghouse Outlet/Inlet HC1 Results—Table 2-23 gives the
FTIR HC1 results for the reverberatory furnace baghouse inlet and outlet during charging of the
furnace with scrap aluminum. Table 2-24 shows the FTIR HC1 results for the reverberatory
furnace #1 hood baghouse inlet and outlet during tapping operations. In all cases, HC1 removal
efficiency due to the lime-injected baghouse was greater than 90 percent.
2-29
-------
Table 2-22. Chip Dryer FTIR HCI Results, ppmv
Date
Time
Location
Average
SD
Maximum
Minimum
NDP
RE
Runl
12/05/97
0800 - 0900
0930 - 1130
inlet
8.91
6.42
22.89
2.11
72
outlet
0.65
0.54
2.54
0.10
72
92.7
Run 2
12/06/97
0835 - 1040
inlet
8.25
11.67
52.05
1.22
48
outlet
5.30
4.17
19.28
1.16
48
35.8
Run 3
12/06/97
1546 - 1746
inlet
6.79
4.44
20.40
0.77
48
outlet
2.42
2.72
13.37
0.86
48
64.4
SD - Standard Deviation
NDP - Number of data points measured
RE- Removal Efficiency in percent: 100 X (Avg. inlet- Avg. outlet)/Avg. inlet
Table 2-23. Reverberatory Furnace #1 Baghouse FTIR HCI Results During
Charging, ppmv
Date
Time
Location
Average
SD
Maximum
Minimum
NDP
RE
Run 1
12/08/97
945 - 1200
inlet
136.94
145.00
645.4
9.80
51
outlet
5.20
4.80
21.50
0.73
56
96.2
Run 2
12/09/97
1220-1420
inlet
58.48
122.37
756.72
7.59
48
outlet
2.72
1.15
6.76
1.14
48
95.3
Run 3
12/10/97
1114-1334
inlet
42.27
71.67
330.79
4.07
56
outlet
3.64
1.65
9.40
1.59
56
91.4
Run 4
12/11/97
0618 - 0848
inlet
132.42
159.55
634.60
12.25
64
outlet
4.57
3.46
14.39
1.36
56
96.6
SD - Standard Deviation
NDP - Number of data points measured
RE-Removal Efficiency in percent: 100 X (Avg. inlet- Avg. outlet)/Avg. inlet
2-30
-------
Table 2-24. Reverberatory Furnace #1 Baghouse FTIR HCI Results During
Tapping, ppmv
Date
Time
Location
Average
SD
Maximum
Minimum
NDP
RE
Runl
12/08/97
inlet
57.95
19.84
89.16
.13.83
56
outlet
2.17
0.66
3.85
1.30
64
96.3
Run 2
12/09/97
1555 - 1825
inlet
54.54
34.67
155.58
0.93
64
outlet
1.96
0.68
3.85
1.06
56
96.4
Run 3
12/10/97
1430 - 1710
inlet
46.84
21.47
84.51
2.27
64
outlet
1.59
0.48
3.07
0.94
64
96.6
Run 4
12/11/97
0958 - 1258
inlet
41.09
15.57
63.45
0.94
72
outlet
1.58
0.58
3.59
0.72
72
96.2
SD - Standard deviation
NDP - Number of data points measured
RE-Removal Efficiency percent: 100 X (Avg. inlet- Avg. outlet)/Avg. inlet
Tables 2-23 and 2-24 clearly show that the respective inlet and outlet concentrations
during charging are somewhat higher on average than during tapping. This result is expected,
due to the nature of the loading process, where hydrocarbons from oils coated on the charge
material provide the source of hydrogen for HCI production. Tapping operations do not involve
the addition of any material to the furnace, so the HCI levels would be expected to be lower.
Further examination of the data shows that the standard deviation of HCI inlet and outlet
levels during loading is significantly higher than during tapping. This variation stems from the
greater variation in the HCI emissions during loading due to the periodic addition of hydrocarbon
material to the furnace. During tapping operations, the furnace is not charged, and less variation
is expected.
Tables 2-25 and 2-26 are the combined loading and tapping results and a grand average of
all 4 runs, respectively. The combined results were generated by an average of the respective
2-31
-------
Table 2-25. Combined Charging and Tapping Reverberatory Furnace #1
Baghouse FTIR HCI Results, ppmv
Date
Location
Average
RE
Run 1
12/08/97
Inlet
95.60
Outlet
3.58
96.25
Run 2
12/09/97
Inlet
56.23
Outlet
2.31
95.89
Run 3
12/10/97
Inlet
44.71
Outlet
2.55
94.30
Run 4
12/11/97
Inlet
84.07
Outlet
2.89
96.56
RE- Removal Efficiency in percent: 100 X (Avg. inlet- Avg. outlet)/Avg. inlet
Table 2-26. Reverberatory Furnace #1 Baghouse FTIR HCI Results -
Grand Average, ppmv
Location
Average
RE
Inlet
70.15
Outlet
2.83
95.96
RE- Removal Efficiency in percent: 100 X (Avg. inlet- Avg. outlet)/Avg. inlet
data in Tables 2-23 and 2-24 weighted by the number of sample points. Computation of the
grand average was a simple unweighted average of the 4 runs.
Table 2-27 gives the FTIR HCI results of the unconditional reverberatory furnace 1
baghouse outlet during two overnight periods.. Five minute averages were collected for each data
point, instead of the usual 1 minute average collected in all other tests.
2.5.2.3 FTIR Process Optimization
The reverberatory furnace #1 hood baghouse HCI destruction efficiencies were measured
as a function of lime injection rate. Examination of Table 2-23 shows there is no apparent effect
of lime injection rate on the measured removal efficiency. Runs 1 and 2 utilized a continuous
lime injection at a rate of 50 Ibs per half hour. Runs 3 and 4 examined the emissions during a
lime
2-32
-------
Table 2-27. Reverberatory Furnace #1 Hood Baghouse Outlet HCI Results
Overnight, ppmv
Date
Time
Location
Average
Standard
Deviation
Maximum
Minimum
Number of
Data Points
Runl
12/(09-10)/97
1947 - 1015
Outlet
0.40
0.44
2.09
0.00
174
Run 2
12/(10-ll)/97
1815-0415
Outlet
0.45
0.48
2.60
0.00
120
injection rate of 50 Ibs per half hour period with 50 Ib being added every 2 hours. In all cases,
90+ percent HCI removal efficiency was obtained.
2.5.2.4 FTIR Screening Results
Screening data for species other than HCI were collected concurrently with the HCI data.
FTIR spectral data were examined for any other species present in the samples. Conditioned
samples were measured to estimate concentrations of aromatic and some hydrocarbon species.
Unconditioned samples were analyzed for other hydrocarbon and criteria species.
Tables 2-28 and 2-29 give summary statistics on the dominant species detected besides
HCI for the chip dryer inlet and outlet, respectively. Tables 2-30 and 2-31 are the screening
results for the furnace 1 inlet and outlet, respectively. In addition to HAP species, non-HAP
species are also reported to aid in understanding of the process chemistry, if desired.
2-33
-------
Table 2-28. Other Species Detected by FTIR - Chip Dryer Inlet
2
1
2
u/c
Average
Std.
Dev.
Max.
Min.
NDP
EDL
8
0>
W
c
5.97
4.25
17.15
<0.2
144
0.2
•*•*
C
0.86
0.60
2.03
0.11
144
0.05
V
g
i
u
CO
C
0.74
0.47
1.87
<0.1
144
O.I
•
g
.c
Ol
s
C
3.51
4.00
18.46
<0.2
144
0.2
u
•a
j;
2
u
0
ta.
U
3.12
8.63
59.64
0.25
168
0.1
u
•a
JS
ai
•d
2
u
"*'•
U
2.49
9.77
56.14
<0.5
168
0.5
'£-
O
(J
U
1.66
0.39
2.48
0.04
168
0.04
0
U
U
184.47
90.81
391.87
49.14
168
0.08
0
U
13.22
4.52
23.95
<3.5
168
3.5
O
z
u
4.16
4.67
14.63
<0.8
168
0.8
33
U
•U
12.08
16.15
125.62
4.45
168
2.0
q,
u
4.53
1.94
10.32
<0.8
168
0.8
+'
(j
U
1.99
5.81
33.32
<0.1
168
O.I
^
•— •
O
£
U
6.86
1.65
10.44
3.18
168
0.0001
to
All values are estimated ppmv, except CO2 and H2O in percent
Statistics of three runs combined
U/C - Unconditioned (U) or Conditioned (C) Sample
C4+ - Total aliphatic hydrocarbons larger than 3 carbons (ppmv hexane equivalent)
NDP - Number of data points
EDL - Estimated detection limit for spectral region used for analysis
-------
Table 2-29. Other Species Detected by FTIR - Chip Dryer Outlet
Parameter
U/C
Average
Std. Dev.
Max.
Min.
NDP
EDL
Ethylene
C
5.99
4.05
17.50
0.42
142
0.2
Acetylene
C
0.87
0.59
2.19
0.09
142
0.05
Benzene
C
0.76
0.48
2.06
<0.1
142
0.1
Methanol
C
3.45
4.59
20.84
<0.2
142
0.2
Formaldehyde
U
1.35
0.76
4.65
0.37
198
O.I
Acetaldehyde
U
0.49
0.62
4.39
<0.5
198
0.5
2
6'
u
u
1.64
0.27
2.35
0.89
198
0.04
O
U
u
174.31
84.61
355.41
8.41
198
0.08
O
z
u
14.49
3.09
22.53
8.37
198
3.5
ft
o
z
u
1.17
2:23
8.06
<0.8
198
0.8
af
u
u
8.16
3.07
19.37
<2.0
198
2.0
O
r«
Z
U
4.30
1.69
9.01
<0.8
198
0.8
+
U
U
0.96
1.47
11.50
<0.1
198
0.1
8
o
r»
U
6.73
1.71
10.17
2.97
198
0.0001
10
All values are estimated ppmv, except CO2 and H2O in percent
Statistics of three runs combined
U/C - Unconditioned (U) or Conditioned (C) Sample
C4+ - Total aliphatic hydrocarbons larger than 3 carbons (ppmv hexane equivalent)
NDP - Number of data points
EDL - Estimated detection limit lor spectral region used for analysis
-------
Table 2-30a. Other Species Detected by FTIR - Reverberatory Furnace #1 Inlet
Parameter
U/C
Average
Std. Dev.
Max.
Min.
NDP
EDL
Ethylene
C
2.16
3.34
17.17
<0.2
104
0.2
Acetylene
C
4.08
7.74
39.16
<0.05
104
0.05
Benzene
C
1.73
2.87
12.48
<0.1
104
0.1
Methanol
C
0.48
0.62
3.76
<0.2
104
0.2
Formaldehyde
U
0.46
1.10
9.66
<0.1
473
O.I
Acetaldehyde
U
0.05
0.39
6.79
<.5
473
0.5
S
«•»
O
U
U
0.14
0.23
1.96
<0.04
473
0.04
O
u
u
45.01
73.88
425.92
1.76
473
0.08
O
Z
U
2.18
5.77
48.90
<2.0
473
2.0
1,3 - butadiene
C
0.17
0.64
6.01
<0.8
104
0.8
SB
U
U
12.25
12.49
91.75
<2.0
473
2.0
O
ft
Z
U
0.84
0.57
5.92
<0.3
473
0.3
+
U
U
0.61
0.80
15.02
<0.1
473
0.1
S
O
»•»
SB
U
1.43
0.59
4.58
0.49
473
0.0001
O\
All values are estimated ppmv, except CO2 and H2O in percent
Statistics of four runs during loading and tapping combined
U/C - Unconditioned (U) or Conditioned (C) Sample
.C4+ - Total aliphatic hydrocarbons larger than 3 carbons (ppmv hexane equivalent)
NDP - Number of data points
EDL - Estimated detection limit for spectral region used for analysis
-------
Table 2-30b. Other Species Detected by FTIR - Reverberatory Furnace #1 Inlet, continued
Parameter
U/C
Average
Std. Dev.
Max.
Min.
NDP
EDL
Ammonia
U
0.04
O.I6
3. 15
<0.1
473
0.1
Propylene
C
0.39
1.63
16.01
<0.4
104
0.4
Sulfur dioxide
U
6.10
10.79
74.85
<1.2
473
1.2
to
OJ
-J
All values are estimated ppmv
Statistics of four runs during loading and tapping combined
U/C - Unconditioned (U) or Conditioned (C) Sample
NDP - Number of data points
EDL - Estimated detection limit for spectral region used for analysis
-------
Table 2-31 a. Other Species Detected by FTIR - Reverberatory Furnace #1 Outlet
L.
Ol
2
K)
Ou
U/C
Average
Std. Dev.
Max.
Min.
NDP
EDL
Ol
Ol
W
C
2.51
3.00
13.50
<0.2
88
0.2
Ol
Ol
t
^ji
C
4.82
7.44
31.31
<0.05
88
0.05
Ol
Ol
N
Ol
ca
C
1.58
2.30
9.57
<0.l
88
O.I
o
a
^
C
0.49
0.64
2.24
<0.2
88
0.2
Ol
•a
01
2
g
o
U
0.32
0.37
2.71
<0.l
477
O.I
;*,
01
2
Ol
U
0.15
1.46
31.26
<0.4
477
0.5
/— S
6*
o
u
0.13
0.18
1.20
<0.04
477
0.04
O
U
U
46.34
71.04
385.37
0.99
477
0.06
O
z
u
1.83
4.11
24.72
<2.0
477
0.8
01
C
Ol
•a .
3
s
i
rf)
C
0.15
0.50
3.03
<0.6
88
0.6
X
U
u
11.14
9.70
86.53
<0.6
477
2.0
O,
z'
U
0.82
0.49
4.08
<0.1
477
0.1
U
U
0.52
0.64
13.07
<0.04
477
0.04
, — .
^
•-^
0
3G
U
1.44
0.65
3.84
0.42
477
0.0001
NJ
i
U)
oo
All values are estimated ppmv, except CO2 and H2O in percent
Statistics of four runs during loading and lapping combined
U/C - Unconditioned (U) or Conditioned (C) Sample
C4+ - Total aliphatic hydrocarbons larger than 3 carbons (ppmv hexane equivalent)
NDP - Number of data points
EDL - Estimated detection limit for spectral region used for analysis
-------
Table 2-31 b. Other Species Detected by FTIR - Reverberatory Furnace #1 Outlet,
continued
Parameter
U/C
Average
Std. Dev.
Max.
Min.
NDP
EDL
Ammonia
U
0.06
0.17
2.92
<0.1
477
0.1
Propylene
C
0.55
1.77
12.96
<0.4
88
0.4
Sulfur dioxide
U
0.91
2.84
24.88
<.1.2
477
1.2
All values are estimated ppmv
Statistics of four runs during loading and tapping combined
U/C - Unconditioned (U) or Conditioned (C) Sample
NDP - Number of data points
EDL - Estimated detection limit for spectral region used for analysis
2.5.2.5 FTIR Sampling and Measurement System Response Time Measurement
FTIR system sampling and measurement system response time was determined by
measurement of concentration versus time of a dynamic spike of the sample gas. HC1 and SF6
spike gas were introduced via a remote-controlled solenoid valve located upstream of the heated
probe filter. The time required to obtain 90 percent response was measured three times.
Figure 2-1 illustrates data gathered on-site which show the three measurements. It is clear from
the figure that the 90 percent response time is approximately 2 minutes (i.e., two data points).
The figure also shows that the SF6 and HC1 response times are approximately the same, with HC1
slightly lagging relative to SF6.
2-39
-------
to
i-
o
FTIR System Response
(3 measurements)
15.00
o
1 10.00
•s f
o>
§ ~
5.00
0.00
19:19
1 minute data points
19:24
19:29
Time
HC1
SF6
0.00
19:34
Figure 2-1. FTIR System Response Profile (Measured on 7 December 1997)
-------
2.5.2.6 Comparison of FTIR and Method 26A Results for HCI
Table 2-32 shows the comparison between the two sets of results for both the chip dryer
and furnace.
Table 2-32. Comparison of FTIR and Method 26A results for HCI, ppm1
Location
Chip Dryer Inlet
Chip Dryer Outlet
Furnace 1 Inlet
Furnace 1 Outlet
FTIR
8.12
2.48
70.15
2.83
Method 26A
27.45.
1.10
70.37
0.862
'Average of test runs at each location
While it is instructive to compare HCI results from both FTIR and manual methods, care
must be taken in interpreting the two sets of results. For the chip dryer, the FTIR system
measured HCI at a given inlet or outlet only 25 % of the time compared to the corresponding
manual method which was integrated over the entire sampling period, due to splitting half of the
FTIR instrument analysis time equally between inlet and outlet as unconditioned and conditioned
samples. Since HCI was measured only in unconditioned samples, this sampling scheme results
in a 25% duty cycle for the total run for HCI measurement at either the chip dryer inlet or outlet.
The corresponding FTIR data capture for either the furnace inlet #1 or outlet was approximately
38%.
Future testing which incorporates both FTIR and Method 26A should include full
concurrent sampling to facilitate unbiased comparison between the two methods.
2-41
-------
3.0 DESCRIPTION OF FACILITY
(To be supplied by Research Triangle Institute).
3-1
-------
4.0 SAMPLING LOCATIONS
The sampling locations that were used during the emissions testing program at Gulp
Aluminum Alloys are described in this section. Flue gas samples were collected at the inlet and
at the outlet of the lime-injected baghouses using manual methods and FTIR, with two 4" ID
ports to allow for the operation of two manual sampling methods and one 3" ID port for the
FTIR. The configurations of the sampling locations are shown in Figures 4-1 (El, chip dryer
baghouse inlet), 4-2 (E2, chip dryer baghouse outlet), 4-3 (E3, reverberatory furnace #1 baghouse
inlet), and 4-4 (E4, reverberatory furnace #1 baghouse outlet).
The chip dryer operated at approximately 150° F, with a slightly negative pressure at the
fan inlet and a slightly positive pressure at the outlet. At the inlet and outlet of the reverberatory
furnace #1 baghouse, 4" ports were available. FTIR ports were installed horizontally and
upstream from manual ports. The baghouse operated at approximately 175° F, with a slightly
positive pressure.
The inlet of the lime-injected baghouse for the chip dryer was a circular duct 18" in
diameter, and the outlet was a circular duct 25" in diameter. Two 4" ID ports were installed at
90 degrees to each other, one horizontally and one vertically on top of the duct, and a third 3" ID
port was installed upstream of the other ports for the FTIR sampling probe.
The inlet to the reverberatory furnace #1 baghouse was a circular duct 42" in diameter.
Two 4" ports and one 3" port were installed; the two 4" ports were 90 degrees to each other. The
outlet was an exhaust stack 48" in diameter, approximately 30 feet above the ground. The outlet
had two 4" ports; a third port (3" ID) was installed for the FTIR upstream of the other two ports.
The position and number of traverse points for each location are shown in Figures 4-5 through
4-8. For stacks having diameters greater than 0.61 m (24 in.), no traverse points were located
within 2.5 cm (1.00 in.) of the stack walls.
4-1
-------
To Baghouse
1 Inlet, Dryer Baghouse
\
Building
Wall
A
\
18"
^ riow
"TpW' ^/
Fan
\
I ^
55" 48"
, •„
i
Ground
•figure 4-1. E1, Chip Dryer Baghouse Inlet
-------
Outlet
Chip Dryer
Baghouse
4" ID Manual
Ports
3" ID FTIR
Port
Lime Injection
Figure 4-2. E2, Chip Dryer Baghouse Outlet
-------
Reverberatory
Furnace
3" ID FTIR
Port
4" ID Ports
Flow
To Baghouse
20'
48'
Lime shed
w
*S^W* -J " j t. 1 s '
•*^v;\.
Flame Arrester
Figure 4-3. E3, Reverberatory Furnace Bagho^fie Inlet
-------
Exhaust
Handrail
Catwallc
48"
6'
3" FTIR
Port
24'
Fan
Ground
10'
Figure 4-4. E4, Reverberatory Furnace Baghouse Outlet
-------
For stack diameters equal to or less than 0.61 m (24 in.), no traverse points was located
within 1.3 cm (0.50 in.) of the stack walls. When any of the traverse points fell within 2.5 cm
(1.00 in.) of the stack walls, they were relocated to a distance of 2.5 cm (1.00 in.) or a distance
equal to the nozzle inside diameter, whichever was larger.
All test ports and their locations met the requirements of EPA Method I.
4-10
-------
5.0 SAMPLING AND ANALYTICAL PROCEDURES BY ANALYTE
The sampling and analytical procedures used for the Gulp Aluminum Alloys plant test
program are the most recent revisions of the published EPA methods. In this section,
descriptions of each sampling and analytical method by analyte are provided.
5.1 Chlorinated Dibenzo-p-Dioxin and Chlorinated Dibenzofuran Emissions
Testing Using EPA Method 23
The sampling and analytical method for determining flue gas emissions of
Polychlorinated Dibenzo-p-Dioxins and Polychlorinated Dibenzofurans (CDD/CDF) is EPA
Method 23. .
5.1.1 Method 23 Sampling Equipment
The method uses the sampling train shown in Figure 5-1. The Method 23 sampling
system is similar to a Method 5 train with the following exceptions:
• All components (glass probe/nozzle liner, all other glassware, filters) are pre-
cleaned using solvent rinses and extraction techniques; and
• A condensing coil and XAD-2® resin absorption module are located between
the filter and impinger train.
5.1.2 Method 23 Equipment Preparation
In addition to the standard EPA Method 5 requirements, Method 23 includes several
unique preparation steps which ensure that the sampling train components are not contaminated
with organics that may interfere with analysis. The glassware, glass fiber filters and absorbing
resin are cleaned and the filters and resin are checked for 42 residuals before they are packed.
5-1
-------
stack wall
Gas Flow
Ul
to
temperature
sensor
1 Ir
—
heated glass liner
> n_
1 c ' I
1
heat
r
L
]
1
id
~1
J
i
cc
condenser
filter
holder
"S" type
pilot
manometer
temperature
sensor
XAD-2 trap
temperature
sensor
t
recirculation
pump
calibrated
orifice
gas exit
manometer
L
ifyg
met
T,
r
c
as
sr
H
Zl
;
empty
•
-"
^
r
1
KJ rtJ |tJ ftJ mJ
ice
bath
^ ^ A i
x A A
100ml ^^ .,~
HPLC Water empty SI"C,a
gel
fine
Mr —^ vacuum
Y I 9aU9e
V
^ coarse
( ) -^^t- vacuum pump
Figure 5-1. Method 23 Sampling Train Configuration
-------
5.1.2.1 Glassware Preparation
The glassware preparation procedure is shown in Table 5-1. Glassware is washed in
soapy water, rinsed with distilled water, baked and then rinsed with acetone followed by
methylene chloride. Clean glassware is allowed to dry under a hood loosely covered with foil to
prevent laboratory contamination. Once the glassware is dry, the air exposed ends are sealed
with methylene chloride rinsed aluminum foil. All the glass components of the sampling train
including the glass nozzles plus any flasks, petri dishes, graduated cylinders and pipets that are
used during sampling and recovery will be cleaned according to this procedure. Non-glass
components (such as the Teflon -coated filter screens and seals, tweezers, Teflon squeeze
bottles. Nylon® probe brushes and Nylon nozzle brushes) are cleaned following the same
procedure except that no baking is performed.
5.1.2.2 XAD-2® Resin and Filter Preparation
XAD-2® absorbing resin and glass fiber filters are pre-cleaned by separate procedures
according to the specified method. Only pesticide grade solvents and HPLC grade water are used
to prepare for organic sampling, and to recover these samples. The lot number, manufacturer and
grade of each reagent used are recorded in the laboratory notebook.
To prepare the filters, a batch of 50 is placed in a Soxhlet extractor pre-cleaned by
extraction with toluene. The Soxhlet is charged with fresh toluene and refluxes for 16 hours.
After the extraction, the toluene is analyzed as described in Sections 5.1 and 5.3 of the reference
method (EPA Method 23) for the presence of tetrachlorodibenzo-p-dioxins (TCDD) and
tetrachlorodibenzofurans (TCDF). If these analytes are found, the filters are re-extracted until the
analyte is not detected. The filters are then dried completely under a clean nitrogen (N2) stream.
Each filter is individually checked for holes, tears, creases or discolorations, and if any are found,
the filter is discarded. Acceptable filters are stored in a pre-cleaned petri dish, labeled by date of
analysis and sealed with Teflon® tape.
5-3
-------
Table 5-1. Method 23 Glassware Cleaning Procedure
(Train Components, Sample Containers and Laboratory Glassware)
NOTE: USE VTTON® GLOVES AND ADEQUATE VENTILATION WHEN RINSING
WITH SOLVENTS
1. Soak all glassware in hot soapy water (laboratory detergent).
2. Rinse with tap water to remove soap.
3. Rinse with HPLC-grade H2O, three times
4. Bake at 450° F for 2 hours.3
5. Rinse with acetone (pesticide grade), three times.
6. Rinse with methylene chloride (pesticide grade), three times.
7. Cap glassware with clean glass plugs or methylene chloride rinsed aluminum foil.
8. Mark cleaned glassware with color-coded identification sticker.
9. Rinse glassware immediately before using with acetone and methylene chloride
(laboratory proof)-
a Step (4) has been added to the cleanup procedure to replace the dichromate soak specified in the
reference method. ERG has demonstrated in the past that baking glassware sufficiently removes
organic artifacts. Step 4 is not used for probe liners and non-glass components of the train that
cannot withstand 450° F (i.e., Teflon®-coated filter screen and seals, tweezers, Teflon® squeeze
bottles, Nylon probe and nozzle brushes).
5-4
-------
To prepare the absorbing resin, the XAD-2 resin is cleaned in the following sequential
order:
• Rinse with HPLC grade water, discard water;
• Soak in HPLC grade water overnight, discard water;
• Extract in Soxhlet with HPLC grade water for 8 hours, discard water;
• Extract with methanol for 22 hours, discard solvent;
• Extract with methylene chloride for 22 hours, discard solvent;
• Extract with methylene chloride for 22 hours, retain an aliquot of solvent for
analysis of CDDs and CDFs by HRGC/HRMS; and
• Dry resin under a clean N2 stream.
Once the resin is completely dry, it is checked for the presence of methylene chloride,
CDDs and CDFs as described in Section 3.1.2.3.1 of the reference method. If any analytes are
found, the resin is re-extracted. If methylene chloride is found, the resin is dried until the excess
solvent is removed. The absorbent is to be used within four weeks of cleaning.
The cleaned XAD-2® resin is spiked before shipment to the field with five CDD/CDF
internal standards. Due to the special handling considerations required for the internal standards,
the spiking is performed by Triangle Laboratories. For convenience and to minimize
contamination, Triangle Laboratories also performs the resin and filter cleanup procedures and
loads the resin into the glass traps.
5.1.2.3 Method 23 Sampling Train Preparation
The remaining preparation includes calibration and leak checking of all sampling train
equipment, including meter boxes, thermocouples, nozzles, pitot tubes, and umbilicals.
5-5
-------
Referenced calibration procedures are followed when available. The results are properly
documented in a laboratory notebook or project file and retained.
5.1.3 Method 23 Sampling Operations
5.1.3.1 Preliminary Measurements
Prior to sampling (data collected during presurvey), preliminary measurements are
required to ensure isokinetic sampling. These measurements include determining the traverse
point locations, performing a preliminary velocity traverse, cyclonic flow check and moisture
determination. These measurements are used to calculate a "K factor." The K factor is used to
determine an isokinetic sampling rate from stack gas flow readings taken during sampling.
Measurements are then made of the duct inside diameter, port nozzle length, and the
distances to the nearest upstream and downstream flow disturbances. These measurements are
then used to determine sampling point locations by following EPA Reference Method 1
guidelines. The distances are then marked on the sampling probe using an indelible marker.
5.1.3.2 Assembling the Train
Method 23 sampling train components are collected in the recovery trailer and final
train assembly is performed at the stack location. First, the empty, clean impingers are
assembled and laid out in the proper order in the recovery trailer. Each ground glass joint is
carefully inspected for hairline cracks. The first impinger is a knockout impinger which has a
short tip. The purpose of this impinger is to collect condensate which forms in the coil and
XAD-2® resin trap. The next two impingers are modified tip impingers which each contain
100 mL of HPLC grade water. The fourth impinger is empty, and the fifth impinger contains 200
to 300 grams of blue indicating silica gel. After the impingers are loaded each impinger is
weighed, the initial weight and contents of each impinger are recorded on a recovery data sheet.
The heights of all the impingers are approximately the same to obtain a leak free seal. The open
5-6
-------
ends of the train are sealed with methylene chloride-rinsed aluminum foil, or clean ground glass
caps.
: The second step is to load the filter into the filter holder in the recovery trailer. The
filter holder is then capped off and placed with the resin trap and condenser coil (capped) into the
impinger bucket. A supply of precleaned foil and socket joints is also placed in the bucket in a
clean plastic bag for the convenience of the samplers. Sealing greases are not used to avoid
contamination of the sample. The train components are transferred to the sampling location and
assembled as previously shown in Figure 5-1. The heated probe and filter box will be a single
®
unit mounted on a vertical monorail. The chilled impinger box with the condenser and XAD-2
trap will be placed on the floor of the scaffolding.
5.1.3.3 Sampling Procedures
After the train is assembled, the heaters for the probe liner and heated filter box are
turned on and the sorbent module/condenser coil recirculating pump is turned on. When the
system reaches the appropriate temperatures, the sampling train is ready for pre-test leak
checking. The temperature of the sorbent module resin must not exceed 50° C (120° F) at any
time and during testing it must not exceed 20° C (68° F). The filter temperature is maintained at
120 ±14° F (248 ±25° F). The probe temperature is maintained above 100° C (212° F).
The sampling trains are leak checked at the start and finish of sampling. (Method 5/23
protocol only requires post-test leak checks and recommends pre-test leak checks.) ERG
protocol also incorporates leak checks before and after every port change. An acceptable pre-test
leak rate is less than 0.02 acfm (ft3/min) at approximately 15 inches of Hg, If during testing, a
piece of glassware needs to be emptied or replaced, a leak check is performed before the
glassware piece is removed, and after the train is re-assembled.
To leak check the assembled train, the nozzle end is capped off and a vacuum of
15 inches Hg is pulled in the system. When the system is evacuated, the volume of gas flowing
5-7
-------
through the system is timed for 60 seconds. After the leak rate is determined, the cap is slowly
removed from the nozzle end until the vacuum drops off, and then the pump is turned off. If the
leak rate requirement is not met, the train is systematically checked by first capping the train at
the filter, at the first impinger, etc., until the leak is located and corrected.
After a successful pre-test leak check has been conducted, all train components are at
their specified temperatures and initial data are recorded (DGM reading), the test can be initiated.
Sampling train data are recorded periodically on standard data forms. A checklist for CDD/CDF
sampling is included in Table 5-2. A sampling operation that is unique to CDD/CDF sampling is
that the gas temperature entering the resin trap must be below 20° C (68° F). The gas is cooled
by a water jacket condenser through which ice water is circulated.
The leak rates and sampling start and stop times are recorded on the sampling task log.
Also, any other events that occur during sampling are recorded on the task log such as sorbent
module heat excursions, pitot cleaning, thermocouple malfunctions, heater malfunctions or any
other unusual occurrences.
If the probe liner breaks while DGM is not running (i.e., during port changes or after the
run is completed), the probe liner is replaced, the run is completed, and sample recovery done on
both the broken sections of the glass liner and the replacement liner. If the break occurs while
the DGM is running and the exact time of the break is noted, the test is stopped so that the probe
liner can be replaced. The run is then completed and sample recovery done on all liner sections.
If the recovered sample appears unusual, the sample is discarded and an additional run is
performed later. If the recovered sample appears normal, the run is tentatively acceptable.
At the conclusion of the test run, the sample pump (or flow) is turned off, the probe is
removed from the duct, a final DGM reading is taken, and a post-test leak check is completed.
The procedure is identical to the pre-test procedure. However, the vacuum should be at least
one inch Hg higher than the highest vacuum attained during sampling. An acceptable leak rate is
less than 4% of the average sample rate or 0.02 acfm (whichever is lower).
5-8
-------
Table 5-2. CDD/CDF Sampling Checklist
Before test starts:
1. Check impinger set to verify the correct order, orientation and number of impingers. Verify
probe markings, and remark if necessary.
2. Check that you have all the correct pieces of glassware. Have a spare probe liner, probe
sheath, meter box and filter ready to go at location.
3. Check for data sheets and barometric pressure.
4. Prepare bag sampling equipment for CO2/O2, except when using CEMs for CO2/O2
determinations.
5. Examine meter box - level it, zero the manometers and confirm that the pump is operational.
6. Verify the filter is loaded correctly and as tightly as possible; place filter in line with the
train and leak check at 15 inches Hg.
7. Add probe to train.
8. Check thermocouples - make sure they are reading correctly.
9. Conduct pitot leak check, recheck manometer zero.
10. Do final leak check; record leak rate and vacuum on sampling log.
11. Turn on variacs and check to see that the heat is increasing.
12. Check that cooling water is on and flowing. Add ice to impinger buckets.
13. Check isokinetic K-factor - make sure it is correct. (Refer to previous results to confirm
assumptions. Two people should calculate this independently to double check it.)
5-9
-------
Table 5-2. COD/CDF Sampling Checklist (continued)
During Test:
1. Notify field task leader of any sampling problems ASAP. Train operator should fill in
sampling log and document any abnormalities.
2. Perform simultaneous/concurrent testing with other locations (if applicable). Maintain filter
temperature between 248 ° F ±25 ° F. Keep temperature as steady as possible. Maintain the
resin trap and impinger temperatures below 68° F. Maintain probe temperature above
212° F.
3. Leak check between ports and record on data sheet. Leak check if the test is stopped to
change silica gel, to decant condensate, or to change filters.
4. Record sampling times, rate, and location for the fixed gas bag sampling (CO, CO2, O2), if
applicable.
5. Blow back pitot tubes periodically if moisture entrapment is expected.
6. Change filter if vacuum suddenly increases or exceeds 15 inches Hg.
7. Check impinger solutions every ¥2 hour; if the knockout impinger is approaching full, stop
test and empty it into a pre-weighed bottle and replace it in the train.
8. Check impinger silica gel every Vi hour; if indicator color begins to fade, request a prefilled,
preweighed impinger from the recovery trailer.
9. Check the ice in the impinger bucket frequently. If the stack gas temperatures are high, the
ice will melt at the bottom rapidly. Maintain condenser coil and silica gel impinger gas
temperatures below 20° C (68° F).
After test is completed:
1. Record final meter reading.
2. Do final leak check of sampling train at maximum vacuum during test.
5-10
-------
Table 5-2. CDD/CDF Sampling Checklist (continued)
3. Do final pitot leak check.
4. Check completeness of data sheet. Verify the impinger bucket identification is recorded on
the data sheets. Note any abnormal conditions.
5. Leak check, check functions (level, zero, etc.) of pitot tubes and inspect for tip damage.
6. Disassemble train, cap sections, and take each section and all data sheets down to recovery
trailer.
7. Probe recovery (use 950 mL bottles)
a) Bring probes into recovery trailer (or other enclosed area).
b) Wipe the exterior of the probe to remove any loose material that could contaminate the
sample.
c) Carefully remove the nozzle/probe liner and cap it off with prerinsed aluminum foil.
d) For acetone rinses (all trains)
Attach precleaned cyclone flask to probe to catch rinses
Wet all sides of probe interior with acetone
- While holding the probe in an inclined position, put precleaned probe brush down
into probe and brush it in and out
- Rinse the brush, while in the probe, with acetone
- Do this at least 3 times until all the particulate has been recovered.
Recover acetone into a preweighed, prelabeled sample container
e) Follow the procedure outlined in (d) using methylene chloride. Recover the solvent
into the same acetone recovery bottle.
f) Follow the procedure outlined in (d) using toluene. Recover this solvent into a separate
preweighed prelabeled sample container.
8. Cap both ends of nozzle/probe liner for the next day, and store in dry safe place.
9. Make sure data sheets are completely filled out, legible, and give them to the field task
leader.
5-11
-------
5.1.4 CDD/CDF Sample Recovery
To facilitate transfer from the sampling location to the recovery trailer, the sampling
train is disassembled into the following sections: the probe liner, filter holder, filter to condenser
glassware, condenser and sorbent module, and the impingers in their bucket. Each of these
sections is capped with methylene chloride rinsed aluminum foil or ground glass caps before
removal to the recovery trailer. Once in the trailer, field recovery follows the scheme in
Figure 5-2. The samples are recovered and stored in cleaned amber glass bottles to prevent light
degradation.
The probe and nozzle are first rinsed with approximately 100 mL of acetone and
brushed to remove any paniculate. This first rinse is followed with a rinse of methylene
chloride. Both of these rinses are collected in the same bottle. The same two solvents are used
to rinse the cyclone, front/back half filter holder, filter support, connecting glassware and
condenser. These rinses are added to the probe rinse bottle. All of the components listed above
are again rinsed with toluene, but collected in a separate container. In addition, the Teflon®
transfer line used with the vertical sampler will be filled with toluene and allowed to stand for
5 minutes before adding to the toluene rinses. The filter is carefully removed from the filter
holder, placed in a pre-labeled petri dish and sealed with Teflon® tape for transport to the
laboratory.
The contents of impingers 1-4 (H2O) and impinger 5 (silica gel) are weighed to 0.5 mg
and then discarded.
The solvents used for train recovery are all pesticide grade. The use of the highest
grade reagents for train recovery is essential to prevent the introduction of chemical impurities
which interfere with the quantitative analytical determinations.
5-12
-------
Probe Probe Cyclone Front Half of Filler Back Half of Connecting Condenser
N
Rinse w
ozzle L
th Acetone A
ner
tach
Filler 1
Housing Sup
port Filter H
jusing Lii
ie
Until all Paniculate 250 mL flask Brush and Brush and
is Removed to Ball Joint rinse with rinse with Rinse with Rinse with Rinse with Rinse with
acetone (3x) acetone (3x) acetoi
Rinse wi
Rinse with
Acetone
Empty Flask
into 950 mL
Bottle
Brush Liner and Rinse
with 3 Aliquols of
Acetone
Check Liner to see if
Paniculate is
removed; if not, repeat
h 3 Aliquots Rin
se with R
nse with Rins
e with
.ofMethylene 3 Aliquots 3 Aliquots 3 Aliquols
Chloride ofMelhylene ofMelhylene ofMethylene
Chloride Chloride Chloride
Rinse
with Rin
se with Rin
se with Rin<
Rcco
ic (3x) acetone (3x) acelon
e (3x) acetone (3x)
Rinse with melhylene Rinse with Rinse with
chloride (3x) (at least methylene melhylene
once let the rinse stand chloride chloride (3x)
5 min in unit) (3x) (at least once let
the rinse stand
ver into
pieweighed
b(
Mile
PR
5 min in unit)
e with Rinse with Toluene (3x) Rinse with Toluene (3x) (at
Toluene (3x)* Toluene (3x) Toluene (3x) Toluene (3x) (at least once let the rinse Toluene (3x) least once let the
stand 5 min in unit) rinse stand 5 inin
*This fraction should not be combined with the other toluene
fractions
I'RT/CRT
in uni
)
Figure 5-2. Method 23 Field Recovery Scheme
-------
u»
Fil
ter
Carefully
remove filler
from support
with tweezers
Brush loose
Paniculate
onlo Tiller
Seal in
pelri
dish
F' . .„ .
Resin
Trap Istlm
(knoc
jinger 2nd Itn
kout)
pinger 3rd Im
pinger 4lh Im
pinger 5th Im
(silic
•
pinger
a gel)
Secure XAD Weigh Weigh Weigh Weigh Weigh
trap openings Impingcr Impingcr Impinger linpinger . Impinger
with glass balls
and clamps
Place in cooler Record weigh! Record weigh! Record weight Record weight Record weight
for storage and and and • and and
calculate gain calculate gain calculate gain calculate gain calculate gain
i'SM 1
Discard
Note: See Table 5-3 for Sample Fractions Identification
Sav
efor
regeneration
Figure 5-2. Method 23 Field Recovery Schedule (continued)
-------
The train components recovered in the field are listed in Table 5-3. All recovered
samples are stored in coolers on ice at all times. The samples will be delivered to the analytical
laboratory upon return to ERG accompanied by written information designating target analytes.
Table 5-3. Method 23 Sample Fractions Shipped To Analytical Laboratory
Container/
Component
1
2
3
4
Code
F
PRa
PRT
CRT
SM
Fraction
Filter(s)
Acetone and methylene chloride rinses of
nozzle/probe, cyclone, front half/back filter
holder, filter support, connecting
glassware, condenser
Toluene rinse of nozzle/probe, cyclone,
front half/back half filter holder, filter
support, connecting line and condenser
®
XAD-2 resin trap (sorbent module)
"Rinses include acetone and methylene chloride recovered into the same sample bottle.
5.1.5 CDD/CDF Analytical Procedures
The analytical procedure used to obtain analyte concentrations from a single flue gas
sample is high resolution gas chromatography (HRGC) and high resolution mass spectrometry
(HRMS) (resolution from 8000-10000 m/z). The target CDD/CDF congeners are listed in
Table 5-4. The analysis was performed by Triangle Laboratories, Inc., by Method 23/8290.
The Method 23 samples are prepared and analyzed according to the scheme in
(R)
Figure 5-3. The XAD-2 and filter (along with the concentrated acetone/methylene chloride
rinses) are placed in a Soxhlet extractor and extracted with toluene. This extract is added to the
toluene train rinses and then concentrated by rotary evaporation. This concentrated sample
extract is added to the toluene train rinses and then concentrated by rotary evaporation. This
concentrated sample is subjected to a sample cleanup procedure before analysis. For the
5-15
-------
Table 5-4. CDD/CDF Congeners To Be Analyzed
DIQXINS:
2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD)
Total tetrachlorinated dibenzo-p-dioxins (TCDD)
i,2,3,7,8-pentachlorodibenzo-/?-dioxin(l,2,3,7,8-PeCDD)
Total pentachlorinated dibenzo-p-dioxins (PeCDD)
1,2,4,5,7,8-hexachlorodibenzo-p-dioxin (1,2,3,4,7,8-HxCDD)
l,2,3,6,7,8-hexachlorodibenzo-/7-dioxin(l,2,4,5,7,8-HxCDD)
l,2,3,7,8,9-hexachlorodibenzo-p-dioxin(l,2,3,7,8,9-HxCDD)
Total hexachlorinated dibenzo-p-dioxins (HxCDD)
l,2,3,4,6,7,8-heptachlorodibenzo-p-dioxin(l,2,3,4,6,7,8-HpCDD)
Total heptachlorinated dibenzo-p-dioxins (HpCDD)
Total octachlorinated dibenzo-p-dioxin (OCDD)
FURANS:
2,3,7,8-tetrachlorodibenzofurans(2,3,7,8-TCDF)
Total tetrachlorinated dibenzofurans (TCDF)
1,2,3,7,8-pentachlorodibenzofuran (1,2,3,7,8-PeCDF)
2,3,4,7,8-pentachlorodibenzofuran(2,3,4,7,8-PeCDF)
Total pentachlorinated dibenzofurans (PeCDF)
l,2,3,4,7,8-hexachlorodibenzofuran(l,2,3,4,7,8-HxCDF)
1,2,3,6,7,8-hexachlorodibenzofuran (1,2,3,6,7,8-HxCDF)
2,3,4,6,7,8-hexachlorodibenzofuran(2,3,4,6,7,8-HxCDF)
l,2,3,7,8,9-hexachlorodibenzofuran(l,2,3,7,8,9-HxCDF)
Total hexachlorinated dibenzofuran (HxCDF)
l,2,3,4,6,7,8-heptachlorodibenzofuran(l,2,3,4,6,7,8-HpCDF)
1,2,3,4,7,8,9-heptachlorodibenzofuran (1,2,3,4,7,8,9-HpCDF)
Total heptachlorinated dibenzofurans (HpCDF)
Total octachlorinated dibenzofuran (OCDF)
5-16
-------
Toluene
Rinses
Rotovap
to 1 mL
Add to SOX
for Toluene
Extraction
AC/MeCl2
Rinses
KDto
1 mL
Add to SOX for Toluene
Extraction
Spike with
PCDD/PCDF Standards
Soxhlet in Toluene
XAD-2®
Prespiked with
5
PCDD/PCDF
Standards
Filter +
XAD-2® Add
to Soxhlet
Split 1:1
50% Toluene Extract to
Dioxins
Do PCDDs/Fs Cleanup
Analyze for PCDDs/Fs Method 8290X
Figure 5-3. Extraction and Analysis Schematic for Method 23 Samples
5-17
-------
CDD/CDF analysis, isotopically-labeled surrogate compounds and internal standards and
surrogates that are used are described in detail in EPA Method 23.
Data from the mass spectrometer are recorded and stored on a computer file as well as
printed on paper. Results such as amount detected, detection limit, retention time, and internal
standard and surrogate standard recoveries are calculated by computer. The chromatograms are
retained by the analytical laboratory and also included in the analytical report delivered to ERG.
5.1.5.1 Preparation of Samples for Extraction
Upon receiving the sample shipment, the samples are checked against the chain-of
custody forms and then assigned an analytical laboratory sample number. Each sample
component is reweighed to determine if leakage occurred during travel. Color, appearance, and
other particulars of the samples are noted. Samples are extracted within 21 days of collection
and processed through cleanup procedures before concentration and analysis.
5.1.5.2 Calibration of GC/MS System
A five-point calibration of the GC/MS system is performed to demonstrate instrument
linearity over the concentration range of interest. Relative response factors are calculated for
each dioxin/furan congener or compound of interest. The response factors are verified on a daily
basis using a continuing calibration standard consisting of a mid-level standard. The instrument
performance is acceptable only if the measured response factors for the labeled and unlabeled
compounds and the ion-abundance ratios are within the allowable limits specified in the method.
5.1.6 CDD/CDF Analytical Quality Control
All quality control procedures specified in the test method are followed. Blanks are
used to determine analytical contamination, calibration standards are used for instrument
calibration and linearity checks, internal standards are used to determine isomer recoveries and
5-18
-------
adjust response factors for matrix effects, surrogate standards are used to measure the collection
efficiency of the sampling methodology and an alternate standard is used as a column efficiency
check.
5.1.6.1 CDD/CDF Quality Control Blanks
Four different types of sample blanks are collected for CDD/CDF analysis. The types
of blanks that are required are shown in Table 5-5.
Table 5-5. Method 23 Blanks Collected
Blank
Field Blanks
Glassware Proof Blank
Method Blank
Reagent Blanks
Collection
One run collected for each
sample location) and
analyzed
Each train to be used (2) will
be loaded and quantitatively
recovered prior to sampling
At least one for each
analytical batch (laboratory
generated)
One 500 mL sample for each
reasent and lot
Analysis
Analyze with field samples
Archive for potential analysis
Analyze with each analytical
batch of field samples
Archive for potential analysis
Reagent blanks of 500 mL of each reagent used at the test site are saved for potential
analysis. Each reagent blank is of the same lot as was used during the sampling program: Each
lot number and reagent grade is recorded on the field blank label and in the laboratory notebook
®
(acetone, methylene chloride, toluene, filter. XAD-2).
A glassware blank (proof blank) is recovered from each set of sample train glassware
that is used to collect the organic samples. The precleaned glassware, which consists of a probe
liner, filter holder, condenser coil, and impinger set, is loaded as if for sampling and then
quantitatively recovered exactly as the samples will be. Analysis of the generated fractions will
be used to check the effectiveness of the glassware cleaning procedure only if sample analysis
indicates a potential contamination problem.
5-19
-------
A field blank is collected from a set of CDD/CDF glassware that has been used to
collect at least one sample and has been recovered. The train is re-loaded, leak checked and left
at a sampling location during a test run. The train is then recovered. The purpose of the field
blank is to measure the level of contamination that occurs from handling, loading, recovering,
leak checking, and transporting the sampling train. The field blanks are analyzed with the flue
gas samples. If they are unsatisfactory in terms of contamination, reagent blanks may be
analyzed to determine the specific source of contamination.
In addition to the three types of blanks that are required for the sampling program, the
analytical laboratory will analyze a method blank with each set of flue gas samples. This method
blank will consist of preparing and analyzing an aliquot of toluene by the exact procedure used
for the samples analysis. The purpose of this method blank is to verify that there is no
laboratory contamination of the field samples.
5.1.6.2 Quality Control Standards and Duplicates
Recoveries of the internal standards must be between 40 to 130% for the tetra- through
hexachlorinated compounds and in the range of 25 to 130% for the hepta- and octachlorinated
homologs. If these requirements are not met, the data will be acceptable if the signal to noise
ratio is greater than or equal to ten. If these requirements are met, the results for the native
(sampled) species are adjusted according to the internal standard recoveries.
Surrogate standard recoveries must be between 70 to 130%. If the recoveries of all
standards are less than 70%, the project director will be notified immediately to determine if the
surrogate results will be used to adjust the results of the native species.
Duplicate analysis is performed for every ten samples. The purpose of this duplicate
analysis is to evaluate the precision of the combined sample preparation and analytical
methodology.
5-20
-------
5.1.7 Analytes and Detection Limits for Method 23
The target analytes are the tetra- through octachlorinated dibenzodioxins and
chlorinated dibenzofurans. The detection limit of the individual compounds is dependent on the
detection limit of the analytical method, the volume of the final extract and the total volume of
gaseous sample collected in the sampling trains. Following the protocol of Method 23, the
fractions to be collected for analysis from each train are:
• Fraction I—Filter;
• Fraction 2—XAD-2 sorbent module;
• Fraction 3—Acetone and methylene chloride rinses of all train components prior
to sorbent module and;
• Fraction 4—Toluene rinses of all train components prior to the sorbent module.
Following the sample preparation protocol outlined in Method 23, a single combined
sample is presented for analysis for D/F by high resolution gas chromatography/high resolution
mass spectrometry. (The individual samples will no longer be available for analysis.) The final
volume of this sample is 200 fu.L of which a 2 /J.L aliquot is injected into the instrument. Using
an instrument detection limit of 50 pg for tetra-, 250 pg for penta- through hepta-, and 500 pg for
octachlorinated D/F, the total minimum detectable amounts can be calculated and are given in
Table 5-6.
Using a four hour sampling time at an assumed sampling rate of 0.65 to 0.75 cfm, the
MDLs shown in Table 5-7 are possible. The sampling flow rate at the outlet location will be
dictated by the flow rate of the stack gas since isokinetic sampling will be performed.
5-21
-------
5.2 Hydrochloric Acid/Particulate Matter Emissions Testing Using EPA
Method 26A
Hydrogen chloride (HC1) sampling is accomplished using EPA Method 26A,
Determination of Hydrogen Halide and Halogen Emissions from Stationary Sources - Isokinetic
Method. Method 26A is particularly suited for sampling at sources emitting acid particulate
matter (i.e., hydrogen chloride dissolved in water droplets). In this method, a gas sample is
extracted isokinetically from the stationary source and passed through acidified water. In
acidified water, HC1 solubilizes and forms chloride (CI~) ions. Ion chromatography (1C) is used
to detect the chloride ions present in the sample. In addition, sampling for Particulate Matter
(PM) is also performed according to the EPA Method 26A protocol. This method is applicable
to the determination of particulate mass emissions collected on a glass fiber filter and any
material that condenses at or above the filter temperature of 120±14°C (248±25°F) from various
types of process controls and combustion sources. The particulate mass, which includes any
material that condenses at or above the filter temperature, is determined gravimetrically after
removal of uncombined water.
Particulate concentrations are based on the weight gain of the filter and any condensible
PM recovered from the acetone rinses of the probe, nozzle, and front half of the filter.
5.2.1 Method 26A Sampling Equipment
The EPA Method 26A methodology uses the sampling train shown in Figure 5-4. The
5-impinger train consists of a borosilicate glass nozzle/probe liner followed by a heated filter
assembly with a Teflon" filter support, a series of impingers and a meter box and vacuum pump
as specified in EPA Method 5. The sample is not exposed to any metal surfaces in this train.
5-23
-------
to
Slack
Temperature /a
Sensor
Gooseneck
Nozzle
Thermometer
Glass Filter Holder
X
Thermometer
S-Type Pilot Tube
Impingers with Absorbing Solution
(see below)
Manometer
Figure 5-4. Schematic of Method 26A Sampling Train
-------
The contents of the sequential impingers are:
• Impinger #1 (Greenburg-Smith) and Impinger #2 (Greenburg-Smith), known
volumes of 0. IN H2SO4 (nominal 100 mL);
• Impinger #3 (modified Greenburg-Smith) and Impinger #4 (modified Greenburg-
Smith), known volumes of 0.1 N NaOH;
• Impinger #5 (modified Greenburg-Smith), indicating silica gel.
5.2.2 Method 26A Sampling Equipment Preparation
5.2.2.1 Glassware Preparation
Glassware is washed in soapy water, rinsed with hot tap water, rinsed with Type n
water, rinsed with acetone to remove the water, rinsed three times with acetone and then air
dried. This procedure is used on all the glass components of the sampling train including the
glass nozzles plus any sample bottles, Erlenmeyer flasks, petri dishes, and graduated cylinders.
Non-glass components (such as the Teflon®-coated filter screens and seals, tweezers, Teflon®
squeeze bottles, Teflon" probe brushes) are cleaned following the same procedure. The cleaning
procedure is summarized in Table 5-8.
5.2.2.2 Reagent Preparation
The sample train filters are Pallflex® TX40HI45 Teflon® mat filters that meet the
criteria specified in Section 3.1.1 of EPA Method 5. These filters are used as received from the
vendor. The acetone is purchased as HPLC grade to ensure a low residue after evaporation. The
reagent water is distilled/deionized grade that meets the requirements of ASTM Type 3 water or
equivalent. The lot number, manufacturer and grade of each reagent that is used are recorded in
the laboratory notebook.
5-25
-------
Table 5-8. Glassware Cleaning Procedure
(Method 26A Train Components)
NOTE: USE DISPOSABLE GLOVES AND ADEQUATE VENTILATION
1. Soak all glassware in hot soapy water (laboratory detergent).
2. Rinse with tap water to remove soap.
3. Rinse with HPLC grade water (three times).
4. Rinse with acetone (three times).
5. Air dry.
6. Cap glassware with clean glass plugs or Parafilm.®
7. Mark cleaned glassware with color-coded identification sticker.
The analyst wears both safety glasses and protective gloves when the reagents are
mixed or handled. Each reagent has its own designated transferTeflon® squeeze bottle and is
marked for identification and used only for the reagent for which it is designated.
5.2.2.3 Equipment Preparation
The remaining preparation includes calibration and leak checking of all of the train
equipment, including meter boxes, thermocouples, nozzles, pitot tubes, and umbilicals.
Referenced calibration procedures are followed when available, and the results are properly
documented and retained. A discussion of the techniques used to calibrate this equipment is
presented below.
Type-S Pitot Tube Calibration. The EPA has specified guidelines concerning the
construction and geometry of an acceptable Type-S pitot tube. If the specified design and
5-26
-------
construction guidelines are met, a pitot tube coefficient of 0.84 is used. Information pertaining to
the design and construction of the Type-S pitot tube is presented in detail in Section 3.1.1 of EPA
Document 600/4-77-0275. Only Type-S pitot tubes meeting the required EPA specifications are
used. Pitot tubes are inspected and documented as meeting EPA specifications prior to field
sampling.
Sampling Nozzle Calibration. Glass nozzles are used for isokinetic sampling.
Calculation of the isokinetic sampling rate requires that the cross sectional area of the sampling
nozzle be accurately and precisely known. All nozzles are thoroughly cleaned, visually inspected
and calibrated according to the procedure outlined in Section 3.4.2 of EPA Document 600/4-77-
027b.
Temperature Measuring Device Calibration. Accurate temperature measurements
are required during source sampling. Bimetallic stem thermometers and thermocouple
temperature sensors are calibrated using the procedure described in Section 3.4.2 of EPA
Document 600/4-77-027b. Each temperature sensor is calibrated at a minimum of two points
over the anticipated range of use against a NIST-traceable mercury-in-glass thermometer. All
sensors are calibrated prior to field sampling.
Drv Gas Meter Device Calibration. Dry gas meters (DGMs) are used in the Method 5
sampling trains to monitor the sampling rate and to measure the sample volume. All DGMs are
calibrated to document the volume correction factor just prior to shipping of the equipment to the
field. Post-test calibration checks are performed as soon as possible after the equipment has been
returned to the ERG Laboratpry. Pre- and post-test calibration should agree to within 5%.
Prior to calibration, a positive pressure leak check of the system is performed using the
procedure outlined in Section 3.3.2 of EPA Document 600/4-77-237b. The system is placed
under approximately 10 inches of water pressure and a gauge oil manometer is used to determine
if a pressure decrease can be detected over a one-minute period. If leaks are detected, they are
eliminated before actual calibration are performed.
5-27
-------
After the sampling console is assembled and leak checked, the pump is to run for
15 minutes, to allow the pump and DGM to warm up. The valve is then adjusted to obtain the
desired flow rate. For the pre-test calibration, data are collected at orifice manometer settings
(AH) of 0.5, 1.0, 1.5, 2.0, 3.0 and 4.0 in H20. Gas volumes of 5 ft3 are used for the two lower
orifice settings, and volumes of 10 ft3 are used for the higher settings. The individual gas meter
correction factors (Yj) are calculated for each orifice setting and averaged. The method requires
that each of the individual correction factors fall within ±2% of the average correction factor or
the meter is cleaned, adjusted, and recalibrated. In addition, ERG requires that the average
correction factor be within 1.00 ±1%. For the post-test calibration, the meter is calibrated three
times at the average orifice setting and vacuum which were used during the actual test.
5.2.3 Method 26A Sampling Operations
5.2.3.1 Preliminary Measurements
Prior to sampling, preliminary measurements are required to ensure isokinetic sampling.
These preliminary measurements include determining the traverse point locations, performing a
preliminary velocity traverse and a cyclonic flow check. These measurements are used to
calculate a "K factor." The K factor is used to determine an isokinetic sampling rate from stack
gas flow readings taken during sampling.
Measurements are then made of the duct inside diameter, port nozzle length, and the
distances to the nearest upstream and downstream flow disturbances. These measurements are
then used to determine sampling point locations by following EPA Reference Method 1
guidelines. The distances are then marked on the sampling probe using an indelible marker.
5.2.3.2 Assembling the Train
Assembling the Method 26A sampling train components is begun in the recovery trailer
and final train assembly is performed at the stack location. First, the empty, clean impingers are
5-28
-------
assembled and laid out in the proper order in the recovery trailer. Each ground glass joint is
carefully inspected for hairline cracks. After the impingers are loaded, each impinger is weighed,
and the initial weight and contents of each impinger are recorded on a recovery data sheet. The
impingers are connected together using clean glass U-tube connectors and arranged in the
impinger bucket. The height of all the impingers is approximately the same to obtain a leak free
seal. The open ends of the train are sealed with Parafilm® or clean ground glass caps.
The second step is to load the filter into the filter holder in the recovery trailer. The
filter holder is then capped off and placed into the impinger bucket. To avoid contamination of
the sample, sealing greases are not used. The train components are transferred to the sampling
location and assembled as previously shown in Figure 5-4.
5.2.3.3 Sampling Procedures
After the train is assembled, the heaters are turned on for the probe liner and heated
filter box. When the system reaches the appropriate temperatures, the sampling train is ready for
pre-test leak checking. The gas stream exiting the heated filter is maintained at a temperature of
120 ±14°C (248 ±25°F). The filter temperature is initially set at 120 ±14°C (248 ±25°F) and the
probe temperature at 100°C (212°F). The temperature of these two heated zones will be
regulated as necessary to maintain the proper temperature of the gas exiting the filter.
The sampling trains are leak checked at the start and finish of sampling. (Method 26A
protocol requires post-test leak checks and recommends pre-test leak checks.) ERG protocol also
incorporates leak checks before and after every port change. An acceptable pre-test leak rate is
less than 0.02 acfm (ftVmin) at approximately 15 inches of mercury (in. Hg). If, during testing, a
piece of glassware needs to be emptied or replaced, a leak check is performed before the
glassware piece is removed, and after the train is re-assembled.
To leak check the assembled train, the nozzle end is capped off and a vacuum of
15 in. Hg is pulled in the system. When the system is evacuated, the volume of gas flowing
5-29
-------
through the system is timed for 60 seconds. After the leak rate is determined, the cap is slowly
removed from the nozzle end until the vacuum drops off, and then the pump is turned off. If the
leak rate requirement is not met, the train is systematically checked by first capping the train at
the filter, at the first impinger, etc., until the leak is located and corrected.
After a successful pre-test leak check has been conducted, all train components are at
their specified temperatures and initial data are recorded (dry gas meter (DGM) reading), the test
can be initiated. Sampling train data are recorded periodically (specific interval to be
determined) on standard data forms. A checklist for sampling is included in Table 5-9.
The leak rates and sampling start and stop times are recorded on the sampling task log.
Also, any other events that occur during sampling are recorded on the task log, such as pitot
cleaning, thermocouple malfunctions, heater malfunctions, or any other unusual occurrences.
At the conclusion of the test run, the sample pump (or flow) is turned off, the probe is
removed from the duct, a final DGM reading is taken, and a post-test leak check is completed.
The procedure is identical to the pre-test procedure; however, the vacuum should be at least
one inch Hg higher than the highest vacuum attained during sampling. An acceptable leak rate is
less than 4% of the average sample rate or 0.02 acfm (whichever is lower). If a final leak rate
on-site does not meet the acceptance criterion, the test run may still be accepted upon approval of
the EPA test administrator. If so, the measured leak rate is reduced by subtracting the allowable
leak rate from it and then multiplied for the period of time in which the leak occurred. This
"leaked volume" is then subtracted from the measured gas volume in order to determine the final
gas sample volume.
5.2.4 Method 26A Sample Recovery
Recovery procedures begin as soon as the probe is removed from the stack and the post-
test leak check is completed.
5-30
-------
Table 5-9. Sampling Checklist for EPA Method 26A
Before Test Starts:
1. Check impinger set (right order and number). Verify probe markings, and re-
mark if necessary.
2. Check that you have all the correct pieces of glassware.
3. Check for data sheets and barometric pressure.
4. Sampling equipment needs to be ready for Method 3 analysis.
5. Leak check pitot tubes.
6. Examine meter box - level it and confirm that the pump is operational.
7. Assemble train to the filter and leak check at 15 in. Hg. Attach probe to train
. and do final leak check; record leak rate and pressure on sampling log.
8. Check out thermocouples - make sure they are reading correctly.
9. Turn on heaters and check to see that their temperatures are increasing.
10. Check that cooling water is on and flowing (if required). Add ice to impinger
buckets.
11. Check isokinetic K-factor - make sure it is correct. (Refer to previous results to
confirm assumptions). (Two people should calculate this independently to
double check it).
12. Have a spare probe liner, probe sheath, meter box and filter ready to go at
location.
5-31
-------
Table 5-9. Sampling Checklist for EPA Method 26A (continued)
During Test:
1. Notify crew chief of any sampling problems ASAP. Train operator should fill in
sampling log.
2. Perform simultaneous/concurrent testing with other locations (if applicable).
Maintain filter temperature at 120 ±14° C (248 ±25° F). Keep temperature as
steady as possible. Maintain impinger temperatures below 68° F. Maintain
probe temperature above 100° C (212° F) or as required to maintain the proper
filter temperature.
3. Leak check between ports and record on sampling log.
4. Record sampling rate times and location for the fixed gas (CO2, O2) sample
(if applicable).
5. Blow back pitot tubes at inlet location every 15 minutes.
6. Change filter if pressure drop exceeds 20 in. Hg.
7. Check impinger silica gel every '/2 hr; if indicator changes color request a pre-
filled impinger from van lab and replace.
8. Check manometer fluid levels and zero every hour.
After Test is Completed:
1. Record final meter reading.
2. Check completeness of data sheet.
3. Do final leak check of sampling train at maximum vacuum during test.
4. Leak check each leg of pitot tubes.
5. Disassemble train. Cap sections. Take sections to recovery trailer.
5-32
-------
Table 5-9. Sampling Checklist for EPA Method 26A (continued)
6. Probe/cyclone recovery (use 500 mL bottles)
For acetone rinses (all trains)
Attach flask to end of probe (separate recovery containers will be
used for each sampling location)
Add 50 mL of acetone
Put a brush down probe, and brush back and forth
Rinse back and forth in probe
Empty out acetone in sample jar
Do this 3 times so that the final combined acetone rinse volume is
< 150 mL.
7. Reattach nozzle and cap for next day, store in dry safe place.
8. Make sure data sheets are completely filled out and give to location leader.
To facilitate transfer from the sampling location to the recovery trailer, the sampling
train is disassembled into three sections: the nozzle/probe liner, filter holder and impingers in
their bucket. Each of these sections is capped with Teflon® tape or Parafilm® before removal to
the recovery trailer. All train components are rinsed and the samples collected in separate,
prelabeled, precleaned sample containers to avoid cross contamination of inlet and outlet
samples. Trains of each type are recovered in separate areas of the mobile laboratory to avoid
cross contamination or mistakes in recovery sequences.
Once in the trailers, the sampling train is recovered as separate front and back half
fractions. A diagram illustrating front half and back half sample recovery procedures is shown in
Figure 5-5. No equipment with exposed metal surfaces is used in the sample recovery
procedures. The weight gain in each of the impingers is recorded to determine the moisture
content in the flue gas. Following weighing of the impingers, the front half of the train is
recovered, which includes the filter and all sample-exposed surfaces forward of the filter. The
5-33
-------
Probe Liner &
Nozzle
Rinse with
acetone
Brush liner with
Teflon brush
and rinse with
acetone
Rinse with
acetone
Front Half of
Filter Housing
Rinse 3x with
acetone
Filter
F. H.
Container #2
Remove filter from
support with tweezers
and place in petri
dish
Brush loose
paniculate onto filter
Seal petri dish with
®
Teflon tape
Container #1
Impingers 1 & 2
(0.1 NH2SO4)
Measure volume
in impingers 1-2
Rinse with
D.I. water
Container #3
Impingers 3 & 4
(0.1 NaOH)
Measure volume
in impingers 3-4
Rinse with
D.I. water
Add 25mg
Sodium
thiosulfate
Container #4
Silica Gel
Measure
weight
gain
Discard
Figure 5-5. Method 26A Sample Recovery Scheme
-------
probe liner is rinsed with acetone by tilting and rotating the probe while squirting acetone into its
upper end so that all inside surfaces are wetted. The acetone will be quantitatively collected into
the appropriate bottle. This rinse is followed by additional brush/rinse procedures using a non-
metallic brush; the probe is held in an inclined position and acetone is squirted into the upper end
as the brush is pushed through with a twisting action. All of the acetone and particulate will be
caught in the sample container. This procedure is repeated until no visible particulate remains
and finished with a final acetone rinse of the probe and brush. The front half of the glass filter
holder is also rinsed with acetone until all visible particulate is removed. These rinses are added
to the probe rinses. After all front half acetone washes are collected, the cap is tightened, the
liquid level marked and the bottle weighed to determine the acetone rinse volume. This sample
is Container #2. The method specifies that a nominal volume "of 100 mL of acetone must be used
for rinsing these components. For blank correction purposes, the exact weight or volume of
acetone used is measured. An acetone reagent blank of approximately the same volume as the
acetone rinses is analyzed with the samples.
The filter is carefully removed from the filter support and placed in a clean, well-
marked glass petri dish (Container # 1) and sealed with Teflon® tape.
After measuring the volume of liquid in the first four impingers and determining the
weight gain of the desiccant in the fifth impinger the contents of the first four impingers are
recovered.
The contents of the first and second impingers (0.1 N H2SO4) and the water rinses of the
impingers and connecting glassware are transferred to a separate container labeled "Container
No. 3." The contents of the third and fourth impingers (0.1 N NaOH) and the water rinses of the
impingers and connecting glassware are transferred to a separate container labeled "Container
No. 4." Add 25 mg of sodium thiosulfate to Container No. 4 and mix well. Seal the sample
bottles and package for transport to the laboratory for analysis.
5-35
-------
A reagent blank is recovered in the field for each of the following reagents:
• Acetone—200 mL sample size;
• Filter blank—one each;
0.1 N H2SO4 - 200 mL sample size; and
• 0.1 N NaOH - 200 mL sample size, containing 50 mg of sodium thiosulfate.
Each reagent blank is of the same lot as was used during the sampling program. The
volumes collected are greater than that required for sample preparation in order to provide
sufficient amounts in case of sample loss during preparation or to compensate for larger volumes
of train rinses. Each lot number and reagent grade is recorded on the reagent blank label.
One field blank was collected at each lime-injected baghouse inlet, and one at each
lime-injected baghouse outlet. A field blank is generated by preparing a sampling train as if for
actual sample collection, performing a leak check at the sampling location, then sealing the inlet
and outlet of the train and leaving it at the sampling location during the length of an actual test
run.
One glassware proof blank will be collected for each train prior to sampling. A proof
blank is generated by rinsing the components of a train, prior to use, with the recovery solvent(s)
specified in the method.
The liquid level of each sample container is marked on the bottle in order to determine
if any sample loss occurred during shipment. If sample loss has occurred, the sample may be
voided or a method may be used to incorporate a correction factor to scale the final results
depending on the volume of the loss.
5-36
-------
Following the protocol of Method 26A, the fractions to be collected for analysis from
each train are:
• Fraction 1—Filter;
• Fraction 2—Probe/nozzle/cyclone and filter front half acetone rinses;
• Fraction 3 - Contents of Impingers 1 and 2 plus water rinses; and
• Fraction 4 - contents of Impingers 3 and 4 plus water rinses.
5.2.5 HCI Analytical Procedures
Before analysis, the samples are checked against the chain of custody forms, logged into
the laboratory sample tracking system, and assigned a laboratory sample number. Each sample is
then examined to determine if any leakage occurred and any color or other particulars of the
samples are noted.
The samples are analyzed using ion chromatography (1C). Analytical conditions are
determined by the type of analytical column used and whether suppressed or nonsuppressed 1C is
used. Prior to-sample analysis, a stable baseline is established and water samples are injected
until no chloride, bromide, or fluoride appears in the chromatogram. The 1C is then calibrated
using standards spanning the appropriate concentration range, starting with the standard at the
lowest concentration. Next, a check sample is injected in duplicate, followed by a water blank
and field samples. The calibration standards are re-injected at the end of the analyses to allow
compensation for any drift in the instrument response during analysis of the field samples. The
chloride sample concentrations are calculated from either the ion peak area or the peak height
and the calibration curve.
5-37
-------
5.2.6 HCI Analytical Quality Control
The 1C is calibrated with a minimum of three concentrations, not including zero. A
correlation coefficient of greater than or equal to 0.995 must be achieved to have an acceptable
calibration. At least 10 percent of the total number of samples are analyzed in duplicate. Ion
concentrations in the duplicates must agree to within ± 20 percent.
5.2.7 Particulate Analysis
The general gravimetric procedure described in Method 5, Section 4.3 is followed.
Both filters and precleaned beakers are weighed to a constant weight before use. The same
balance used for taring is used for weighing the samples. The balance room is maintained at a
constant temperature and humidity. The preparation and analysis scheme for Method 5 is shown
in Figure 5-6. The particulate was determined as part of the Method 26A Train samples.
The filter (Container #1) is desiccated to a constant weight for a minimum of 24 hours
and then an initial weighing is performed. Weight gain is reported to the nearest 0.1 mg. A
second weight determination is made after again desiccating for a minimum of 6 hours.
"Constant weight" means a difference of no more than 0.5 mg or 1% of the total weight less tare
weight, whichever is greater, between two consecutive weighings made 6 hours apart. Report the
final weight as the average of these two values. The filter tare and final weights will be
determined under the same conditions of temperature and humidity.
The acetone rinses (Container #2) are transfer to a tared beaker, along with three
acetone rinses of Container #2, and evaporated to dryness at ambient temperature, placed in a
desiccator for 24 hours and weighed to a constant weight. The total volume of acetone used in
preparation of the sample is duplicated for the preparation of a reagent blank.
5-38
-------
Container #1
Container #2
Filter
Transfer to tared glass weighing dish
Desiccate to constant weight
Determine particulate filter weight
Front half rinses
Evaporate to dryness at ambient temperature and pressure
in a Tared heaker
I
Desiccate to constant weight
Determine PM weight
Figure 5-6. Method 5 Preparation and Analysis Scheme (Integral Part of Method 26A)
-------
5.2.8 Quality Control for Gravimetric Procedures
All quality control procedures specified in the test method are followed. All field
reagent blanks are processed and analyzed as specified in the test method. Prior to each
gravimetric determination, the balance calibration is verified using a series of certified weights
covering the range of weights encountered for the samples.
5.3 FTIR EPA Method 320
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.
5.3.1 FTIR Sampling Equipment
The FTIR measurement system met 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® coated, heated-head sample pump;
• FTIR spectrometer;
5-40
-------
• FTIR sample conditioning system; and
QA/QC apparatus.
Figure 5-7 illustrates the 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 which will remove any particulate matter
from the sample stream to protect the remainder of the sampling and analysis system. The probe
liner and filter body are made of glass, and the filter element is polytetrafluoroethylene (PTFE or
Teflon®). In addition to providing an inert surface, the glass body filter allows the operator to
observe the filter loading during sampling operations. The probe and filter are contained in a
heated box which is mounted on the stack and maintained at a temperature of 121 ° C (250° F).
After passing through the filter assembly, the sample gas is transported to the FTIR
spectrometer by a primary heat-traced PTFE sample line maintained at 149° C (300° F) driven
by a heated- PTFE head sample pump maintained at 204° C (400° F). The sampling flow rate
through the probe, filter, and sampling line is a nominal 20 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.
FTIR spectrometer sample gas is taken from the distribution manifold by a secondary
heated PTFE head sample pump maintained at 204° C (400° F) and directed into the FTIR
sample cell maintained at 185° C (365° F) for real-time analysis. The cell is made of nickel-
plated aluminum, with gold-plated glass substrate mirrors and potassium chloride windows.
Exhaust gas from the cell is vented to the atmosphere.
Sample conditioning (when required) is achieved by passing raw sample gas through a
PermaPure® drier 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 CO2
and other acid gases. The sample conditioning apparatus is switched into the FTIR sample
5-41
-------
N)
Heat-traced line
Sample
Gas In
Spike or QA/QC Gas
Vaporization
block
I
QA/QC Gas Standard Manifold
Main Sample Pump
Heated Flow Meter
Legend
Bold text and lines = Heated
Normal text and lines = Unheated
Heat-traced line
(up to 100 feet)
6
FPIR
Sample
Pump/
Flowmeter^
QA/QC Gas Standards
Sample Distribution Manifold
To Other Instruments
FTIR Sample Cell
Spiking Solution
Excess sample to
atmosphere
Exhaust to atmosphere
Fio"re 5-7. FTIR Sampling and Measurement System
-------
path by a valving system. Lower detection limits for some compounds can be achieved with a
conditioned sample.
5.3.2 Preparation for Sampling
The heated sampling lines, probes, and 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 was performed. The leak check was performed by
plugging the end of the probe and watching the main sample rotameter to see that the value goes
to zero.
A background spectrum was measured using zero air or zero nitrogen through the cell.
Next the QC gases were measured by flushing the cell and they must agree to within ±10% of
target value. The QC gases used for this program included:
Halocarbon 22, 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 ±5 percent of
certified concentration;
Methane/nitric oxide/carbon dioxide mixture, used for overall system
performance check (calibration transfer standard) (acceptance limits are ±5% of
the certified concentration); and
Hydrogen chloride standard, analyzed to verify the instrumental response of HC1,
a key target analyte (acceptance limits are ±10% of certified concentration).
The sampling and measurement system spike test was used 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
5-43
-------
"Measurement of Vapor Phase Organic and Inorganic Emissions By Extractive Fourier
Transform Infrared Spectroscopy". Section B. l.C of Method 320 gives a description of the
dynamic spiking apparatus.
The FTIRS spiking procedure used was the following:
• Measure native stack gas for a 5 minute period;
• Start spike gas flow into sample stream, upstream of the heated filter;
• Let system equilibrate for 5 minutes;
• Measure spiked sample stream for 5 minutes;
• Turn off spike gas flow;
• Let system equilibrate with native stack gas for 5 minutes; and
• Repeat cycle, two more times.
The above procedure produces 3 spiked/unspiked sample pairs per hour. Spike
recovery and three relative standard deviations for 3 spiked/unspiked sample pairs were
computed from the procedure given in Section 8.6.2 of EPA Draft Method 320. The recovery
must be 70-130% and the Percent Relative Standard Deviation must be less than or equal to 50%
for the method to be valid for this source category.
The spiked/unspiked pairs are not simultaneously recorded, since only one FTIRS
system will be available, but due to the expected steady nature of the source, this procedure
produced acceptable results.
The FTIR sampling and analysis system was validated for HCI at the outlet of the chip
dryer baghouse and the inlet and outlet of the reverberatory furnace #1 and was used as a
screening tool for the other HAPs.
5-44
-------
5.3.3 Sampling
FTIR sampling was performed simultaneously with the manual testing. The start and
stop times, as well as port change times, were coordinated with the bilk operator, so that FTIR
data files could be coordinated with manual method start and stop times. FTIR inlet/outlet
sampling was accomplished using two heated transfer lines, using a valving system to switch
from one to the other.
Table 5-10 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 1-1000 ppm). Some of these parameters are sample matrix dependent.
Table 5-10. 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 - 4000
0.5 (or better)
3.2 (variable-- 1-10)
185
9 (3.0 optical cell volumes/minute)
1 (Average of 40 spectra)
Sample flow rate was determined by the data averaging interval and FTIR spectrometer
sample cell volume. A minimum of 3 sample cell volumes of gas must flow through the 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 liters per
minute (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.
5-45
-------
The temperature of all sampling system components were nominally 221-204° F (250-
400° C) to prevent condensation of water vapor or other analytes in the sampling system. The
Kl'lR sample cell temperature was maintained at 365° F (185° C) to ensure that condensation of
high-boiling point analytes on the cell optics is minimized.
FTIR sample cell pressure was monitored in real-time in order to calculate analyte
concentration in parts-per-million. It is normally operated near atmospheric pressure with the
cell pressure continuously monitored.
Stack gas temperature was also be monitored to provide information on potential
sample analyte condensation in the sampling system. If the stack gas temperature is higher than
the lowest sampling system component temperature, then an assessment by the spectroscopist or
field team leader must be made whether any analytes of interest may condense within the
sampling system, resulting in measurement bias.
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 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 manual test methods.
Before testing, sample matrix effects were assessed on-site by the spectroscopist and
adjustments to the optical pathlength and spectral analysis regions were made. Once the
adjustments have been made, they rarely need to be further refined at a given source type.
Sampling and analysis procedures are straightforward for a single-source measurement.
Once QA/QC procedures have been completed for a given test day, the sample is allowed to flow
continuously through the FTIR spectrometer cell and the software is instructed to start spectral
data collection. Usually, the spectrometer collects one interferogram per second and averages a
number of interferograms to form a time-integrated interferogram. Typical averaging times
5-46
-------
range from 1 to 5 minutes. The interferogram is converted into a spectrum and analyzed for the
target analytes. After spectral analysis, the spectrum is stored on the computer and later
permanently archived. Spectral data collection is stopped after a pre-determined time,
corresponding to a "run".. Typical runs were 4 hours long, giving 240 one-minute averaged
points for each target analyte. At the end of the test day, the end-of-day QA/QC procedures were
conducted.
Before any testing is started at a given site, an initial "snapshot" of the stack gas is
taken with the FTIR measurement and analysis system to determine the true sample matrix. If
any target analytes are present at significantly higher levels than expected, adjustments will be
made to the cell pathlength and/or the spectral analysis regions used for quantitative analysis.
These adjustments will minimize interferences due to unexpectedly high levels of detected
analytes.
Since sample conditioning was required for certain analytes, the FTIR spectrometer
divided its analysis time between conditioned and unconditioned samples. Usually, the analysis
time is split into blocks to minimize dead time due to switching between sample types. For
example, the first half of the run period is dedicated to conditioned samples, and the last half of
the run is committed to unconditioned samples. The order used at Gulp Aluminum Alloys is
shown in the table below.
Sampling
Conditions
Chip Dryer
Unconditioned
Chip Dryer
Conditioned
Furnace
Unconditioned
Furnace
Conditioned
Furnace
Unconditioned
Sampling Time
First half of Test
Second half of
Test
First half of
Charging
Second half of
Charging
Duration of
Mixing Top Out
Inlet
2 minute cell purge
8 minute sample collection
2 minute cell purge
8 minute sample collection
2 minute cell purge
8 minute sample collection
2 minute cell purge
8 minute sample collection
2 minute cell purge
8 minute sample collection
Outlet
2 minute cell purge
8 minute sample collection
2 minute cell purge
8 minute sample collection
2 minute cell purge
8 minute sample collection
2 minute cell purge
8 minute sample collection
2 minute cell purge
8 minute sample collection
5-47
-------
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
every 10 minutes to provide twelve ten-minute sample collections during each two-hour period.
FTIR method performance is gauged from the results of the QA/QC procedures given in
Section B5 of Draft EPA Method 320. Acceptable spiking tests must meet acceptance criteria of
50 percent relative standard deviation (RSD) and accuracy of within ± 30 percent. The
acceptable instrument diagnostic and system response check accuracy must be within ± 5 percent
of target. Acceptable system response check precision was 5 percent RSD.
The ERG validated spectral database includes the compounds shown in Table 5-11.
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 spectral acquisition.
5.3.4 FTIR Method Data Review, Validation, and Verification Requirements
Quantitative analysis is 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 non-linear correction, possibly even at levels as low as 100 ppm-meters (concentration
times pathlength). Analytes greater than 50-60 amu molecular weight usually do not require non-
5-48
-------
Table 5-11. Compounds for Which Reference FTIR Spectra Are Available in the
ERG Spectral Library3
1,3-butadiene
1-butene
2-methyl-2-propanol
2-methylbutane
2-methoxyethanol
2-methyIpropane
2-propanol
4-vinylcyclohexane
acetic acid
acetone
acrolein
benzene
acetylene
c/.y-2-butene
fra/i5-2-butene .
ethylene
ethane
propylene
propane
chlorobenzene
acetaldehyde
methanol
methane
carbon monoxide
carbon dioxide
cyclopropane
cvclopentane
cyclohexane
ethylbenzene
formaldehyde
water vapor
hydrogen chloride
hydrogen fluoride
isobutylene
methylene chloride
methyl ethyl ketone
m-xylene
p-xylene
o-xylene
phenol
o-cresol
m-cresol
/7-cresol
nitrous oxide
n-butane
/i-butanol
ammonia
nitric oxide
nitrogen dioxide
H-pentane
carbonyl sulfide
sulfur dioxide
styrene
toluene
' Spectra were collected at a cell temperature of 185° C.
5-49
-------
linear corrections. An experienced spectroscopist can determine whether non-linear corrections
are necessary for an analyte in a given source testing scenario.
The following procedures were conducted to review the FTIR data:
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 which
was taken immediately prior in time to the indicated time region.
4. Manually quantitate (including any non-linear corrections) for the species in
question and compare the result to. the difference in software-computed
concentrations for respective spectra.
5. If concentration values in Step 4 do not agree to within 5 percent, determine
whether the difference is due to a recoverable or non-recoverable error.
6 (i). If the error is non-recoverable, the spectra in the indicated time region are
declared invalid.
6 (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.
7. Determine the peak-to-peak scatter or the root mean square (RMS) noise-
equivalent-absorbance (NEA) for the representative spectra.
8. If the NEA exceeds 1 x 10"3 absorbance units, the spectra in the time region are
declared invalid (due to non-recoverable error).
9. Data found invalid are subject to re-measurement.
5-50
-------
B. Final Data Review (off-site)
The procedures for final data review included those given above; however, if a non-
recoverable error was found during this phase, the data were considered invalid. In addition, the
following procedures were 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 which were not detected or detected at low levels:
a) estimate detection limits from validated data;
b) check for measurement bias.
5.3.5 QCfortheFTIR
The FTIR QA/QC apparatus was used to perform two functions:
• Dynamic analyte spiking; and
• Instrumental performance checks.
Dynamic analyte spiking is 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.
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.
5-51
-------
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. . "
Before any testing is started at a given site, an initial "snapshot" of the stack gas is taken
with the FTIRS measurement and analysis system to determine the true sample matrix. If any
target analytes are present at significantly higher levels than expected, adjustments will be made
to the cell pamlength and/or the spectral analysis regions used for quantitative analysis. These
adjustments will minimize interferences due to unexpectedly high levels of detected analytes.
FTIRS method performance is gauged from the results of the QA/QC. Acceptable
spiking tests will meet Method 301 criteria (i.e., 50 percent relative standard deviation (RSD)
and accuracy of within ± 30 percent) or a statistical equivalent when less than 12 spiked/unspiked
pairs are collected. The acceptable instrument diagnostic and system response check accuracy
will be within ± 5 percent of target. Acceptable system response check precision will be
5 percent RSD.
5-52
-------
6.0 QUALITY ASSURANCE/QUALITY CONTROL
Specific Quality Assurance/Quality Control (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
train leak checks met the QC criteria as specified in the methods. Isokinetic sampling rates were
kept within 10% of 100% for all test runs. Acceptable spike recoveries and close agreement
between duplicate analyses were shown for the sample analyses: The data completeness was
better than 95%. .
6.1 Sampling QC Results
The following sections discuss the QC results of the sampling methods employed during
this project.
6.1.1 Leak Checks
Tables 6-1 and 6-2 list the pre- and post-test and port change leak checks results for the
chip dryer and furnace tests. The acceptance criterion that all post-test leak checks must be less
than 0.02 cfm or 4 percent of the average sampling rate (which ever is less) at the highest
vacuum achieved during sampling was met for all test runs.
6-1
-------
Table 6-1. Summary of Dioxin/Furan Test Leak Check Results
Location
CD Outlet
CD Outlet
CD Inlet
CD Inlet
CD Outlet
CD Outlet
CD Inlet
CD Inlet
CD Outlet
CD Outlet
CD Inlet
CD Inlet
RF Outlet
RF Outlet
RF Inlet
RF Inlet
RF Outlet
RF Outlet
RF Inlet
RF Inlet
RF Outlet
RF Outlet
RF Inlet
RF Inlet
RF Outlet
RF Outlet
RF Inlet
RF Inlet
Run#/
Port
I/A
1/B
I/A
1/B
2/A
2/B
2/A
2/B
3/A
3/B
3/A
3/B
I/A
1/B
I/A
1/B
2/A
2/B
2/A
2/B
3/A
3/B
3/A
3/B
4/A
4/B
4/A
4/B
Initial Leak
Check
0.018@15"
0.006@15"
0.02@15"
0.016@23"
0.00@10"
0.00@14"
0.01 @ 10"
0.018@16"
0.01 @ 12
0.018@15"
0.01 @ 11"
0.015@ll"
0.01 @ 10"
0.01 1@ 10"
Port
Change
0.01 @ 10"
0.01 @ 10"
0.008 @23"
0.01 @23"
0.01 @ 10"
0.01 @ 10"
0.016@21"
0.018@18"
0.01 @ 10"
0.01 @ 10"
0.00@11"
0.00@H"
Not Recorded
Not Recorded
0.008® 8"
0.008 @8"
Not Recorded
Not Recorded
0.005 @ 10"
0.005 @ 10"
Not Recorded
Not Recorded
0.00@7"
0.00@7"
0.015@15"
0.015@15" .
0.006@5"
0.006@5"
Final Leak
Check
0.01 @ 15"
0.005 @ 8"
0.01 @ 15"
0.01 @8"
0.01 @ 10"
0.003 @ 10"
0.00@10"
0.006@7"
0.005@11"
0.00@10"
0.005@5"
0.00@6"
0.005® 10"
0.004® 8"
6-2
-------
Table 6-2. Summary of HCI/PM Test Leak Check Results
Location
CD Outlet
CD Outlet
CD Inlet
CD Inlet
CD Outlet
CD Outlet
CD Inlet
CD Inlet
CD Outlet
CD Outlet
CD Inlet
CD Inlet
RF Outlet
RF Outlet
RF Inlet
RF Inlet
RF Outlet
RF Outlet
RF Inlet
RF Inlet
RF Outlet
RF Outlet
RF Inlet
RF Inlet
RF Outlet
RF Outlet
RF Inlet
RF Inlet
Run#/
Port
I/A
1/B
I/A
1/B
2/A
2/B
2/A .
2/B
3/A
3/B
3/A
3/B
I/A
1/B
I/A
1/B
2/A
2/B
2/A
2/B
3/A
3/B
3/A
3/B
4/A
4/B
4/A
4/B
Initial Leak
Check
0.01@10"
0.01 1@ 13"
0.01 @ 15"
0.01 @ 15"
0.01 @ 10"
0.005 @ 14"
0.01 @ 10"
0.02@15"
0.01 @9"
0.005 @ 10"
0.01 @ 10"
0.004@ 10"
0.02 @ 12"
0.012@9"
Port
Change
0.01@10"
0.01 @ 10"
Not Recorded
Not Recorded
0.01 @ 10"
0.01 @ 10"
0.009@7"
0.009@7"
0.01 @ 10"
0.01 @ 10"
0.00@6"
0.00@6"
0.01 @ 10"
0.01 @ 10"
0.016@6"
0.016@6"
Not Recorded
Not Recorded
0.00@8"
0.00@ 10"
Not Recorded
Not Recorded
0.00@5"
0.00@5"
0.01 @ 10"
0.01 @ 10"
0.009@9"
0.009@9"
Final Leak
Check
0.01 @ 15"
0.00@13"
0.01@10"
0.007@11"
0.01 @ 10"
0.0046® 8"
0.00@12"
0.004 @ 8"
0.01 @ 10" •
0.008@8"
0.005 @ 10"
0.00@5"
O.OI5@12"
0.00@7"
6-3
-------
6.1.2 Percent Isokinetics
Table 6-3 presents the isokinetic sampling rates percentages for the D/F and HC1/PM
sampling runs. The acceptance criteria that the average sampling rate must be within 10% of
100% isokinetic was met for all sampling runs.
Table 6-3. Summary of Isokinetic Percentages
Location/Method
CD Inlet D/F
CD Outlet D/F
CD Inlet HC1/PM
CD Outlet HC1/PM
RF Outlet D/F
RF Inlet D/F
RF Outlet HC1/PM
RF Inlet HC1/PM
Run#
1
2
3
1
2
3
1
2
3
1
2
3
1
2
3
4
1
2
3
4
1
2
3
4
1
2
3
4
Percent Isokinetic
97.5
101
98.4
102
98.5
96.9
104
100
101
102
101
103
97.9
98.3
98.5
96.9
101
102
101
101
96
103
103
102
102
102
101
106
6-4
-------
6.1.3 Meter Box Calibrations
All dry gas meters are fully calibrated every six months against an EPA approved
intermediate standard. The full calibration is used to correct the actual metered sample volume
to the true sample volume. To verify the full calibration, a post-test calibration is performed.
The full and post-test calibrations must be within 5% to meet ERG's internal QA/QC acceptance
criterion. As shown in Table 6-4, the dry gas meters used for this testing met this criterion.
Table 6-4. Dry Gas Meter Post-Test Calibration Results
Sampling
Train1
D/F CD Outlet
D/F CD Inlet
HC1 CD Outlet
HC1 CD Inlet
D/F RF Outlet
D/F RF Inlet
HC1 RF Outlet
HC1 RF Inlet
Meter Box #
A-38
A-40
A-37
A-39
A-37
A-39
A-38
A-40
Full Calibration
Factor
0.981
0.98
0.988
0.994
0.988
0.994
0.981
0.98
Post-Test
Calibration
Factor
0.978
0.979
0.995
0.974
0.995
0.974
0.978
0.979
Post-Test2
Deviation, %
-0.30
-0.10
-0.70
-2.00
-0.70
-2.00
-0.30
-0.10
'CD=Chip Dryer, RF=Reverberatory Furnace
2Post-Full x 100
Full
6.1.4 Field Blank Results
Field Blanks are collected to determine the level, if any, of sample contamination
resulting from the exposure of the sampling train to ambient conditions in the vicinity of the
sampling locations or to sample "carry over" from one run to the next. A field blank train for
each test method and for each location was assembled as if for sampling, leak checked at the
6-5
-------
sampling location, left at the sampling location for the duration of a test run and then recovered.
The samples were returned to the laboratory for analysis along with the test samples. The results
of the analysis for the Method 26A field blanks are shown in Table 6-5. A small amount of HC1
was detected in the Chip Dryer field blank, but represents less than 1% of the amount detected in
most of the test samples and less than 5% of that detected in all samples. Because the level of
contamination was so low, no blank corrections were made on the emission results. No HC1
above the instrument detection limit was detected in the furnace field blanks.
Table 6-5. Method 26A Field Blank Analysis Results, |jg Detected
Location
Chip Dryer Inlet
Chip Dryer Outlet
Reverberatory Furnace Inlet
Reverberatory Furnace Outlet
Mg HC1 Detected
20.0
Not Required
< 14.0
< 14.0
Table 6-6 shows the results of the analysis of the D/F field blanks. The levels detected in
the blank are less than 1% of that detected for any congener in the chip dryer inlet samples and
less than 1% for most and less than 5% for all detected in the chip dryer outlet samples except for
OCDD and OCDF. The levels detected in the furnace inlet field blank were less than 1% for
most congeners and less than 5% for all except for 2,3,7,8-TCDD and 1,2,3,7,8-TCDD which
were less than 10%. Trace amounts of all but three congeners were detected in the furnace outlet
field blank. Of the ones detected all but seven were less than 5 times the detection limit and the
others were less than 10 times the detection limit. All but six of the congeners were at levels
equivalent to those found in the furnace outlet samples and all were detected at levels less than
one nanogram.. Since the levels detected were insignificant, no blank correction to the data was
performed. .
6-6
-------
Table 6-6. Method 23 Field Blank Analysis Results, ng Detected
Congener
2,3,7,8 -TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
1,2,3,4,6,7,8,9-OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2.3,7.8.9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
1,2,3,4.6,7,8,9-OCDF
Chip Dryer Inlet
<0.006
0.04
0.02
0.04
0.05
0.12
0.25
0.45
0.14
0.22
0.31
0.12
0.14
0.02
1.2
0.17
0.41
Furnace Inlet
0.07
0.48
0.26
0.46
0.57
1.2
0.65
7.6
1.7
2.9
6.0
2.3
2.4
0.15
6.1
0.72
1.5
Furnace Outlet
<0.004
0.02
<0.01
0.02
0.03
<0.09
0.16
0.29
0.07
0.12
0.23
0.09
0.12
<0.007
0.43
<0.05
0.31
6.1.5 FTIR Sampling Quality Control
FTER sampling system quality control procedures used in this test program were:
• Sampling system leak check;
• Dynamic spiking (also analytical quality control); and
• Monitoring of all pertinent system temperatures and flow rates.
6-7
-------
Sampling system leak checks were carried out before and after each run. The leak check
procedure used is identical to that given in EPA Method 320. The sample gas inlet to the probe
was covered and the total sample flow rate rotameter was monitored to observe zero flow
(i.e., indicator ball sits on bottom of scale). In all cases in this program, the system passed both
before and after run leak checks for all runs performed.
Dynamic spiking was carried out to test the complete FTIR sampling and analysis system.
Spiking was carried out twice daily on both inlet and outlet for HC1, and three EPA Method 301
validation tests were carried out. The Method 301 tests were carried out on the following
locations:
• Chip dryer outlet;
• Furnace hood inlet; and ,
• . outlet.
Method 301 validation results are given in Section 2.5.2.1. Daily spiking results are given below
in Section 6.2.4.
To insure that the sampling system was performing correctly during all measurement
operations, selected temperatures and flows were monitored during each run. Temperature data
were recorded every 15 minutes on a data sheet. Sample flows were monitored but not recorded.
The following data were monitored or recorded:
• Inlet/outlet stack temperature; .
• Inlet/outlet probe temperature;
• Inlet/outlet filter temperature;
• Inlet/outlet heat-traced sample line temperature;
• Inlet/outlet main sample pump head temperature;
6-8
-------
• FTIR sample pump head temperature;
• Sample pump enclosure temperature;
• Sample manifold temperature;
• Controller electronics box temperature;
• Heated sample line jumper temperature(2);
• Main sample flow rate;
• FTIR sample flow rate; and
• Excess sample flow rate.
FTIR cell temperature was controlled at 185°C sample gas temperature (not cell wall
temperature), and cell pressure was recorded. No unusual readings of any parameter were found
during testing.
6.2 Analytical Quality Control Results
6.2.1 D/F Analytical Quality Control
All quality control procedures specified in the test method were followed. Blanks were
used to determine analytical contamination, calibration standards were used for instrument
calibration and linearity checks, internal standards were used to determine isomer recoveries and
adjust response factors for matrix effects, surrogate standards were used to measure the
collection efficiency of the sampling methodology and an alternate standard was used as a
column efficiency check.
6.2.1.1 D/F Quality Control Blanks
Reagent blanks of 500 mL of each liquid reagent used at the test site were saved for
analysis. Each reagent blank was of the same lot as was used during the sampling program.
6-9
-------
Each lot number and reagent grade was recorded on the field blank label and in the laboratory
notebook (acetone, methylene chloride, toluene, filter, XAD-2®). Two reagent blanks were
collected in the field. The analysis results showed the absence of any analytes, at the detection
limit, for approximately half of the congeners with the remaining being detected at less than 5
times the detection limit. These insignificant amounts are most likely due to laboratory
contamination.
6.2.1.2 Quality Control Standards
Recoveries of the internal standards must be between 40 to 130% for the tetra- through.
hexachlorinated compounds and in the range of 25 to 130% for the hepta- and octachlorinated
homologs. These requirements were met for all of the D/F samples except for the following:
chip dryer inlet Run 1, isotopically labeled HpCDD (134%).
Surrogate standard recoveries must be between 70 to 130%. The recoveries of all
standards met this requirement except for the following: isotopically labeled HxCDD for chip
dryer outlet run 1 (158%), chip dryer outlet run 2 (137%) and chip dryer outlet run 3 (142%).
These % recoveries were all just outside of the recovery limits and will not have an effect on the
analysis results.
6.2.2 HCI Analytical Quality Control
The IG is calibrated with a minimum of three concentrations, not including zero. A
correlation coefficient of greater than or equal to 0.995 must be achieved to have an acceptable
calibration. At least 10 percent of the total number of samples are analyzed in duplicate. Ion
concentrations in the duplicates must agree to within ± 20 percent. All QC results were within
the acceptance criteria
Reagent blanks were collected in the field and returned to the laboratory for analysis.
HCI, as Cl'1, was not detected in any of the blanks at the detection limit.
6-10
-------
Every sample was analyzed in duplicated with the relative percent difference for every
sample duplicate less than 5.
A matrix spike and matrix spike duplicate analysis was performed on the chip dryer outlet
run 1 sample. The percent recoveries were 106 and 104, respectively.
6.2.3 Quality Control for Gravimetric Procedures
All quality control procedures specified in-the test method are followed. All field reagent
blanks were processed and analyzed as specified in the test method. Prior to each gravimetric
determination, the balance calibration was verified using a series of certified weights covering
the range of weights encountered for the samples.
6.2.4 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. EPA Method 320 limits the dilution of the sample gas to
10 percent.
Before any testing was started at a given site, an initial "snapshot" of the stack gas is
taken with the FTIR measurement and analysis system to determine the true sample matrix. If
any target analytes are present at significantly higher levels than expected, adjustments were
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.
6-11
-------
FTIR method performance is gauged from the results of the QA/QC. All spiking tests
met Method 301 criteria (i.e., 50 percent relative standard deviation (RSD) and accuracy of
within ± 30 percent). The acceptable instrument diagnostic and system response check accuracy
will be within ± 6 percent of target.
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; and
• direct measurement of a CH4, NOX, and CO2 standard.
Dynamic spiking runs were conducted twice daily: before and after testing. Three
spiked/unspiked data pairs were collected. Statistical calculations consistent with EPA Method
301 were performed on the data. Recovery of 70-130 percent and less than 50 percent RSD were
the acceptance criteria. Table 6-6 summarizes 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, and a CH4, NOX 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
+ NO2. Examination of Tables 6-7 through 6-9 shows that all QC checks met the above criteria.
6-12
-------
Table 6-6. QC Spiking Results
Run
1
1
2
2
3
3
4
5
6
6
7
7
8
8
9
9
10
10
11
12
13
13
14
14
Date
12/5/97
12/5/97
12/5/97
12/5/97
12/6/97
12/6/97
12/6/97
12/6/97
12/8/97
12/8/97
12/8/97
12/8/97
12/9/97
12/9/97
12/9/97
12/9/97
12/10/97
12/10/97
12/10/97
12/10/97
12/11/97
12/11/97
12/11/97
12/11/97
Time
AM
AM
PM
PM
AM
AM
PM
PM
AM
AM
PM
PM
AM
AM
PM
PM
AM
AM
PM
PM
AM
AM
PM
PM
Inlet/outlet
outlet
inlet
outlet
inlet
inlet
outlet
outlet
inlet
outlet
inlet
outlet
inlet
inlet
outlet
inlet
outlet
inlet
outlet
inlet
outlet
inlet
outlet
inlet
outlet
% Recovery
97.61
112.85
102.62
98.09
93.71
101.91
105.34
103.53
99.97
96.34
95.40
89.50
94.54
100.85
106.45
103.16
96.21
103.44
104.00
110.78
101.36
102.84
107.16
118.67
Sample gas dilution was held to 10 percent or less in all runs.
6-13
-------
Appendix A
Field Data Sheets
cah/A:\APPX-CVRWP6
-------
Facility: Gulp Alum. Alloy
Date: 12/05/97
Location: Dryer In
Run Number: 1
Sample Type: M26
Total Sampling Time (min) 240.0
Corrected Barometric Pressure (in Hg) 29.39
Absolute Stack Pressure (in Hg) 29.02
Stack Static Pressure (in H2O) -5.00
Average Stack Temperature (°F) 244.13
Stack Area (sq in) 240.53
Actual Meter Volume (cu ft) 70.339
Average Meter Pressure (in H2O) 0.24
Average Meter Temperature (°F) 60.00
Moisture Collected (g) 110.10
Carbon Dioxide Concentration (%V) 0.5
Oxygen Concentration (%V) 20.0
Nitrogen Concentration (%V) 79.5
Dry Gas Meter Factor 0.9940
Nozzle Diameter (in) 0.131
Pitot Constant 0.84
Average Sampling Rate (dscfm) 0.291
Standard Metered Volume (dscf) - 69.785
Standard Metered Volume (dscm) .. 1.976
Stack Moisture (%V) 6.92
Mole Fraction Dry Stack Gas 0.931
Dry Molecular Weight 28.88
Wet Molecular Weight 28.13
Stack Gas Velocity (fpm) 4428.45
Stack Gas Velocity (mpm) 1349.79
Volumetric Flow Rate (acfm) 7396.99
Volumetric Flow Rate (acmm) 209.48
Volumetric Flow Rate (dscfm) 5007.09
Volumetric Flow Rate (dscmm) 141.80
Percent Isokinetic 103.63
Percent Excess Air 1992.23
Concentration (g/dscm) 0.00
Concentration (kg/hr) 0.00
Concentration (ppmv) 0.00
Emissions (Ib/hr) 0.00
-------
Eastern Research Group. Inc.
MODIFIED METHOD 5 DATASHEET
Run
Page 1 of
Plant tio.ll)
Date
Operator
Sampling Location T>UV£>
' i?jwcw/w (in
UoL
\
2rt" -•£.&
7-4, '*?
XAD Trap Number
Filter Heater Setting (°F)
Probe Length & Type
Probe Heater Setting (°F)
Minimum Sample Volume (ft3)
Initial Leak Check
Final Leak Check
«S\
rg *ju
H-'6Llrt5
">VZ>
NlA
61
Meter Box Number
Meter delta H @
PGM Factor (Y)
Nozzle Type & ID (in.)
Ambient Temperature (°F)
Assumed Moisture (% H2O)
K-Factor
A^l
1-TZ-
• ^V^t
«i^5\
M *r
t;n >
^^n
.,,v
r?.~s/ A- ii-LO^I.^L^ DlagramofDud
Schematic of Traverse Point Layout
Read and record all data every ^S__ minutes
Traverse
Point
Number
Sampling
Time
(mln)
0
Clock
Time
(24hr)
Gas
Meter
Reading
((Vm).ft3)
Velocity
Head
((delta Ps).
in.H20)
Stack
Ts
CF)
Orifice Pressure
Differential
(delta H. in.H2O)
Desired Actual
Probe
Temp.
(•F)
Filter
Temp.
(•F)
Adsorbent
Trap
Temp.
Dry Gas Meter
Inlet
(Tm in)
Outlet
(Tm out)
Impinger
Exit
Temp.
CF)
Pump
Vacuum
(in.Hg)
'
it
•3- "50
ST3
ac-
/r
aO^O
.3
3
\
Z3S
^
HfO
ft
(1,
H-7
ji
42-.
2-?
SN
.2.3
i-
L/"
v-s
\\3
-------
Plant
Date
Location
Sample Type
Run Number
Operator
Page
Traverse
Point
Number
Sampling
.Time
(min)
Clotk
Time
(24hr)
Meter
Reading
Velocity
Head
((delta Ps),
in.H20)
Stack
Ts
(T)
Orifice Pressure
Differential
(delta H, in.H2O)
Desired
Actual
Probe
Temp.
(•F)
Filter
Temp.
•CF)
Adsorbent
Trap
Temp.
Dry Gas Meter
Inlet
(Tm in)
Outlet
(Tm out)
Impinger
Exit
Temp.
(eF)
Pump
Vacuum
(in.Hg)
B 1
."Z.
S/
IL
11
no*
.IB
si
LLL
-TA
.-7,1
LOT
\-\
SI
l-l
:T,\
-Z.
c-0-
/ .
(1
I5"
-r
10
/.r
rr
? T
t-r-
(O
(.5-
\ ,
J5
-Z
UO
*
25
GO
-2.40
./TD.C
Comments:
-------
frt
:n Group, inc.
MOISTURE RECOVERY FORM FOR METRO
Plant
Date
Sampling Location
SampleType
Run Number
Impinger Box Number
Recovery Person
Recovery Rinses
Sample Identification
Filter Number
XAD Number
P.I Q 1 ' Q ii
^ -IxJrt M \\: _IY\ i fS i Lf-rA I*11lnV5
r> L' /\ Ti L ~t— ^f
L ./i '.^ / JA ji°r- • no/?rvv i<*» i r\ (^ 1
^P1 ' *
no.rr AJnU /Tt^V C,.wi<'.n
7
//q'(^97-jQ
Impinger
Number
Impinger
Solution
Amount of
Solution
(g)
Impinger Tip
Configuration
Impinger Weight
Final
Initial
(9)
Weight
Gain
O.i V
Hf r~\
z.^^n
31.3
/S/c^CH
77..T
(CD
0"
Total Weight Gain (g)
-------
Facility: Gulp Alum. Alloy
Date: 12/06/97
Location: Dryer In
Run Number: 2
Sample Type: M26
Total Sampling Time (min) 240.0
Corrected Barometric Pressure (in Hg) 29.51
Absolute Stack Pressure (in Hg) 29.14
Stack Static Pressure (in H2O) -5.00
Average Stack Temperature (°F) 238.46
Stack Area (sq in) 240.53
Actual Meter Volume (cu ft) 74.692
Average Meter Pressure (in H20) 1.22
Average Meter Temperature (°F) 47.94
Moisture Collected (g) 60.70
Carbon Dioxide Concentration (%V) 0.5
Oxygen Concentration (%V) 20.0
Nitrogen Concentration (%V) 79.5
Dry Gas Meter Factor 0.9940
Nozzle Diameter (in) 0.130
Pitot Constant 0.84
Average Sampling Rate (dscfm) 0.318
Standard Metered Volume (dscf) 76.206
Standard Metered Volume (dscm) . 2.158
Stack Moisture (%V) 3.62
Mole Fraction Dry Stack Gas 0.964
Dry Molecular Weight 28.88
Wet Molecular Weight 28.49
Stack Gas Velocity (fpm) 4833.21
Stack Gas Velocity (mpm) 1473.16
Volumetric Flow Rate (acfm) 8073.08
Volumetric Flow Rate (acmm) 228.63
Volumetric Flow Rate (dscfm) 5728.25
Volumetric Flow Rate (dscmm) 162.22
Percent Isokinetic , 100.45
Percent Excess Air 1992.23
Concentration (g/dscm) 0.00
Concentration (kg/hr) 0.00
Concentration (ppmv) 0.00
Emissions (Ib/hr) 0.00
-------
Eastern Research Group. Inc.
MODIFIED METHOD 5 DATA SHEET
«i •
Run 0*2-
Page 1 of 2,
Plant OuLf
Date
Operator
Sampling Location <)ry-«v b
Sample Type
Run Number
StatitrPreSsure (±) (in. H2O)
Barometric Pressure (in. H2O)
qiu/nnvj^ «
t9--l*- 17
«*/4-O
}rVi>i<* 10
/Wit-L
oz.
- i
t1.£i
XAD Trap Number
Filter Heater Setting (°F)
Probe Length & Type
Probe Heater Setting (*F)
Minimum Sample Volume (ft3)
Initial Leak Check
Final Leak CheCk
fJlA
O^b
<4'£l(4,.y
Z^D
Ma
.Oio^jS1
' ' * * Q
Meter Box Number
Meter delta H @
DGM Factor (Y)
Nozzle Type & ID (In.)
Ambient Temperature (°F)
Assumed Moisture (% H2O)
K-Eactor
A- 31
\.Ti-
-!<*«/
.(?0
3 I
.ZH
13
24.
1 -
I.
f
^.
36
l-H
SH&
Mo..
1.5-
a 3-1
2*
^4-7
SC
-
1-3
.2.*
M-B
1-S
fr
Lo
0*134
L-T
1--7
Ml,
2 e
.32-
."7
6D
38
"Tts
i:
It/T?
a. i
So
vio
73
Hz,
«£>.<>
Comments:
-------
if :.-7_ ^
Traverse
Point
Number
Sampling
Time
(min)
Clock
Time
(24hr)
Gas
Meter
Reading
((Vm).tt3)
Velocity
Head
((delta Ps),
in.H2O)
Stack
Ts
cn
Orifice Pressure
Differential
(delta H, in.H2O)
Desired
• Actual
Probe
Temp.
C-F)
Filter
Temp.
Adsorbent
Trap
Temp.
, Dry Gas Meter
Inlet
(Tm in)
Outlet
(Tm out)
Impinger
Exit
Temp.
Pump
Vacuum
(in.Hg)
A 1
_Lk.
Ji-
to
•2.^0
11*6"-
l.C
MS .en
2-St
3-?
«•
as
USSL
2-3 <&
338 '
-a£l
t/
\ -Z-
2 Ho
o
HI
2-2-
51
10
1.3
1-3
5 1
90
ftC
s>
1.3
25-
SC,
1-3 .
.2.5"
tub
23
•51
ret
xoS
5-7
US'
: T.M»
''4
Comments:
-------
EcBtem 0«a*arcn GfOup. ire.
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
L*J |> l~\ \ \ ! I*\ 1 f\ L L ;
Uuf-
Date
Sampling Location
Sample Type
Run Number
Impinger Box Number
Recovery Person
'Recovery" Rinses
Sample Identification
XAD Number
Impinger
Number
Impinger
Solution
Amount of
Sofution
(g)
Impinger Tip
Configuration
Impinger Weight
Final
(g)
Initial
(g)
Weight
Gain
fg)
O.i
\CC
C.ih/
JOG
/S/a-CH
|C&
0
'767.7
Total Weight Gain (g)
(,0
°
-------
Facility: Gulp Alum. Alloy
Date: 12/06/97
Location: Dryer In
Run Number: 3
Sample Type: M26
Total Sampling Time (min) 240.0
Corrected Barometric Pressure (in Hg) 29.51
Absolute Stack Pressure (in Hg) 29.14
Stack Static Pressure (in H20) -5.00
Average Stack Temperature (°F) 235.63
Stack Area (sq in) 240.53
Actual Meter Volume (cu ft) 77.350
Average Meter Pressure (in H2O) 1.11
Average Meter Temperature (°F) 51.47
Moisture Collected (g) 136.80
Carbon Dioxide Concentration (%V) 0.0
Oxygen Concentration (%V) 20.0
Nitrogen Concentration (%V) 80.0
Dry Gas Meter Factor 0.9940
Nozzle Diameter (in) 0.140
Pitot Constant 0.84
Average Sampling Rate (dscfm) 0.326
Standard Metered Volume (dscf) 78.344
Standard Metered Volume (dscm) 2.219
Stack Moisture (%V) 7.61
Mole Fraction Dry Stack Gas 0.924
Dry Molecular Weight 28.80
Wet Molecular Weight 27.98
Stack Gas Velocity (fpm) 4426.55
Stack Gas Velocity (mpm) 1349.21
Volumetric Flow Rate (acfm) 7393.83
Volumetric Flow Rate (acmm) 209.39
Volumetric Flow Rate (dscfm) 5049.75
Volumetric Flow Rate (dscmm) 143.01
Percent Isokinetic 101.01
Percent Excess Air 1760.56
Concentration (g/dscm) 0.00
Concentration (kg/hr) 0.00
Concentration (ppmv) 0.00
Emissions (Ib/hr) 0.00
-------
Eastern Research Group. Inc.
MODIFIED METHOD 5 DATA SHEET
Plant (LuAf /V]
Date
Operator
Sampling Location TVo*/- V
Sample Type
Run Number
Static Pressure (±) (in. H20)
Barometric Pressure (in. H2O)
kj»'Vllnv»Tl
(•3,-^^")
NtAi& •
WyW^L, toVl>
^4^*-
ft
XAD Trap Number
Filter Heater SettingJ°F)
Probe Length & Type
Probe Heater Setting (°F)
Minimum Sample Volume (ft3)
Initial Leak Check
Final Leak Check
Nfl
a£fc
«4' mlnirtei
Traverse
Point
Number
Sampling
. Time
(min)
icr
Clock
Time
(24hr)
Gas
Meter
Reading
((Vm).tt3)
Velocity
, Head
((delta Ps).
in.H2O)
Stack
Ts
CF)
Orifice Pressure
Differential
(delta H, in.H2O)
Desired . Actual
Probe
\ Temp.
Filter
Temp.
Adsorbent
Trap
Temp.
(•F)
Dry Gas Meter
Inlet
(Tm in)
Outlet
(Tm out)
Impinger
Exit
Temp.
Pump
Vacuum
(in.Hg)
31T
So
1 )
a-*,
/.t
vlt>
lltl*
6. 01
T^U
37-7
l(,30
T.tf-7
tuns
^tb.
218
2 s
4
^s\
tf «
,i>-i6
it
/os:
33
-53
.-•41
?•
.3
74-7
(.Z
'ZT^f
-"2-
-2S3
I'LO
Z3G
«f8
31
-fr
1,1*0
•Z-3
'SO
sr
•231
/« I
.20:3
/ 00
±
<^S
6?
-L4-
Comments:
-------
Plant
Date
Location
Sample Type
Run Number
Operator
Page
Traverse
Point
Number
0 L
& 7
»
' • »
"
; • •
• «
4 4
• -
• . .
. *•
•*
Sampling
Time
(min)
•ZOZ-.TT
-2. to
•z.n-5-
zz/r
Z.12..F
2,4rO
*
.
".
-
Clock
Time
(24hr)
i^zr.T
c<733
mo,r
^a
ffifrE
•d&o*
*»
w
•
" *
^
i
*
t
- G3s
• _ Mefer
. Reading
«Vrrt),ft3)
»HtoS2
iHl 4 o
As*i
iH^.Mr
l^-fl-7
iss. r-»1
• C
^ ,•«
J
•f-
*
••^
\
: .
. • '
' ''• ^
.
.
Velocity
Head
((delta Ps),
in.H2O)
\,«4
\\k
••\A
L($l
V6
-.
'
f
r
•
-
-
Stack
Ts
(°F)
a**i/j
taaA
Z^O
^o
^4-0
"". *
..
i •
»""
. *
• •
*.'
•
.
Orifice F
Ditto
(delta H,
Desired
NA>
f
yn
.oe>f^
t
^
• •
-
•
• .
-.
%
'ressure
ential
4n.H2O)
Actual
. **
i *
*
•
Pump
Vacuum
(in.Hg)
°\
X
_^v
^
^
••j
»
• ;
'*
.
Comments:
-------
E
Q
-------
Facility: Gulp Alum. Alloy
Date: 12/05/97
Location: Dryer In
Run Number: 1
Sample Type: M23
Total Sampling Time (min) 240.0
Corrected Barometric Pressure (in Hg) 29.39
Absolute Stack Pressure (in Hg) 29.02
Stack Static Pressure (in H2O) -5.00
Average Stack Temperature (°F) 236.29
Stack Area (sq in) 240.53
Actual Meter Volume (cu ft) 157.093
Average Meter Pressure (in H2O) 1.36
Average Meter Temperature (°F) 58.28
Moisture Collected (g) 216.90
Carbon Dioxide Concentration (%V) 0.5
Oxygen Concentration (%V) 20.0
Nitrogen Concentration (%V) 79.5
Dry Gas Meter Factor 0.9800
Nozzle Diameter (in) 0.192
Pitot Constant 0.84
Average Sampling Rate (dscfm) 0.644
Standard Metered Volume (dscf) 154.653
Standard Metered Volume (dscm) 4.380
Stack Moisture (%V) 6.20
Mole Fraction Dry Stack Gas 0.938
Dry Molecular Weight 28.88
Wet Molecular Weight 28.21
Stack Gas Velocity (fpm) 4765.28
Stack Gas Velocity (mpm) 1452.46
Volumetric Flow Rate (acfm) 7959.61
Volumetric Flow Rate (acmm) 225.42
Volumetric Flow Rate (dscfm) 5490.84
Volumetric Flow Rate (dscmm) 155.50
Percent Isokinetic 97.50
Percent Excess Air 1992.23
Concentration (g/dscm) 0.00
Concentration (kg/hr) 0.00
Concentration (ppmv) 0.00
Emissions (Ib/hr) 0.00
-------
Eastern Rewirch Group. Inc.
MODIFIED METHOD 5 DATA SHEET
Run \n-oi
Page 1 of 2.
Plant
Date nkfll
Operator '
Sampling Location
Sample Type
Run Number
Static Pressure (±) (in. H2O)
Barometric Pressure (in. H2O)
C-AA _
ilJMl'V'l
piO£VOi6
o.cy^)»Yl
Meter Box Number
Meter delta H @
DGM Factor (Y)
Noz2le Type & ID (in.)
Ambient TemperatureJ'F)
Assumed Moisture (% H2O)
K-Factor
44O
I™jO /I
• / Or
JJftO
t\Q2_
>S
_v 1 ,
•4^
K - JVtfc- 1 * V~" ^ ,*. Diagram of Duct
Schematic of Traverse Point Layout
Read and record all data every minutes
Traverse
Point
Number
Sampling
Time
(min)
e
Clock
Time
(24hr)
Gas
Meter
Reading
((Vm).ft3)
Velocity
Head
((delta Ps).
in.H2O)
Stack
Ts
Orifice Pressure
Differental
(delta H. in.H2O)
Desired
Actual
Probe
Temp.
Filter
Temp.
(•F)
Adsorbent
Trap
Temp.
Dry Gas Meter
Inlet
(Tm in)
Outlet
(Tm out)
Impinger
Exit
Temp.
(T)
Pump
Vacuum
(in.Hg)
\,c\
HO
38
ib
\f\
'/Q
3ft
Zl
6-1
\r\
(a
Ml
40
IOL -
-LO-
m
41
Ul
Ml
U
Uo
m
M8
Ll-
4^
\2-
Ml
''
^f
11
-t-.O
7,*
SO
1.1
Ifc
••\\p
\.
*-i_
'f
if
C.
I" JU
<«*
I'll
Kit
^^\
'1
IVJJ
•2,33
LS
S"
M3
Ml-
MM
loU
I.M
_u2>-
Ji2_
M2,
04-
-W4-
Comments:
liAi*-^1 cx^4(g> r^"
-------
Plant
Date
Ill-Cm
Location
Sample Type
Run Number
Operator
Traverse
Point
Number
Sampling
Time
(min)
Clock
Time
(24hr)
Gas
Meter
Reading
((Vm),ft3)
Velocity
Head
((delta Ps),
in.H20)
Stack
Ts
CF)
Orifice Pressure
Differential
(delta H, in.H20)
Desired Actual
Probe
Temp.
Filter
Temp.
Adsorbent
Trap
Temp.
Dry Gas Meter
Inlet Outlet
(Tm in) (Tm out)
Impinger
Exit
Temp.
CF)
Pump
Vacuum
(in.Hg)
< -72
/.
Ml
i
1.4
Q-1
-Hi,-
(Ski,
1.4
i a
V
w
L U
MO
1.1
i.O
-U-
1-0
•tf-
O-Hb
\.o
Wi
tfO
,1*0
4U
Ul
ill.
I.O
to
C.MO-
*O. oo Ci
c-til
Jli
'UO
1.0
'1
J-4-
1.0
2-3?
_b£-
CVU
,c
7X^"
-•As
i»40
040
-y-
0.0<
&
Comments:
-------
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Sampling Location
Sample Type
Run Number
Impinger Box Number
Recovery Person
Recovery Rinses
Sample Identification
Filter Number
XAD Number
f ,i lr\ . hi \ ii IVN, CMirrN H Hi»5\/
rt--*f-
-------
Facility: :Culp Alum. Alloy 1
Date: 1 12/06/97
Location: i Dryer In
Run Number: i 2 !
Sample Type: IM23
Total Sampling Time (min) ; \
Corrected Barometric Pressure (in Hg)
Absolute Stack Pressure (in Hg)
Stack Static Pressure (in H2O) ;
Average Stack Temperature (°F) |
Stack Area (sq in) ! i !
Actual Meter Volume (cu ft) i
Average Meter Pressure (in H20) ;
Average Meter Temperature J°F)
Moisture Collected (g) i
Carbon Dioxide Concentration (%V)
Oxygen Concentration! (%V)
Nitrogen Concentration (%V)
Dry Gas Meter Factor
Nozzle Diameter (in)
Pitot Constant
Average Sampling; Rate (dscfm)
Standard Metered Volume (dscf) '••
Standard Metered Volume (dscm)
Stack Moisture (%V) i '••
Mole Fraction Dry Stack Gas ;
Dry Molecular Weight
Wet Molecular Weight
Stack Gas Velocity (fpm) ;
Stack Gas Velocity (mpm)
Volumetric Flow Rate (acfm)
Volumetric Flow Rate (acmm)
Volumetric Flow Rate (dscfm)
Volumetric Flow Rate (dscmm)
Percent Isokinetic '
Percent Excess Air j
Concentration (g/dscm) :
Concentration (kg/hr) :
Concentration (ppmv)
Emissions (Ib/hr)
|
i
i \
240.0
! 29.51
29.14
i -5.00
i 236.91
240.53
163.784
1.24
49.86
119.50
; 0.5
20.0
79.5
0.9800
0.192
i 0.84
: 0.686
164.544
i 4.660
6.98
0.930
28.88
28.12
; 4932.08
1503.30
8238.23
233.31
5654.20
160.13
100.73
i 1992.23
0.00
0.00
0.00
0.00
-------
Ejjtem Retcarch Group. Inc.
MODIFIED METHOD 5 DATA SHEET
Run //; CfjQ" ° 2-:"
Page 1 of 2^
Plant
Date
Operator
Sampling Location
Sample Type
Run Number
Static Pressure (±) (in. H2O)
Barometric Pressure (in. H2O)
(>w piu ftL-
U.|taJr»
XAD Trap Number
Filter Heater Setting (°F)
Probe Length & Type
Probe Heater Setting (°F)
Minimum Sample Volume (ft3)
Initial Leak Check
Final Leak Check
2<
| 7*H
.1*0
,R2-
i<*
6.2-
>t*~ ,1^^. 1 M PC/Ati
Diagram of Duct
Schematic of Traverse Point Layout
Read and record all data every minutes
Traverse
Point
Number
Sampling
Time
(min)
Clock
Time
(24hr)
Gas
Meter
Reading
((Vm).ft3)
Velocity
Head
((delta Ps),
in.H2O)
Stack
Ts
Orifice Pressure
Differential
(delta H. in.H2O)
Desired Actual
Probe
Temp.
CF)
Filter
Temp.
CF)
Adsorbent
Trap
Temp.
Dry Gas Meter
Inlet
(Tm in)
Outlet
(Tm out)
Impinger
Exit
Temp.
Pump
Vacuum
(in.Hg)
A.o
-%-
7- •'
"L.M/1
Vl
i£
Hi
10
¥.1 .of-7
Wo
wo
it
•L»K
VD
(I
MO
MP,
40
I'M-
l.'T
MO
MO
-U-
L^fj j
(Oil?
HO
Jo
y» 0.
f\o
AC?
a;
MT-
^^•I).o\
MS"
\.V
\.\
M1-
^M^.^^
Ul
s'n
ML*
\sl-i
Mb
\.-z-
I -
v,t
iv
Comments:
-------
Ecjtefn Se»earcn Greco, 'nc.
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Sampling Location
Sample Type
Run' Number '*m?>'^--.:-~
Impinger Box Number
Recovery Person
Recovery Rinses
Sample Identification
Filter Number
XAD Number ;
1 : . 1 p • M 1 ,i MK, fiLVf^PN H U r>\J
/^L/5-/9>
Cb<ca (j
•lOG-360
Total Weight Gain (g)
-------
Facility: Gulp Alum. Alloy
Date: 12/06/97
Location: Dryer In
Run Number: 3
Sample Type: M23
Total Sampling Time (min) 240.0
Corrected Barometric Pressure (in Hg) 29.51
Absolute Stack Pressure (in Hg) 29.14
Stack Static Pressure (in H2O) -5.00
Average Stack Temperature (°F) 236.41
Stack Area (sq in) 240.53
Actual Meter Volume (cu ft) 148.612
Average Meter Pressure (in H2O) 1.14
Average Meter Temperature (°F) 52.30
Moisture Collected (g) 202.90
Carbon Dioxide Concentration (%V) 0.0
Oxygen Concentration (%V) 20.0
Nitrogen Concentration (%V) 80.0
Dry Gas Meter Factor 0.9800
Nozzle Diameter (in) 0.192
Pitot Constant 0.84
Average Sampling Rate (dscfm) 0.619
Standard Metered Volume (dscf) 148.463
Standard Metered Volume (dscm) 4.204
Stack Moisture (%V) 6.05
Mole Fraction Dry Stack Gas 0.939
Dry Molecular Weight 28.80
Wet Molecular Weight 28.15
Stack Gas Velocity (fpm) 4506.95
Stack Gas Velocity (mpm) 1373.72
Volumetric Flow Rate (acfm) 7528.11
Volumetric Flow Rate (acmm) 213.20
Volumetric Flow Rate (dscfm) 5222.01
Volumetric Flow Rate (dscmm) 147.89
Dercent Isokinetic 98.41
3ercent Excess Air 1760.56
Concentration (g/dscm) 0.00
Concentration (kg/hr) 0.00
Concentration (ppmv) 0.00
Emissions (Ib/hr) 0.00
-------
Eiilern Research Group. Inc.
MODIFIED METHOD 5 DATA SHEET
Run
Page-1 of
Plant
Date
Operator
Sampling Location
Sample Type
Run Number
Static Pressure{±) (in. H2O)
Barometric Pressure (in. H2O)
(.uV Ai. AC.
izltri-7
Dtt/y/t,
UUA
»vi5-S
•4
•-"i
XAD Trap Number
Filter Heater Setting (°F)
Probe Length & Type
Probe Heater Setting (°F)
Minimum Sample Volume (ft3)
Initial Leak Check
Final Leak Check
2-Hc?
VYrH^
Z-^S
& do&[4
fl.rAooSfSio1
Meter Box Number
Meter delta H @
DGM Factor (Y)
Nozzle Type & ID (in.)
Ambient Temperature (°F)
Assumed Moisture (% H2O)
K-Factor
A<+rv
I.-154
.'Wo
.ITJ-
4tT
U>. J-
*-.^2-
/-) . 2<3 Diagram of Duct
Schematlc of Traverse Point Layout
Traverse
Point
Number
Sampling
Time
(min)
Clock
Time
(24hr)
Gas
Meter
Reading
((Vm).ft3)
Velocity
Head
((delta Ps).
in.H20)
Read and record all data uvery ±
Stack
Ts
Orifice Pressure
Differential
(delta H, in.H?O)
Desired
Actual
minutes
CGt-° ^/Vll^
Probe
Temp.
Filter
Temp.
Adsorbent
Trap
Temp.
(•F)
Dry Gas Meter
Inlet Outlet
(Tm in)
(Tm out)
Impinger
Exit
Temp.
(•F)
Pump
Vacuum
(in.Hg)
.1
43
37
ft
\5.0
\uoO
,1
IS
-SI.
3SL
ISi
"Sw.iu
bO
Ml
v,o
Vi
AA.
40
bo
•ft
4o
-7
41
ao
l.U
tfi
r».t.
l.U
41
iai
44-
'L-S""
.. 2.1
5.3
so
1 -
MI.
t.M
45
__L3_
H\
1.3
U-O
/tl.ifc.
I'D
IfS
S
'S
I.I
t.o
9)
JL£
,32
L-Slo
Comments:
-------
Pagl
of
Plant
Date
Location
Sample Type
Run Number
Operator
Traverse
Point
Number
A-G.
i*
^ 7
7
flj?
£
Sampling
Time
(min)
^OZ.i>~
2.16-
ill.*"
i^5T~
-z.it.s-
-MjO
Clock
Time
(24hr)
\'\l±'.^~
iflS^
iH^.b"
1^4'X
mc-sT.^"
lisQS
Gas
Meter
Reading
((Vm).n3)
/Vt.Coif
\MU,%
\ S>0.-)
Kg.«\
f^.Sv
/bl.-7JO
Velocity
Head
((delta Ps).
in.H2O)
\ .\
I.I
W
^
2^^
2.3^
tSq
Z3T
Orifice Pressure
Differential
(delta H, in.H2O)
Desired Actual
i.jiA\*-
*.O
/,o
,3?U
•*1
^7
.^L.
/- ^>.^l.t
Probe
Temp.
CF)
•i4/
^-SV
£SS~
23 W
•z-V«^
250
4G,P/t^"
Fitter
Temp.
(°F)
•Z±*
;xuo
•^^n
•i.^i-
1L.O
Adsorbent
Trap
Temp.
(°F)
((V
^i
'-i'4
HV
Wi~"
%
Dry Gas
Inlet
(Tm in)
s •/
^"2-
S'.S^
s"^:
<7j
\> /
^1
> Meter
Outlet
(Tm out)
V.-s-
>V5""
-------
Eastern Qeaaarcn G«sco. '-r\c.
MOISTURE RECOVERY FORM FOR METHOD 4
Plant
Date
Sampling Location
Sample Type
Run Number
Impinger Box Number
Recovery Person
Recovery Rinses
Sample Identification
Filter Number
XAD Number
/":. i> . ftV.^'.r^tVN R lUx,
/^J^/T-
Cft(\ /Wl€l
rv++-v^ ,03
^^
/qo^ fy.i4e. / P ~^.\ ^,.i-Vci5. (rei
ZCC -3
Total Weight Gain (g)
-------
Facility: Gulp Alum. Alloy
Date: 12/05/97
Location: Dryer Out
Run Number: 1
Sample Type: M26
Total Sampling Time (min) 240.0
Corrected Barometric Pressure (in Hg) 29.38
Absolute Stack Pressure (in Hg) 29.30
Stack Static Pressure (in H2O) -1.00
Average Stack Temperature (°F) 186.44
Stack Area (sq in) 490.87
Actual Meter Volume (cu ft) 98.879
Average Meter Pressure (in H2O) 0.56
Average Meter Temperature (°F) 59.04
Moisture Collected (g) 133.90
Carbon Dioxide Concentration (%V) 1.0
Oxygen Concentration (%V) 19.0
Nitrogen Concentration (%V) . 80.0
Dry Gas Meter Factor 0.9880
Nozzle Diameter (in) 0.215
Pitot Constant 0.84
Average Sampling Rate (dscfm) 0.409
Standard Metered Volume (dscf) 98.146
Standard Metered Volume (dscm) 2.779
Stack Moisture (%V) 6.04
Mole Fraction Dry Stack Gas 0.940
Dry Molecular Weight 28.92
Wet Molecular Weight 28.26
Stack Gas Velocity (fpm) 2112.59
Stack Gas Velocity (mpm) 643.92
Volumetric Flow Rate (acfm) 7201.48
Volumetric Flow Rate (acmm) 203.95
Volumetric Flow Rate (dscfm) 5411.99
Volumetric Flow Rate (dscmm) 153.27
Percent Isokinetic 102.17
Percent Excess Air 889.51
Concentration (g/dscm) 0.00
Concentration (kg/hr) 0.00
Concentration (ppmv) 0.00
Emissions (Ib/hr) 0.00
-------
Eastern ftneinh Group. Inc.
MODIFIED METHOD 5 DATA SHEET
CO 1 -
Run
Page 1 of
Plant
Date
Operator
Sampling Location \&\ < K.
Sample Type
Run Number
Static Pressurejt) (in. H2O)
Barometric Pressure (in. H2O)
CwJ> M/ A
'2/ffa*
Alum / 3"S
€H ooT
Pm/H^L
1
-1-0 "
2.9 .-S 3ct
XAD Trap Number
Filter Heater Setting (°F)
Probe Length & Type
Probe Heater Setting (°F)
Minimum Sample Volume (ft3)
Initial Leak Check
Final Leak Check
ZSO
G'iNflt*
150
feo
• OI^IO"
.C)@ IS"'
Meter Box Number
Meter delta H @
DGM Factor (Y)
Nozzle Type & ID (in.)
Ambient Temperature (°F)
Assumed Moisture (% H20)
K-Factor
d-3>
l.m
O,q&£
O.l\$
3o*
8%
|,(,i_
Diagram of Duct
Schematic of Traverse Point Layout
Read and record all data every _^_ minutes
Traverse
Point
Number
Sampling
Time
(min)
Clock
Time
(24hr)
Gas
Meter
Reading
«Vm).ft3)
Velocity
Head
((delta Ps),
' in.H2O)
Stack
Ts
Orifice Pressure
Differential
(delta H, in.H2O)
Desired Actual
Probe
Temp.
(T)
Filter
Temp.
Adsorbent
Trap
Temp.
Dry Gas Meter
Inlet
(Tm in)
Outlet
(Tm out)
Impinger
Exit
Temp.
Pump
Vacuum
(in.Hg)
-r
A-V
1ft. 0
i .3
"LOT
7 H
i
OS :
2 .
M-
0%
loi
\ , >M
H
40
l.jd.
iMO
Sb.Y2.0-?-
V
. O
£
6 O
(,0
3.
33
7.4 I
2-0
10
6, \ ,
\6 "
C ,
Qv(_
O
O. G
Z-s O
O
'
r.\i
O.C'L
1ST-
o.os'
6 i
10
\\
fo > b
n-01/
2-5 2-
Ii±
5H
O
J C ' <
/ o
i : <>" o
•K-O
frl.l.
^
S-o
H
Q
o.i
£,0
JO
SO
11: fco
ZOO
1.04
S'f
ILO
(n 1
0
tsv
fo
AE
:>-.£
iVfi
0
O.tS
T--O
U v -H
*
n.i i
60
O
00
fi. IV
14,1
r/
to
IS
io~v -
q
Z-0
H "
\il-C?
0 MS
H 30
S, 0
o^o
3Z
2 -S
t
Comments:
-------
Plant
Date
Location
Sample Type
Run Number
Operator
Traverse
Point
Number
-
Sampling
Time
(min)
Clock
Time
(24hr)
Gas
Meter
Reading
((Vm).ft3)
Velocity
Head
((delta Ps),
in.H2O)
—
Stack
Ts
CF)
Orifice F
Differ
(delta H.
Desired
'reusure
ential
in.H2O)
Actual
\
Probe
Temp.
(°F)
Filter
Temp.
(°F)
Adsorbent
Trap
Temp.
(°F)
Dry Gas Meter
Inlet Outlet
(Tm in) (Tm out)
Implnger
Exit
Temp.
(°F)
Xj
,
Pump
Vacuum
(in.Hg)
i
Comments:
-------
.G
. inc.
MOISTURE RECOVERY FORM FOR METHO
C
Plant
Date
Sampling Location
Sample Type
Run Number
Impinger Box Number
Recovery Person
Recovery Rinses
Sample Identification
Filter Number
XAD Number
C ^ LjJ (> R \ 1 i Tr\ i (\ i ^~»-\ M 1 1 n V 5
*Y / " 11 fjt ^ ^V ^0-*K*
^\,p Jrv<"-F J/5 ^rT1 LL^ (Jj-^
^44^^^ ^/nA " ~~
/
rOd-r,- r^uJoV**. / 1 ^Ct-^-n V (-Ti^V-k'i.1
7
ill ^?^i( 'v — /
Impinger
Number
Impinger
Solution
Amount of
Sofution
(g)
Impinger Tip
Configuration
Impinger Wefght
Final
(g)
'
Initial
(g)
Weight
Gain
(g)
o.i
-------
Facility: Gulp Alum. Alloy
Date: 12/06/97
Location: Dryer Out
Run Number: 2
Sample Type: M26
Total Sampling Time (min) 240.0
Corrected Barometric Pressure (in Hg) 29.50
Absolute Stack Pressure (in Hg) 29.42
Stack Static Pressure (in H2O) -1.00
Average Stack Temperature (°F) 181.83
Stack Area (sq in) 490.87
Actual Meter Volume (cu ft) 108.753
Average Meter Pressure (in H2O) 0.14
Average Meter Temperature (°F) 57.27
Moisture Collected (g) 80.00
Carbon Dioxide Concentration (%V) 0.5
Oxygen Concentration (%V) 19.5
Nitrogen Concentration (%V) 80.0
Dry Gas Meter Factor 0.9880
Nozzle Diameter (in) 0.215
Pitot Constant 0.84
Average Sampling Rate (dscfm) 0.451
Standard Metered Volume (dscf) 108.124
Standard Metered Volume (dscm) 3.062
Stack Moisture (%V) . 3.37
Mole Fraction Dry Stack Gas 0.966
Dry Molecular Weight 28.86
Wet Molecular Weight 28.49
Stack Gas Velocity (fpm) 2270.87
Stack Gas Velocity (mpm) 692.16
Volumetric Flow Rate (acfm) 7741.05
Volumetric Flow Rate (acmm) 219.23
Volumetric Flow Rate (dscfm) ' 6050.61
Volumetric Flow Rate (dscmm) 171.35
Percent Isokinetic 100.67
Percent Excess Air 1191.93
Concentration (g/dscm) 0.00
Concentration (kg/hr) 0.00
Concentration (ppmv) 0.00
Emissions (Ib/hr) 0.00
-------
..Inc.
MODIFIED METHOD 5 DATASHEET
Run
Page 1 of
Plant
Date
Operator
Sampling Location ""bft-f'et^-
Sample Type
Run Number
Static Pressure (±) (in. H2O)
Barometric Pressure (in. H2O)
|lv /\i_
<\^.
SS
fyv<^K)*AOUT
HCL,L.TKVN
•^_
-l-oo"
^liSl
XAD Trap Number
Filter Heater Setting (°F)
Probe Length & Type
Probe Heater Setting (°F)
Minimum Sample Volume (ft3)
Initial Leak Check
Final Leak Check
2.SG
rVN^t*
2^0
6iO
• Oi/OiV
,0|£jO''
Meter Box Number
Meter delta H @
DGM Factor (Y)
Nozzle Type & ID (in.)
Ambient Temperature (°F)
Assumed Moisture (% H2O)
K-Factor
ft-l^-
l.£]3
o 1^8
0 !XlS
30°
%**
1 iCjT-
i T ^ ^
~IQ i t
1 F^
Diagram of Duct
Schematic of Traverse Point Layout
Read and record all data every I P minutes
Traverse
Point
Number
Sampling
Time
(min)
0
Clock
Time
(24hr
(7 S3
£
Gas
Meter
Reading
((Vm).tt3
Velocity
Head
((delta Ps),
in.H20)
Stack
Ts
Orifice Pressure
Differential
(delta H, in.H2O)
Desired
Probe
Temp.
Actual
Filter
Temp.
CF)
Adsorbent
Trap
Temp.
Dry Gas Meter
Inlet
(Tm in)
Outlet
(Tm out)
Impinger
Exit
Temp.
Pump
Vacuum
(in.Hg)
B-
/o
7_
2V
20
2«3
±t
HZ-
0,5-3
V3
2.3V
O
JO
on
ft
S
40
0 ,
O-SE
,, S
SO
O, Xf.
/ o
0.2.G
o.xt,
r-o
'9-
.V
o,
/o '
ILO
1.7,$
/.2.S
/oo
/o:
/.ffc
-TV/
"3 o
HO
/o:
25C,
yt,
4^
IIP
0. O/
/0i-
u:io
1*0
i I -O
I.ZO
I9
^
V 0
it
ISO
70 1
V-0
(0
ICO
n to
T.C.V/.O
l.oA
3 .0
II'OG
ft.-f-S
o
iv./o
70
ISO
1-C.CJ
r
42 ' J>0
1C
-5
/ 0
0
0,07.
Uo
.<3.o V
vc,
i a
l o
O.o1/
60
/. o
i <;
Lo
/. o
(0
Comments:
-------
Plant
Date
Location
Sample Type
Run Number
Operator
Traverse
Point
Number
Sampling
Time
(min)
Clock
Time
(24hr)
Gas
Meter
Reading
((Vm),fl3)
Velocity
Head
((delta Ps),
in.H2O)
Stack
Ts
CF)
Orifice F
Differ
(delta H,
Desired
ressure
entia!
in.H2O)
Actual
Probe
Temp.
CF)
Filter
Temp.
CF)
Adsorbent
Trap
Temp.
CF)
Dry Gas
Inlet
(Tm in)
3 Meter
Outlet
(Tm out)
Impinger
Exit
Temp.
CF)
Pump
Vacuum
(in.Hg)
Comments:
-------
ire.
MOISTURE RECOVERY FORM FOR METHOD*
Plant
Date
Sampling Location
Sampfe Type
Run Number
Impinger Box Number
Recovery Person
Recovery Rinses
Sample Identification
Filter Number
XADNumber
duJ^ RL^'.CS,^ ftiUy*
r^M^\ 3j A
A
^"^
rO^r,- A.JnU / T c.^cv C, vk'.n
'
II 1 ft^l "3.
Impinger
Number
Impinger
Solution
Amount of
Sofution
(g)
Impinger Tip
Configuration
Impinger Weight
Final
(g)
Initial
(g)
Weight
Gain
(9)
o.i
\Cfi
ICC
-------
Facility: Gulp Alum. Alloy
Date: 12/06/97
Location: dryer out
Run Number: 3
Sample Type: M26
Total Sampling Time (min) 240.0
Corrected Barometric Pressure (in Hg) 29.35
Absolute Stack Pressure (in Hg) 29.28
Stack Static Pressure (in H20) -1.00
Average Stack Temperature (°F) 187.92
Stack Area (sq in) 490.87
Actual Meter Volume (cu ft) 102.267
Average Meter Pressure (in H2O) 0.58
Average Meter Temperature (°F) 51.52
Moisture Collected (g) 151.40
Carbon Dioxide Concentration (%V) 0.5
Oxygen Concentration (%V) 20.0
Nitrogen Concentration (%V) 79.5
Dry Gas Meter Factor 0.9880
Nozzle Diameter (in) 0.215
Pitot Constant 0.84
Average Sampling Rate (dscfm) 0.427
Standard Metered Volume (dscf) 102.390
Standard Metered Volume (dscm) 2.900
Stack Moisture (%V) 6.52
Mole Fraction Dry Stack Gas 0.935
Dry Molecular Weight 28.88
Wet Molecular Weight 28.17
Stack Gas Velocity (fpm) 2212.16
Stack Gas Velocity (mpm) 674.27
Volumetric Flow Rate (acfm) 7540.91
Volumetric Flow Rate (acmm) 213.56
Volumetric Flow Rate (dscfm) 5620.93
Volumetric Flow Rate (dscmm) 159.18
Percent Isokinetic 102.62
Percent Excess Air 1992.23
Concentration (g/dscm) 0.00
Concentration (kg/hr) 0.00
Concentration (ppmv) 0.00
Emissions (Ib/hr) 0.00
-------
Extern Research Group, Inc.
MODIFIED METHOD 5 DATA SHEET
Run
Page 1 of
Plant
Date
Operator ,
Sampling Location ^bV-it £-
Sample Type
Run Number
Static Pressure (±) (in. H2O)
Barometric Pressure (in. H2O)
C<,ur* fo.flL
Mt.ll*
m«)>(/^rS
*AH oJT
rvta_/?n
3 '
- |,oo"
ZS.3G
XAD Trap Number
Filter Heater Setting (°F)
Probe Length & Type
Probe Heater Setting (°F)
Minimum Sample Volume (ft3)
Initial Leak Check ,
Final Leak Check
*-
•2,^0°
6'N/acy
2^0°
CoO
0,0l@/o"
O.Oltfio'1
Meter Box Number
Meter delta H @
DGM Factor (Y) l
Nozzle Type & ID (in.)
Ambient Temperature (°F)
Assumed Moisture (% H2O)
K-Factor
d-3v
l.frl^
o.«ttS
oa\S
3£»
**%
1 ,k2-
Diagram of Duct
Schematic of Traverse Point Layout
Read and record all data every _j_j_ minutes
Traverse
Point
Number
Sampling
Time
(minf
Clock
Time
Gas
Meter
Reading
Velocity
Head
((delta Ps),
in.H2O)
Stack
Ts
CF)
Orifice Pressure
Differential
(delta H. iri.H2Oj
Desired Actual
Probe
Temp.
Filter
Temp.
CF)
Adsorbent
Trap
Temp.
Dry Gas Meter
Inlet
(Tm in)
Outlet
(Tm out)
Impinger
Exit
Temp.
Pump
Vacuum
(in-Hg)
ft-12-
SL
43
S.O
10
2.HI.-V
zss
IL' K
fl .<
.0
o
It. '
.>
V?
4-0
S.o
2.0
30
0.
J^o.
80
.0 b
0. fG
-ia.
10
*
•2.0 -
OH
0, Ot>
1.0
IV:
.O
1
D
. 1
OCi
1 0
iio
6-OO
O.ec
1-0
10"
VTO
132 .8*0
no
1 0
iHo
ISO
. 33
> 2-
(Go
.SS
MS
>o
5*4
^•s
,3?
-*ia.
loo
Zoo
5-ci
XI 0
(•of
.Z.C
feO
-40
c 1
6/0
ISO
2S2.
263
• 0
o|
ID"
Comments:
-------
Plant
Date
Location
Sample Type
Run Number
Operator
Traverse
Point
Number
Sampling
Time
(min)
Clock
Time
(24hr)
Gas
Meter
Reading
((Vm).ft3)
Velocity
Head
((delta Ps),
in.H2O)
Stack
Ts
(°F)
Orifice Pressure
Differential
(delta H, in.H2O)
Desired Actual
Probe
Temp.
(°F)
Filter
Temp.
m
Adsorbent
Trap
Temp.
(°F)
Dry Gas Meter
Inlet Outlet
(Tm in) (Tm out)
Impinger
Exit
Temp.
(°F)
Pump
Vacuum
(in.Hg)
Comments:
-------
Eawem Ow*orcn G/oco.
MOISTURE RECOVERY FORM FOR METHOD
Plant
Date
Sampling Location
Sample Type
Run Number
Impinger Box Number
Recovery' Person
Recovery Rinses
Sample identification
Fitter Number
XAD Number
r* .1 Q i . • r\ i i
C^'.D \V^