EPA-450/4-84-0141
NATIONAL DIOXIN STUDY
TIER 4 — COMBUSTION SOURCES
Final Test Report — Site 3
Sewage Sludge Incinerator SSI — B
By
Michael A. Palazzolo
D. Blake Bath
Martha H. Keating
Radian Corporation
Research Triangle Park, North Carolina 27709
Contract Number: 68-03-3148
Donald Oberacker, Project Officer
Hazardous Waste Engineering Research Laboratory
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268
U.S. Environmental Protection Agency
Office Of Air And Radiation
Office Of Air Quality Planning And Standards
Rese^-ch Triangle Park, North Carolina 27711
And
Office Of Research And Development
Washington DC 20460
April 1987
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This report has been reviewed by the Office Of Air Quality Planning And Standards, U.S.
Environmental Protection Agency, and approved for publication as received from the
contractor. Approval does not signify that the contents necessarily reffect the views and
policies of the Agency, neither does mention of trade names or commercial products
constitute endorsement or recommendation for use.
EPA-450/4-84-0141
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FOREWORD
This report is the result of a cooperative effort
between the Office of Research and Development's Hazardous
Waste Engineering Research Laboratory (HWERL) and the
Office of Air Quality Planning and Standard's Monitoring
and Data Analysis Division (MDAD). The overall management
of Tier 4 of the National Dioxin Study was the responsi-
bility of MDAD. In addition, MDAD provided technical
guidance for the source test covered by this report.
HWERL was directly responsible for the management and
technical direction of the source test.
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TABLE OF CONTENTS
Section Page
1.0 INTRODUCTION . . , 1-1
i
2.0 SUMMARY OF RESULTS 2-1
2.1 Source Sampling and Analysis Overview 2-1
'2.2 Summary of Results. ' 2-4
3.0 PROCESS DESCRIPTIONS 3-1
3.1 Treatment Plant - . 3-1
3.2 Incinerator Description 3-1
3.3 Heat Recovery and Air Pollution Control
for Incinerator SSI-B 3.5
3.3.1 Quad Cyclone !!.'!! 3-6
3.3.2 Waste Heat Recovery Boiler 3-6
3.3.3 Wet Scrubber System 3-6
3.4 Process Data Monitored ] 3-8
4.0 TEST DESCRIPTION 4.1
4.1 Field Sampling '.'.'.'.'. 4-1
4.2 Process Data Collection . '.'.'.'.'.'. 4-4
4.3 Laboratory Analyses ] 4.4
4.3.1 Dioxin/furan analyses . 4.5
4.3.2 Dioxin/furan precursor analyses. ! 4-5
5.0 TEST RESULTS 5,! '
5.1 Process Data 5-1
5.1.1 Incinerator Operating Data '.'.'. 5-1
5.1.2 Emission-Control Equipment Data. ......... 5-3
5.2 Continuous Monitoring 5.3
5.3 Flue Gas Parameter Data '.'.'.'.'.'.'. 5-11
5.4 Dioxin/Furan Emissions Data ...... 5-18
5.5 Dioxin/Furan Precursor Data ...!!!!!! 5-18
5.6 Bottom Ash and Scrubber Slowdown Dioxin/Furan Data. . . . 5-25
5.7 Solids Dioxin/Furan Data. 5-25
6.0 SAMPLING LOCATIONS AND PROCEDURES 6-1
6.1 Gaseous Samples '.'.'.'. 6-1
6.1.1 Gaseous Sampling Locations . ] ', e-l
6.1.2 Gaseous Sampling Procedures 6-5
6.2 Liquid/Slurry Samples ...... 6-10
6.3 Solids Sampling . . . . 6-13
7.0 ANALYTICAL PROCEDURES 7_!
7.1 Dioxins/Furans • '.'.'..'.'.'.'. 7-1
7.2 Dioxins/Furans Precursors ........ ....
7.2.1 GC/MS Analyses !!!!!!! 7-2
7.2.1.1 Sample Preparation. 7-3
7.2.1.2 Analysis. • 7.5
7.3 Total Chlorine Analysis . . ' 7-8
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TABLE OF CONTENTS
(cont'd.)
Page
Section
8.0 QUALITY ASSURANCE/QUALITY CONTROL (QA/QC) ........... : 8-1
8.1 Manual Gas Sampling ................ ' . . . 8-1
8.2 Continuous Monitoring/Molecular Weight Determination. . . • 8-5
8.3 Systems and Performance Audits .............. 8-5
8.3.1 Systems- Audit ..... .............. 8-5
8.3.2 Performance Audit ................. 8-7
8.4 Laboratory Analyses .................... 8-12
8.4.1 Dioxin/Furan QC Data ............... 8-12
8.4.2 Precursor QC Data ................ ; 8-16
8.4.3 Total Chlorine QC Data .............. 8-18
9.0 REFERENCES .......................... i g_i
APPENDIX A FIELD RESULTS ;
A.I Modified Method 5 and EPA Methods 1 - 4 Field Results. . .• A-l
A. 2 Continuous Emission Monitoring Results ...... A-9
A. 3 EPA Method 3 Fixed Gas Field Results ........... A-17
A. 4 Modified Method 5 and EPA Methods 1-4 Sample
Calculations ................. ..... A-21
APPENDIX B PROCESS DATA SUMMARY ................... ', B-l
APPENDIX C SAMPLE SHIPMENT LETTER .................. ; c-1
APPENDIX D DIOXIN/FURAN ANALYTICAL DATA FOR GASEOUS SAMPLES ..... D-l
APPENDIX E RUN-SPECIFIC DIOXIN/FURAN EMISSIONS DATA
E.I Run-Specific Dioxin/Furan Emissions Data :
(As-Measured Concentrations) . . .. ............ E-l
E.2 Run-Specific Dioxin/Furan Emissions Data
(Corrected to 3% Oxygen) ................ E-7
APPENDIX F Run-Specific Risk Modeling Input Data ........... F-l
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LIST OF FIGURES
Figure
2-1
2-2
3-1
3-2
4-1
5-1
5-2
5-3
.5-4
5-5
5-6
5-7
5-8
5-9
6-1
6-2
6-3
6-4
6-5
6-6
Simplified Flow Diagram of the Sewage Sludge Incinerator/
Wet Scrubber System at Site SSI-B
Data Summary for Site SSI-B. .....
Wastewater Treatment and Sludge Processing Flow Diagram
for Site SSI-B
Schematic Diagram of Incinerator SSI-B and Associated Air
Pollution Control Equipment
Sample Point Diagram for Site SSI-B
Incinerator SSI-B Hearth Temperatures During Run 1 . -. .
Incinerator SSI-B Hearth Temperatures During Run 3 . .
Incinerator SSI-B Hearth Temperatures During Run -5 . . . .
Oxygen Concentration Vs. Time for Incinerator SSI-B
Carbon Monoxide Concentration Vs. Time for Incinerator SSI-B
Carbon Dioxide Concentration Vs. Time for Incinerator SSI-B. .
Nitrogen Oxide Concentration Vs. Time for Incinerator SSI-B. .
Total Hydrocarbon Concentrations Vs. Time for
Incinerator SSI-B
Distribution of Dioxin and Furan Homologues in Scrubber
Outlet Emissions
Sample Point Diagram for Site SSI-B
Diagram of Outlet Stack Sampling Locations
Modified Method 5 Train
Adsorbent Sampling System
Schematic of Tap Sampling
Apparatus for Pressure Filtration of Scrubber Slowdown Slurry
Page
2-2
2-5
3-2
3-4
4-3
5-5
5-6
5-7
5-12
5-13
5-14
5-15
5-16
5-22
6-3
6-4
6-7
6-8'
6-11
6-12
VI 1
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Figure
7-1
8-1
LIST OF FIGURES
(cont'd)
'Sample Preparation Flow Diagram for Site SSI-B Feed Samples.
Modified Method 5 Systems Audit Checklist
Page
: 7-4
8-8
viii
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LIST OF TABLES
Page
2-1 Source Sampling and Analysis Overview .............. 2-3
2-2 Summary of Mean Dioxin and Furan Emissions Data for Site SSI-B. . 2-6
3-1 Incinerator and Sludge Design Parameters for Incinerator SSI-B. . 3-5
3-2 Design Data for Incinerator SSI-B Air Pollution Control System. . 3-7
4-1 Source Sampling and Analysis Matrix - Plant SSI-B . ....... 4-2
5-1 Mean Incinerator Operating Parameters During Tests at Site SSI-B. 5-2
5-2 Mean Hearth Temperatures During Dioxin Emissions Testing
at Site SSI-B . . . . ................ ..... 5.4
5-3 Control Equipment Operating Parameters During Dioxin Tests
at Site SSI-B . ............. . .......... 5.8
5-4 Summary of Continuous Monitoring Results for Site SSI-B ..... 5-9
5-5 Summary of Continuous Monitoring Results for Incinerator SSI-B
at 3 Percent Oxygen ........... , .......... 5_10
5-6 Flue Gas Parameters for Incinerator SSI-B (Scrubber Outlet) . . . 5-17
5-7 Summary of Dioxin and Furan Emissions Concentrations and
Emission Rate Data for Site SSI-B (Stack Location) ....... 5-19
5-8 Summary of Dioxin/Furan Emissions Data for Site SSI-B
(At Actual Stack Oxygen Concentration) ............. 5-20
5-9 Summary of Dioxin/Furan Emissions Data for Site SSI-B
(Concentrations Corrected to 3 Percent Oxygen) ......... 5-21
5-10 Dioxin/Furan Emission Factors for Site SSI-B ........... 5-23
5-11 Summary of Precursor Analyses on Sludge Feed Samples. ...... 5-24
5-12 Summary of Total Chloride Data in Sludge Feed Samples ...... 5-26
5-13 Dioxin/Furan Concentrations in the Sludge Feed at Site SSI-B. . . 5-27
5-14 Dioxin/Furan Concentrations in the Bottom Ash at Site SSI-B . . . 5-28
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LIST OF TABLES
(cont'd.)
Table
5-15
5-16
6-1
7-1
7-2
8-1
8-2
8-3.
8-4
8-5
8-6
8-7
8-8
Page
Dioxin/Furan Concentrations in the Scrubber Filtrate
at Site SSI-B • 5-29
Dioxin/Furan Concentrations in the Filterable Scrubber Solids
at Site SSI-B 5-30
Source Sampling and Analysis Matrix - Site SSI-B 6-2
Instrument Consitions for GC/MS Precursor Analyses i 7-6
Components of the Calibration Solution : 7-7
Glassware Precleaning Procedure 8-2
Results of Isokinetic Calculations and Moisture Determinations. .: 8-4
Summary of Drift Check and Control Standard Results ,8-6
Continuous Emission Monitoring System (CEM) Audit Results .... 8-11
Mettler 360 (S/N C99712) Balance Audit Results 8-13
Summary, of Surrogate Recoveries for Dioxin/Furan Analyses
on Site SSI-B Samples 8-14
Summary of Results for Diox-in/Furan Blank Samples and
Fortified QC Samples 8-15
Summary of Surrogate Recoveries for Dioxin Precursor Analyses . . 8-17
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1.0 INTRODUCTION
*
" This report summarizes the results of a dioxin/furan emissions test of
a sewage sludge incinerator equipped with a wet scrubber system for
particulate matter emissions control. The test was the third in a series of
thirteen dioxin/furan emissions tests conducted under Tier 4 of the National
Dioxin Study. The primary objective of Tier 4 is to determine if various
combustion sources are sources of dioxin and/or furan emissions. If any of
the combustion sources are found to emit dioxin or furan, the secondary
objective of Tier 4 is to quantify these emissions.
Sewage sludge incinerators are one of eight combustion source categories
tested in the Tier 4 program. The tested sewage sludge incinerator, hereafter
referred to as incinerator SSI-B, was selected for this test after an initial
information screening and a one-day pretest survey visit.
This test report is organized as follows: A summary of test results
and conclusions is provided in Section 2.0, followed by a detailed process
description.in Section 3.0. The source sampling and analysis plan is
outlined in Section 4.0, and the dioxin test data are presented in
Section 5.0. Sections 6.0 through 9.0 present various testing details.
These include descriptions of the sampling locations and procedures
(Section 6.0), descriptions of the analytical procedures (Section 7.0), and
a summary of the quality assurance/quality control results (Section 8.0).
The appendices contain data generated during the field sampling and
analytical activities.
The term "dioxin/furan" and the acronyms PCDD and PCDF as used in this report
refer to the polychlorinated dibenzo-p-dioxin and dibenzofuran isomers with
four or more chlorine atoms.
1-1
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2.0 SUMMARY AND CONCLUSIONS
2.1 SOURCE SAMPLING AND ANALYSIS OVERVIEW
The host plant (Site SSI-B) is a large municipal wastewater treatment
plant that operates several multiple hearth sewage sludge incinerators. The
incinerator tested is one of two identical units built in 1983. A
simplified diagram of the multiple hearth incinerator/wet scrubber system
tested is shown in Figure 2-1.
Sampling for dioxin emissions was performed at the scrubber exhaust
stack during each of three test runs conducted between November 15 and 19,
1984. All of the field sampling was performed by Radian Corporation. The
gaseous, liquid, slurry, and solids sampling that was performed is summarized
in Table 2-1. Dioxin sampling at the scrubber exhaust stack was based on the
Modified Method 5 (MM5) sampling protocol developed by the American Society of
Mechanical Engineers (ASME) for measuring emissions of chlorinated organic
compounds. The MM5 train components and train rinses were analyzed by
EMSL-RTP.and ECL-Bay St. Louis, two of three EPA laboratories collectively
*
known as Troika. The dioxin/furan analyses quantified 2378-TCDD and the
tetra- through octa-dioxin/furan homologues present in the samples.
Sludge feed samples were obtained directly from the incinerator feed
conveyor during the test. Analyses for dioxin/furan precursors were performed
by Radian on the sludge feed samples. The specific dioxin/furan precursors
analyzed for included chlorophenols, chlorobenzenes, polychlorinated biphenyls
(PCB), and total chlorine.
Continuous emissions monitoring (CEM) for CO, C02, total hydrocarbons
(THC), NO , and 07 was performed at the incinerator outlet. Bottom ash
A £
samples were taken during each test run for dioxin/furan analysis. Scrubber
system blowdown slurry samples were also taken, and the samples were filtered
to separate the solids from the aqueous filtrate. The filtrate was analyzed
The terms TCDD and TCDF as used in this report refer to tetrachlorodibenzo-
p-dioxin and tetrachlorodibenzofuran respectively. The acronyms PCDD and
PCDF as used in this report refer to dioxin and furan homologues with four or
more chlorine atoms.
2-1
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TABLE 2-1. SOURCE SAMPLING AND ANALYSIS OVERVIEW
Item
Item Description.
1. Number of test runs
2. Gaseous sampling
3. Liquid and slurry sampling
4. Solids sampling
- Three identical test runs (Runs l,3,5)a
- MM5 sampling at scrubber outlet (Runs 1,
3,5). Dioxin/furan analysis.
- Continuous CO, C02, 0?, NO , and THC
monitoring at incinerator Qutlet (Runs
1,3,5).
- EPA Reference Methods 2,3, and 4 at
scrubber outlet (Runs 1,3,5)
- Scrubber system blowdown sampling/filtra-
tion (Runs 1,3,5). Dioxin/furan analysis
- Sludge feed sampling (Runs 1,3,5)
Dioxin/furan precursor analysis.
- 'Incinerator bottom ash sampling (Runs
1,3,5). Dioxin/furan analysis.
- Soil sampling (one composite sample from
10 locations). Potential dioxin/furan
analysis.
aTest run 2 was invalidated due to sampling malfunctions; test run 4 was aborted
due to unrepresentative process operation.
2-3
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for dioxin/furan content. Soil samples were also collected for potential
dioxin/furan analysis.
2.2 SUMMARY OF RESULTS
Figure 2-2 summarizes test results for Site SSI-B. According to plant
personnel, the incinerator and wet scrubber system operated under conditions
representative of normal operation during the sampling periods. The average
sludge feed rate (wet basis) was 6.3 Mg/hr (6.9 TPH), and the average solids
content of the sludge was 36.2 wt%. The maximum hearth temperature in the
furnace was approximately 870°C (1600°F). The average total pressure drop of
the wet scrubber system was 34.8 inches of H20. The average exhaust gas T
temperature from the scrubber system was 22°C (71°F). As shown,in Table 2-2,
the 2378-TCDD isomer was not detected in stack gas emissions from the j
scrubber. Average as-measured stack gas concentrations of total PCDD and
total PCDF at the scrubber exhaust outlet were 0.33 ng/dscm and 5.59 ng/dscm,
respectively. The average hourly emissions rates at the scrubber exhaust
outlet were 11.6 ug/hr for total PCDD and 194 ug/hr for total PCDF. The
tetra-chlorinated and octa-chlorinated dioxin homologues were the largest!
contributors to the total PCDD emissions and the tetra-chlorinated furan
homologue were the largest .single contributor to the total PCDF emissions.
At the scrubber exhaust stack, the measured flue gas flow rate was 582
dscmm (20,600 dscfm) at a temperature of 77°C (170°F). Average flue gas
concentrations measured at the incinerator outlet by the Radian continuous
emissions monitoring system were: 02, 13.1 volume percent; CO, 4676 ppmv
@ 3 percent 02; C02, 18.9 volume percent @ 3 percent 02 (dry); NOX, 523 ppmv
@ 3 percent 02 (dry); and THC, 28 ppmv @ 3 percent 02 (wet).
Samples of bottom ash from the multiple hearth incinerator did not
contain detectable levels of the 2378-TCDD isomer. The bottom ash samples
contained 0.01 ppb and 0.042 ppb of total PCDD and total PCDF, respectively.
Precursor analysis of the sludge feed detected 0.03 ppm of
1 !
chlorobenzenes, but PCB's and chlorophenols v/ere not detected. Total chloride
analysis of the sludge feed detected 21.4 ppm total chlorides. The composite
soil sample for Site SSI-B has not yet been analyzed for dioxin/furan content;
2-4
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2-5
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TABLE 2-2. SUMMARY OF MEAN DIOXIN AND FURAN EMISSIONS DATA FOR SITE SSI-B
Parameter
2378 TCDD Total PCDD Total PCDF
Emissions Concentration
(ng/dscm)
As-measured
Corrected to 3% 02
Emissions Rate (ug/hr)
ND
ND
ND
0.33
1.60
11.6
5.59
27.9
194
2-6
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3.0 PROCESS DESCRIPTION
The wastewater treatment plant and sewage sludge incinerator tested at
Site SSI-B are described in this section. The description includes a
discussion of the heat recovery and air pollution control systems associated
with the incinerator.
3.1 TREATMENT PLANT
Site SSI-B is a large municipal wastewater treatment plant that operates
several multiple hearth sewage sludge incinerators. Plant influent consists
of approximately 25 percent industrial waste and 75 percent domestic sewage.
Based on plant data, there are no known large sources of potential dioxin
precursors (e.g., chlorophenols, chlorobenzene, PCB, etc.) in the plant
influent.
A wastewater treatment and sludge processing flow diagram for the
facility-is shown in Figure 3-1. Treatment of the wastewater includes
screening, grit removal, primary sedimentation, aeration for biological
treatment (activated sludge), secondary sedimentation, and chlorination. The
treatment plant effluent is discharged into a river. Since this study,
dechlorination facilities have been added to the plant.
Primary and secondary sludges are processed according to the' diagram in
Figure 3-1. Most of the primary sludge is gravity thickened and conditioned
with polymer. All of the secondary sludge and the remainder of the .primary
sludge are combined in a 3:1 ratio prior to thermal conditioning. Thermal
conditioning oxidizes and breaks down the solids-water bond in the sludge
which allows for improved dewatering.- The polymer-conditioned primary sludge
and the thermally conditioned primary/secondary sludge blend are sent to a
holding tank and then dewatered on roll presses. Use of roll presses at
Site SSI-B results in a drier sludge feed cake than that obtained at most
facilities using either filter presses or vacuum filters. The blended,
dewatered sludge is burned in the multiple hearth incinerators.
3.2 INCINERATOR DESCRIPTION
The incinerator tested at Site SSI-B is one of two identical Envirotech
nine-hearth sewage sludge incinerators that were installed at the plant in
3-1
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1983. A schematic diagram of the incinerator tested and its heat recovery and
air pollution control systems is shown in Figure 3-2. Table 3-1 lists some of
the more important design parameters of the incinerator;
Conditioned primary and secondary sludge with a solids content of 30 to
40 percent by weight is fed to the second hearth of the incinerator (hearth
one) at a rate of about 2.3 to 2.7 dry Mg (2.5 to 3.0 dry tons) per hour. The
design capacity of the incinerator is 3.39' dry Mg (3.75 dry tons) per hour.
The sludge typically has a volatiles content of 65 percent by weight (dry
solids basis) and a heating value of 24.4 J/g (10,500 Btu/lb) of volatiles.
The upper hearths are used for drying of the sludge cake, the middle hearths
are used for burning, and the bottom hearths are used for ash cooling.
An auxiliary fuel system consisting of natural gas-fired burners is
available to provide supplemental heat when necessary. However, efforts by
plant personnel to minimize energy usage usually results in these burners
being used only during incinerator startup. Incinerator SSI-B also has the
.capability of firing scum from the wastewater treatment process, but scum
was not fired during the test program. Ordinarily, all the scum produced by
the plant is fired in a dedicated scum incinerator. The scum incinerator is
never used to burn sludge and was not part of the test program. Combustion
air for Incinerator SSI-B consists of ambient air and odorous air collected
from ventilation systems on various wastewater treatment plant processes,
including thermal conditioning. A shaft cooling air system is used to prevent
overheating of the rabble arm shaft. The shaft cooling air exhaust is vented
directly to the atmosphere via a stack separate from that used for the
incinerator air pollution control system. None of the shaft cooling air
exhaust is recycled for use as combustion air.
Incinerator SSI-B is typically operated to maintain a temperature of
870°C (1,600°F) on Hearth No. 3 (fourth hearth from the top). The temperature
•
is controlled by a microprocessor-based system that varies the combustion air
intake dampers. The percent oxygen in the incinerator exhaust gas is
typically 12 to 15 percent.
Under normal feed rate .conditions, Incinerator SSI-B produces about 22 Mg
(20 tons) per day of bottom ash, which is pneumatically conveyed to silos for
storage. The ash is ultimately loaded onto trucks or rail cars and hauled
away for land disposal.
3-3 . '
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TABLE 3-1. INCINERATOR AND SLUDGE DESIGN PARAMETERS
FOR INCINERATOR SSI-B
Design Parameter
Value
Incinerator
1. Manufacturer
2. Number of Hearths
3. Sludge burning capacity
4. Exhaust gas volume
5. Bottom ash production
6. Auxiliary fuel
Sludge Feed
1. Sludge type
2. Solids content
• Envirotech
• 9
t 3.75 tons/hr (dry)
• 82,000 acfm @ 1,200°F
• 28 tons/day (typical)
• 34 tons/day (maximum)
• Natural gas (startup only)
t Conditioned and dewatered
primary and secondary sludge
• 30% to 40%
3-5
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3.3 HEAT RECOVERY AND AIR POLLUTION CONTROL SYSTEMS FOR INCINERATOR SSI-B:
The exhaust gas train for Incinerator SSI-B consists of a quad cyclone, a
waste heat recovery boiler, a wet scrubber system, an induced draft fan, and
an exhaust stack. Table 3-2 gives design parameters for some of these
devices; The heat recovery and air pollution control system components are
described below.
3.3.1 Quad Cyclone
The quad cyclone is used for large particulate removal prior to the waste
heat boiler system. The cyclone has a rated gas flow capacity of 38.7 m /s @
650°C (82,000 acfm @ 1,200°F) and typically operates at a pressure drop of 1.2
kPa (5 inches of water). The rated particulate matter removal efficiency of
the cyclone is 72 percent. Uncontrolled particulate matter emissions entering
the cyclone are estimated to be approximately 617 Mg (680 tons) per year.
3.3.2 Waste Heat Recovery Boiler
The waste heat boiler recovers heat from the incinerator offgas to
produce steam. The nominal steam capacity of the boiler is 8200 kg/hr @ 2.8
MPa (17,000 Ib/hr steam @ 400 psig). The steam is used in the thermal
conditioning .process and for other auxiliary equipment such as steam
turbines. Waste heat boiler offgas is sent to the wet scrubber system at a
temperature of about 230°C (490°F).
3.3.3 Wet Scrubber System
The wet scrubber system consists of a precooler, a venturi scrubber, iand
a packed tower subcooler with demister (Figure 3-3). Subcooler exhaust is
reheated and discharged to a stack. In the precooler, blowdown water from the
subcooler is sprayed into'the gas stream to provide cooling from about 254° to
80°C (490°F to 180°F). The design precooler water flow rate is 136 m3/hr (600
gpm). Precooler exhaust gas enters the venturi scrubber, which is operated at
a pressure drop of about 5.0 to 7.5 kPa (20 to 30 inches of water). Blowdown
water from the subcooler is injected at the venturi scrubber throat at a
design rate of 114 m /hr (500 gpm). Design gas flow through the venturi '
scrubber is about 16.5 m /s @ 80°C (35,000 acfm @ 180°F), and the waterrgas
3 3
ratio is on the order of 1.3 m per 1000 m (10 gallons per 1,000 acf). The
rated particulate matter removal efficiency of the venturi scrubber is 99
percent.
Gas exits the scrubber at about 80°C (160°F) and is sent to the,
3-6
-------
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subcooler, which consists of a three-tray packed tower with a demister. Fresh
makeup water (wastewater treatment plant effluent) is added to the subcooler
at a design rate of 454 m3/hr (2,000 gpm). Actual water flow rates and gas
flow rates during normal operation are generally 50 tp 80 percent of the
design rates. The offgas temperature from the subcooler is about 22°C ;
(71°F). Slowdown water from the subcooler is partially recycled to the
precooler and venturi scrubber, with the remainder sent to a drain. The
solids content of the subcooler blowdown streams is estimated to be on the
order of 40 mg solids/liter (3.4 x 10"4 Ib solids/gal).
Offgas from the subcooler is reheated with steam and discharged to a
stack using an induced draft fan. The exhaust stack diameter is 0.8 m (2.5
feet), and the stack discharge is 27 m (90 feet) above the ground. Measured
particulate matter emissions at the exhaust stack during the initial
performance test for the incinerator were 0.20 g/kg (0.40 Ib/ton) dry sludge
solids, or about 0.8 kg/hr (1.7 Ib/hr).
3.4 PROCESS DATA MONITORED ;
Process data monitored by the plant include data on both the incinerator
and the air-pollution control system. The incinerator operating data include
wet sludge feed rate (Ib/hr), sludge solids content (weight %), hearth '
temperatures (°F), and auxiliary fuel usage (scf). The air pollution control
system data include temperatures and pressure drops, (°F, inches of H20) for
the cyclone, precooler, venturi scrubber, and subcooler. Water flow rates for
the precooler, venturi scrubber, and subcooler are also monitored. These data
are maintained in daily logbooks and summarized on a monthly basis using a
computer.
3-8
-------
4.0 TEST DESCRIPTION
This section describes the field sampling, process monitoring, and
analytical activities that were performed at Site SSI-B. The purpose of this
section Js to provide sufficient descriptive information about the test so
that the test data presented in Section 5.0 can be easily understood.
Specific testing details (specific sampling locations and procedures) are
presented in Section 6.0.
This section is divided into three parts. Section 4.1 summarizes field
sampling activities, Section 4.2 summarizes process monitoring activities, and
Section 4.3 summarizes analytical activities performed during the test
program.
4.1 FIELD SAMPLING
Table 4-1 shows the source sampling and analysis matrix for Site SSI-B.
Five sets of dioxin/furan emissions tests were performed on consecutive days
at the scrubber outlet sampling location. This location is shown as Point E-
in Figure 4-1. Dioxin/furan sampling was based on the Modified Method 5 (MM5)
sampling protocol developed by the American Society of Mechanical Engineers
(ASME) for measuring emissions of chlorinated organic compounds. Sampling was
performed isokinetically for a minimum of 4 hours. A total of five MM5 test
runs were performed at Site SSI-B. However, the second test run was
invalidated because the filter popped up from the teflon frit during the test
run and the fourth test run was aborted after completion of 13 of 24 traverse
points due to extended non-representative incinerator operation.
Continuous emissions monitoring (CEM) of 09, CO, CO,, NO , and total
£ b A
hydrocarbons (THC) was performed during the MM5 test runs. These data were
obtained to assess variations in combustion conditions during the sampling
periods. Instantaneous concentrations of each species monitored were
determined and recorded every five minutes by the CEM system.
Three types of process samples were taken during the MM5 test .periods:
sewage sludge, bottom ash, and scrubber blowdown. The sewage sludge samples
were taken to characterize the dioxin/furan precursor contents of the
materials fed to the incinerator. These samples were taken on an hourly
4-1
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4-3
-------
basis, and individual composite samples were prepared for each test run. The
bottom ash and scrubber blowdown samples were taken to determine the potential
for using dioxin/furan analyses of these materials as indicators of the ,
presence or absence of dioxin/furan in the flue gas emissions. These samples
were also taken on an hourly basis. Individual composite ash samples were
prepared for each test run and scrubber blowdown samples were filtered on-site
to provide separate composite samples of scrubber blowdown solids and aqueous
filtrate.
Soil samples were collected from ten locations at the plant site and
combined into a single composite, which was transferred to Tier 7 of the
National Dioxin Study for potential dioxin/furan analysis. ;
i
4.2 PROCESS DATA COLLECTION ;
Process data were collected on-site to characterize the operation of the
multiple hearth incinerator and wet scrubber system during the MM5 test
periods. Incinerator process data obtained include hourly average sludge feed
•rates, continuous strip chart recordings of individual hearth temperatures,
hourly furnace draft measurements, daily average sludge moisture content, and
daily average sludge volatiles content. These data were used with the CEM
data to evaluate and compare combustion conditions during the MM5 test ;
periods.
Scrubber system process data obtained include scrubber water flow rates,
cyclone, venturi and subcooler section pressure drops, and scrubber system
outlet temperature. These data were taken to characterize the consistency of
the scrubber system operation during the three MM5 test periods.
4.3 LABORATORY ANALYSES
Laboratory analyses performed on samples from Site SSI-B included ;
dioxin/furan analyses and dioxin/furan precursor analyses. Samples analyzed
for dioxin/furan are discussed in Section 4.3.1 and samples analyzed for
dioxin/furan precursors are discussed in Section 4.3.2.
4-4
-------
4.3.1 Dioxin/Furan Analyses
All dioxin/furan analyses for Site SSI-B samples were performed by
EMSL-RTP and ECL-Bay St. Louis laboratories, two of three EPA laboratories
collectively referred to as Troika.
Dioxin/furan analyses were performed by gas chromatography/mass
spectrometry. Specific isomers identified included 2378-TCDD and 2378-TCDF.
Other dioxin/furan compounds were quantitated in groups according to the
number of chlorine atoms per molecule. The tetra- through octa-chlorinated
homologues were quantified.
Field samples requiring dioxin/furan analysis were prioritized based on
their relative importance to the Tier 4 program. The priority_.Jeyels, in
order of decreasing importance, were designated Priority 1, Priority 2,'~and~"
Priority 3. \
Priority 1 samples were sent to Troika with instructions to perform
immediate extraction and analysis. These included the MM5 train components
and MM5 field blanks for the scrubber exhaust stack, the MM5 lab proof blank,
the bottom ash samples and the scrubber blowdown solids/filtrate samples.
Priority 2 samples were sent to Troika to be analyzed for dioxin/furan
pending the results of the Priority 1 analyses. The only Priority 2 samples
were the sludge feed samples, which were characterized for precursor content
only.
The composite soil sample (Priority 3} was transferred to Tier 7 of the
National Dioxin Study for potential dioxin/furan analysis.
4.3.2 Dioxin/Furan Precursor Analyses
Dioxin/furan precursor analyses of sludge feed samples were performed by
Radian using gas chromatography/mass spectrometry. The specific dioxin/furan
precursors being analyzed for included chlorophenols, chlorobenzenes, and
PCB's. Composite feed samples were also analyzed for total chlorine by Parr
bomb combustion followed by ion chromatography.
4-5
-------
-------
5.0 TEST RESULTS
The results of the Tier 4 dioxin/furan emissions test of incinerator
SSI-B are presented in this section. The individual test runs are
designated as 1, 3, and 5. Process data obtained during the test runs are
presented in Section 5.1, and continuous monitoring results for 02, CO, C02,
NO , and THC are presented in Section 5.2. The flue gas dioxin/furan
A
emissions data are contained in Section 5.3. Sludge feed dioxin/furan
precursor data are presented in Section 5.4 and the results of dioxin/furan
analyses of bottom ash and scrubber blowdown samples are contained in
Section 5.5.
5.1 PROCESS DATA
Process data were obtained to document incinerator and scrubber system
operation during the testing. The incinerator data are summarized in Section
5.1.1 and the scrubber system data are summarized in Section 5.1.2. Plant
personnel indicated that incinerator and scrubber operation was fairly typical
during the test runs.
5.1.1 Incinerator Operating Data
Data summarizing the operation of multiple hearth sewage sludge
Incinerator SSI-B during the three MM5 test runs are shown in Table 5-1.
Conditions during these test runs were similar except that there was a higher
sludge feed rate and a higher percent solids in the sludge during Run 3 as
compared to Runs 1 and 5. The amount of dry sludge being fed to the
incinerator during Run 3 was 50 percent greater than that fed during Runs -1
and 5.
Oxygen concentration data presented in Table 5-1 are based on analysis
of integrated bag samples collected at the air pollution control system
exhaust stack. Comparison of the oxygen concentrations for the three test
runs shows similar values for Runs 3 and 5. The higher oxygen value for Run 1
compared with Runs 3 and 5 suggests that there was a slightly greater amount
of excess combustion air in the incinerator during this test. Oxygen data
collected using a continuous monitor at the incinerator outlet indicate this
5-1
-------
TABLE 5-1. MEAN INCINERATOR OPERATING PARAMETERS
DURING DIOXIN TESTS AT SITE SSI-B.
Parameter
Wet Sludge Feed Rate
[Mg/hr (tph)]
Dry Sludge Feed Rate
[Mg/hr (tph)]
Percent Solids of Wet
Sludge (wt %)
Percent Volatiles of
Dry Sludge (wt %)
Percent 0, in stack gasa
(vol. %f
Run 1
6.6
(7.3)
2.3
(2.5)
33.9
74.2
17:9
Run 3
8.0
(8.8)
3.4
(3.7)
41.7
74.8
15.6
Run 5
6.3
(6.9)
2.1
(2.3)
32.9
75.1
15.9
Average
6.9
(7.6)
2.5
(2.8)
36.2
74.7
16.5
Oxygen concentration at system exhaust stack based on integrated bag sample
analysis using gas chromatography/thermal conductivity detector.
5-2
-------
same result, but are less conclusive due to a leak in the CEM sampling system
during Run 5. The CEM data are discussed in Section 5.2.
Mean temperatures for each of the incinerator hearths during the MM5
runs are shown in Table 5-2. The temperature profiles for Runs 1 and 5 are
very similar. During Run 3 the temperatures for the hearths above Hearth 3
were higher than during Runs 1 and 5, and the temperatures for the hearths
below Hearth 3 were^lower than during Runs 1 and 5. The observed difference
in the temperature profile for Run 3 is a result of both the higher sludge
feed rate and the higher solids content for Run 3.
Figures 5-1, 5-2, and 5-3 show the continuous strip chart recordings of
the hearth temperatures during the MM5 test runs. As shown in these
figures, the temperature on the primary combustion hearth (Hearth 3) was
maintained constant during all three tests.
5.1.2 Emission Control Equipment Data
Control equipment operating data collected during the MM5 test runs are
summarized in Table 5-3. The data presented in Table 5-3 show average values
for various control system parameters based on hourly readings taken during
each test run. Comparison of data for the three runs shows no significant
differences in operating conditions, with the exception of higher pressure •
drops and greater steam production during Run 3. The higher pressure drops
and greater steam production for Run 3 results from the higher sludge feed
rate (Table 5-1). - •
5.2 CONTINUOUS MONITORING DATA
Mean values and 95 percent confidence intervals for combustion gas
concentrations monitored continuously at the incinerator outlet breeching are
presented 'in Tables 5-4 and 5-5. Concentrations of CO, C07, NO and THC
£ J\
presented in Table 5-5 were corrected or normalized to 3 percent oxygen by
volume. Data in Table 5-4 are given at actual stack 02 levels. The 02, CO,
C02, and NOX values were measured on a dry basis. The sample for THC analysis
was pulled through a sample line separate from that used for the other gases
and was analyzed on a wet basis.
The 02 value for Run 5 was invalidated due to an apparent leak in the
sample acquisition system. Since the CO, CO,, and NOV values presented in
£ J\
5-3
-------
TABLE 5-2. MEAN HEARTH TEMPERATURES DURING DIOXIN
EMISSIONS TESTING AT SITE SSI-B
Hearth
Number
•o
1
2
3
4
5
6
7
8
Hearth Teraoeratures, °F
Run 1
1063
1143
1417
1600
1180
883
180
100
95
Run 3
1245
1180
1508
1603
873
428
140
110
100
Run 5
1148
1120
1420
1585
1105
790
200
140
110 '
b
Average
1152
1148
1448
1596
1053
700 ;
173 ;
117 .
102 ;
aHearths are designated according to plant nomenclature. Hearth No. 0
is the top hearth, Hearth No. 8 is the bottom. Other hearths are
..numbered sequentially from top to bottom.
DNote: °C = (°F - 32J/1.8
5-4
-------
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5-5
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5-6
-------
s
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-------
TABLE 5-3. CONTROL EQUIPMENT OPERATING PARAMETERS
DURING DIOXIN TESTS AT SITE SSI-B.
Parameter
Venturi AP
(in H20)
Venturi Water
Flowrate (gpm)
Steam Production
(Ib/hr)
Subcooler Outlet
Temperature ( F)
Subcooler AP
(in H20)
Scrubber Slowdown3
Run 1
24.8
190
9690
69.0
4.9
936
Run 3
25.4
187
13980
74.9
6.0
1185
Run 5
25.0
190
10040
68.0
4.1
821
Average
25.1 :
189 i
11240
70.6 ;
5.0 i
981
Water Flowrate
Cyclone AP
(in H20)
3.8
7.5
2.9
4.7
aThe scrubber blowdown flowrate is a combination of the venturi and •
subcooler water flowrates.
5-8
-------
TABLE 5-4. SUMMARY OF CONTINUOUS MONITORING
RESULTS FOR SITE SSI-B.
Parameter
Run Number 1
Mean Value
(Std. Dev.)
Run Number 3
Mean Value
(Std. Dev.)
Run Number 5
Mean Value
(Std. Dev.)
Oxygen
(Volume %)
Carbon Monoxide
(ppmv)b
Carbon Dioxide
(volume %)
Nitrogen oxides
(ppmv)b
Total hydrocarbons
(ppmv)c
14.5
(0.5)
2271
(228)
7.3
(1.0)
285
(26)
12. 9d
(6.4)
11.7
(0.4)
894
(244)
9.1.
(1.0)
392
(33)
6.4
(2.2)
NAa
NA
NA
NA
48.8
(18.7)
Not available. Oxygen value for this run was invalidated due to a leak in
the continuous monitor sampling system. Assumed flue gas 0? to be 13 percent
by volume. Values for CO, CO,,, and NOV corrected to 3% 00 are presented in
Table 5-5. ^ x Z
ppmv = parts per million by volume.
°Parts per million by volume as propane.
Based on only 21 consecutive observations. No data collected during second
half of test run due to instrument malfunction.
5-9
-------
TABLE 5-5. SUMMARY OF CONTINUOUS MONITORING RESULTS FOR
INCINERATOR SSI-B (VALUES REFERENCED TO 3% OXYGEN)
Parameter
Run Number 1
Mean Value
(Std. Dev.)
Run Number 3
Mean Value
(Std. Dev.)
Run Number 5
Mean Value
(Std. Dev.)
Oxygen
(Volume %)
Carbon Monoxide
(ppmv)b
Carbon Dioxide
(volume %)c
Nitrogen Oxides
(ppmv)b
Total hydrocarbons .
(ppmv)d
14.5
(0.5)
6337
(627)
20.3
(1.9)
804i3
(53.2)
36. le
(4.5)
11.7
(0.4)
1745
(507)
. 17.7
' (1.9)
761.3
(70.3)
12.5
(3.3)
NAa
i
5947 :
(1096) ;
18.7
(4.7) !
798.9 :
(71.3)
110.6
(17)
Not available. Oxygen value for this run was invalidated due to a leak in
the continuous monitor sampling system. Assumed flue gas 02 to be 13 percent
by volume.
ppmv ~ parts per million by volume corrected to 3% oxygen.
cVolume percent corrected to 3% oxygen.
Parts per million by volume as propane, corrected to 3% oxygen.
eBased on only 21 consecutive observations. No data collected during second
half of test run due to instrument malfunction.
5-10
-------
Table 5-5 are'corrected to 3 percent 02, the presence of the sampling system
leak does not affect the results for these three parameters. There is no
reason to suspect that a leak was also present in the separate sampling system
used for THC. To correct the THC value for Run 5 to 3 percent CL, the actual
mean flue gas 02 concentration at the sample location was assumed to be 13
percent by volume.
Comparison of the mean CL values in Table 5-5 for Runs 1 and 3 shows a
somewhat lower value for Run 3. The lower CL observed for Run 3 is expected
to be the result of a higher sludge feed rate during this test run. Data
presented for CO in Table 5-5 show similar concentrations for Runs 1 and 5
with a considerably lower concentration for Run 3. Concentrations of C02 and
NO corrected to 3 percent 02 were similar for all three test runs.
Comparison of the mean concentrations in Table 5-5 for THC shows a relatively
high THC concentration for Run 5. There is no apparent explanation for the
higher THC value for this run.
Instantaneous five-minute values for the continuously monitored gases
are shown graphically in Figures 5-4 through 5-8 and are tabulated in
Appendix A-2. Values for CO, C02, NOX, and THC are again reported as
corrected to 3 percent 02 by volume. Review of the data presented in
Figures 5-4 through 5-7 for 02, CO, C02, and NOX indicate steady operation of
the incinerator throughout each test run. Data presented in Figure 5-8,
however, show an increase in THC concentration during Runs 1 and 5 and a
.slight decrease in concentration during Run 3. In reviewing the THC data
presented in Figure 5-8, the difference in the time scale for Run 1 and the
concentration scale for Run 5 should be noted. Also, no THC data were
collected during the second half of Run 1 because of an instrument
malfunction.
5.3 FLUE GAS PARAMETER DATA
Table 5-6 summarizes flue gas temperature, moisture content, and
volumetric flow rate data obtained at the incinerator SSI-B outlet stack.
These parameters were fairly consistent between the three test runs. The
average flue gas temperature and moisture content measured at the scrubber
outlet sampling location were 77.1°C (172°F) and 3.72 percent by volume,
5-11
-------
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TABLE 5-6. FLUE GAS PARAMETERS FOR INCINERATOR SSI-B
(AIRSTREAM IN STACK AT SCRUBBER OUTLET)
Flue Gas Parameters
Temperature (°C)
Moisture (Vol. %)
Vol umetri c F1_ow_Rat_e
Actual (acmm)
Dry Standard (dscmm)
Run 01
76.4
3.38
748
590
Run 03
76.4
4.76
792
622
Run 05
78.4
3.01
667
534
Average
77.1
3.72
736
582
5-17
-------
•respectively. The average exhaust gas flow rate under actual stack [
temperature and moisture conditions was 736 acmm (25,990 acfm),-and the -;
average dry, standard flow rate was 582 dscmm (20,550 dscfm). Standard EPA
conditions are 20°C (68°F) and 1 atm.
5.4 DIOXIN/FURAN EMISSIONS DATA
Emission concentrations and emission rate data determined for 2378-TCDD,
total PCDD, and total PCDF during Runs 1, 3 and 5 are shown in Table 5-7.
Data presented in Table 5-7 include the total dioxin/furan collected in the
MM5 sample train (probe, filter, XAD sorbent trap and impingers). Analytical
values obtained for each MM5 train were not corrected for blanks. Surrogate
recoveries and blank sample train results are discussed in Section 8.0.
As shown in Table 5-7, no detectable quantities of 2378-TCDD were found
for any of the three test runs. Emission rates of total PCDD and PCDF
averaged 11.6 and 194 ug/hr, respectively. :
Isomer- and homologue specific emission concentration data are summarized
in Tables 5-8 and 5-9 for the three test runs. Run-specific data tables
showing homologue emission concentrations in both ng/clscm and
parts-per-trillion units and homologue emission rates in ug/hr units are •
included in Appendix D. Detectable quantities were found for about half of
the target isomers and homologues. Figure 5-9 is a histogram that shows the
relative distributions of the homologues that were detected in the stack gas.
Emission factors based on incinerator feed rates (dry basis) are shown in
Table 5-10. Average emissions factors for total PCDD's and total PCDF's were
0.05 ug and 0.83 ug per kg of dry solids feed, respectively.
5.5 DIOXIN/FURAN PRECURSOR DATA
Composite sludge feed samples collected for each test run were analyzed
for chlorobenzenes, chlorophenols, chlorinated biphenyls, and total chlorine
content.
The results of the compound-specific precursor analyses are summarized in
Table 5-11. As shown in Table 5-11, the only precursors found in the sludge
5-18
-------
TABLE 5-7. SUMMARY OF DIOXIN AND FURAN EMISSION CONCENTRATION
AND EMISSION RATE DATA FOR SITE SSI-B (STACK LOCATION)
Run Number 2378 TCDD
Emission Rate (ug/hr)
Run 01
Run 03
Run 05
Average
Emissions Concentration
at actual Op, ng/dscm
Run 01
Run 03
Run 05
Average
Emissions Concentration
(corrected to 3% 02), ng/dscm
Run 01
Run 03
Run 05
Average
NDa
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
Total PCDD
21.8
6.53
6.44
11.6
0.62
0.18
0.20
0.33
3.52
0.59
0.68
1.60
Total PCDF
396
66.2
121
194
11.2
1.77
3.79
5.59
64.0
5.94
12.9
27.9
ND = not detected. Detection limits ranged from 0.4 to 8.4 ug/hr and 0.01
to 0.24 ng/dscm, depending on the particular homologues.
DFlue gas concentration data corrected, to 3% 0,, using the EPA Method 3
data presented in Table 5-1. L
5-19
-------
TABLE 5-8. SUMMARY OF DIOXIN/FURAN EMISSIONS DATA FOR SITE SSI-B
(At Actual Stack Oxygen Concentration) •
Dioxin/Furan
Isomer
Isomer Concentration in Flue Gas
(ng/dscm)
Run 01 Run 03 Run 05
Avg,
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
ND( 1.15E-02)
1.92E-01
ND( 1.92E-02)
ND( 1.85E-01)
1.15E-01
3.08E-01
6.15E-01
7.31E-01
7.50E+00
2.08E+00
8.46E-01
ND( 2.38E-01)
3.85E-02
1.12E+01
ND( 6.00E-02)
ND( 6.00E-02)
ND( 4.50E-02)
ND( 1.02E-01)
ND( 6.75E-02)
-1.75E-01
1.75E-01
2.50E-01
1.52E+00
ND( 4.50E-02)
ND( 5.75E-02)
ND( 7.25E-02)
ND( 1.25E-02)
1.77E+00
ND( 1.15E-02)
2.87E-02
ND( 5.75E-02)
.~ND4~8,62E-03)-
ND( 4.02E-02)
1.72E-01
2.01E-01
• 4.02E-01
2.67E+00
7.18E-01
ND( 2.13E-01)
ND( 2.01E-02)
ND( 1.72E-02)
3.79E+00
.OOE+00
7.37E-02
.OOE+00
.OOE+00
3.85E-02
2.18E-01
3.31E-01
4.61E-01
3.90E+00
9.32E-01
2.82E-01
.OOE+00
1.28E-02'
5.59E+00
NOTE: Isomer concentrations shown are at as-measured oxygen conditions.
ND » not detected (detection limit in parentheses).
ng - 1.0E-09g
8760 operating hours per year
5-20
-------
TABLE 5-9. SUMMARY OF DIOXIN/FURAN EMISSIONS DATA FOR SITE SSI-B
(Concentrations Corrected to 3% Oxygen)
Dioxin/Furan
Isomer
Isomer Concentration in Flue Gas
(ng/dscm @ 3% oxygen)
Run 01 Run 03 Run 05
Avg.
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
ND(
ND(
ND(
ND(
6
1
1
1
6
1
3
4
4
1
4
1
2
6
.59E-02)
.10E+00
.10E-01)
.05E+00)
.59E-01
.76E+00
.52E+00
.18E+00
.29E+01
.19E+01
.84E+00
.36E+00)
.20E-01
.40E-I-01
ND<
ND'I
NDI
NDI
ND
ND
ND
ND
ND
; 2
, 2
[ 1
[ 3
[ 2
5
5
8
5
i
i
o
4
5
.01E-01)
.01E-01)
.51E-01)
.43E-01)
.26E-01)
.86E-01
.86E-01
.36E-01
.10E+00
.51E-01)
.92E-01)
.43E-01)
.18E-02)
.94E+00
ND(
ND(
ND(
ND(
ND(
ND(
ND(
3
9
1
2
1
5
6
1
9
2
7
6
5
1
.90E-02)
.74E-02
.95E-01)
.92E-02)
.36E-01)
.84E-01
.82E-01
.36E+00
.06E+00
.44E+00
.21E-01)
.82E-02)
.84E-02)
.29E+01
3
2
9
1
2
1
4
1
7
2
.OOE+00
.99E-01
.OOE+00
.OOE+00
.20E-01
.76E-01
.59E+00
.13E+00
.90E+01
.77E+00
.61E+00
.OOE+00
.33E-02
.76E+01
NOTE: Isomer concentrations shown are corrected to 3% oxygen.
ND = not detected (detection limit in parentheses).
ng = 1.0E-09g
8760 operating hours per year
5-21
-------
DIOX1N HOMOLOGUES AT THE OUTLET
SSl-B
1 -
0.9 -
o.a-
O.7-
O.8-
0.5-
O.4-
O.3-
0.2-
O.1 -
1
I
-
1
\
1
1
i
i
I
2378 TCDD Othar TCDD Panta-CDD Hexa-CDD H«pta-COO Octa-CDD
RUN 01
DIOXIN
RUN 03
,^^,
K3 RUN 03
FURAN HOMOLOGUES AT THE-OUTLET
SSI-B
0.9-
O.B-
0.7-
0.8-
O.S-
O.4-
0.3
0.2
0.1
X^
?A
xf
/M
4%
'/w
237B TCOF Oth«r VcDF Penta-COF H«xa-COF H«pta-COF Octa-CDF
RUN O1
FURAN HOMOLOttUES,__
RUN O3 PTXl RUN OS
Figure 5-9. Distribution of dioxin and furan homologues in
scrubber outlet emissions.
5-22
-------
TABLE 5-10. DIOXIN/FURAN EMISSION FACTORS FOR'SITE SSI-B
Dioxin/Furan
Isomer
Dioxin/Furan Emission Factors (ug/kg)
Run 01 Run 02 Run 03
NO - not detected (detection limit in parentheses).
ug » 1.0E-06g
8760 operating hours per year
Avg.
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS •
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF •
Octa-CDF
Total PCDF
ND( 1.77E-04)
2.96E-03
ND( 2.96E-04)
ND( 2.84E-03)
1.77E-03
4.73E-03
9.47E-03
1.12E-02
1.15E-01
3.19E-02
1.30E-02
ND( 3.67E-03)
5.92E-04
1.72E-01
-
ND{ 6.59E-04)
ND( 6.59E-04)
ND( 4.94E-04)
ND( 1.12E-03)
ND( 7.41E-04)
1.92E-03
1.92E-03
2.74E-03
1.67E-02
ND( 4.94E-04)
ND( 6.31E-04)
ND( 7.96E-04)
ND( 1.37E-04)
1.95E-02
ND( 1.75E-04)
4.38E-04
ND( 8.77E-04)
ND( 1.31E-04)
ND( 6.14E-04)
2.63E-03 .
3.07E-03
6.14E-03
4.08E-02
1.10E-02
ND( 3.24E-03)
ND( 3.07E-04)
ND( 2.63E-04)
5.79E-02
-
.OOE+00
1.13E-03
.OOE+00
.OOE+00
5.92E-04
3.09E-03
4.82E-03
6.71E-03
5.76E-02
1.43E-02
4.34E-03
.OOE+00
1.97E-04
8.32E-02
5-23
-------
TABLE 5-11. SUMMARY OF PRECURSOR ANALYSES
ON SLUDGE FEED SAMPLES
Precursor Compounds
TOTAL CHLORINATED BENZENES
Dichlorobenzenes
Other chlorobenzenes
TOTAL CHLORINATED BIPHENYLS
TOTAL CHLORINATED PHENOLS
• Precursor Concentration (DDITI bv weiqht)
Run 1
0.03
0.03
NDa
ND
ND
Run 3
0.04
0.04
ND
ND
ND
Run 5
0.02 !
0.02 :
ND
ND
ND
ND - not detected. Detection limit was approximately 0.02 parts per million.
5-24
-------
feed was dichlorobenzene, at levels ranging from 0.02 to 0.04 ppm by weight.
No chlorinated biphenols or chlorinated phenols were found.
Results for the total chlorine analyses are presented in Table 5-12. The
sludge chlorine content was similar for all three test runs and averaged 214
ppm by weight.
5.6 SLUDGE, BOTTOM ASH AND SCRUBBER SLOWDOWN DIOXIN/FURAN DATA
Samples of the sludge feed were taken during the test runs and composited
for analysis. The dioxin/furan concentrations in the sludge feed are shown in
Table 5-13. With the exception of TCDD, TCDF, and penta-CDF, all other
homologues were detected. Hourly samples of incinerator bottom ash and
scrubber blowdown water were taken during the test runs and composited for
analysis. The dioxin/furan concentrations in the bottom ash are shown in
Table 5-14. The only homologues detected were octa-CDD, TCDF, and octa-CDF.
The scrubber water samples were filtered, resulting in two components:
filterable scrubber solids, and scrubber filtrate. Approximately 16 liters of
scrubber blowdown water was filtered each run. Results of the dioxin/furan.
analysis of the scru.bber filtrate are shown in Table 5-15. Only TCDF and
penta-CDF homologues were detected at concentrations less than 2 ng per 16
liters of filtrate. Results of the dioxin/furan analysis of the filterable
scrubber solids are shown in Table 5-16. All of the homologues were detected
in these samples.
5.7 SOIL DIOXIN/FURAN DATA
The soil sample was turned over to Tier 7 for analysis. Because of the
low stack concentrations of dioxins/furans, it was decided that analysis of
the soil sample was not warranted.
5-25
-------
TABLE 5-12. SUMMARY OF TOTAL CHLORIDE DATA IN SLUDGE FEED SAMPLES
Test
Run
Total
Chloride
(ppm)
01
02
05
Average
208
201
232
214
appm * parts per million, weight basis (ug/g),
blank corrected.
5-26
-------
TABLE 5-13. DIOXIN/FURAN CONCENTRATIONS IN THE SLUDGE FEED AT-SITE SSI-BC
Dioxin/Furan
Homo!ogue
Dioxin/Furan
Concentration (ppb)
Dioxins
2378-TCDD
Other TCDD
Penta-CDD
Hexa CDD
Hepta CDD
Octa CDD
Total PCDD
ND (0.03)
0.05
1.4
0.9
2.8
5.15
Furans
2378-TCDF
Other TCDF
Penta-CDF
Hexa CDF
Hepta CDF
Octa CDF
Total PCDF
ND (0.05)
ND (0.05)
0.07
0.2.
0.1
0.37
ND = Not detected at specified minimum limit of detection.
Composite sludge feed sample.
ND for 2378 isomers is estimated to be less than half of
the ND shown for TCDD's and TCDF's.
5-27
-------
TABLE 5-14. DIOXIN/FURAN CONCENTRATIONS IN THE BOTTOM ASH AT SITE SSI-B
Dioxin/Furan
Homologue
Dioxins
2378-TCDD
Other TCDD
Penta CDD
Hexa CDD
Hepta CDD
Octa CDD
Total PCDD
Furans
2378-TCDF
Other TCDF
Penta CDF
Hexa CDF
Hepta CDF
Octa CDF
Total PCDF
Dioxin/Furan
Run 01
ND
ND
ND
ND
ND
0.01
0.01
ND
ND
ND
ND
ND
ND
ND
Concentration
Run 03
ND
ND
ND
ND
ND
0.01
0.01
ND.
0.04
• ND
ND
0.007
ND
0.047
(cob)
Run 05
ND
ND
ND
ND
ND
0.01
0.01
ND
0.08
ND
ND
ND
ND
0.08
ND = not detected. Detection limits ranged from 0.001 to
0.01 ppb. The average detection limit was 0.01 ppb.
5-28
-------
TABLE 5-15. DIOXIN/FURAN CONCENTRATIONS IN SCRUBBER FILTRATE AT SITE SSI-B
Dioxin/Furan
Homologue
Pi oxi n/Furan Concentrati on (ng V
Run 03
Run 05
Dioxins
2378-TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
Furans
2378-TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
•Octa-CDF
Total PCDF
ND
0.2
ND
ND
ND
ND
0.2
ND
1.7
0.7
ND
ND
ND
2.4
Approximately 16 liters of scrubber blowdown water was filtered
each run. Results of the analysis for Run 01 were unavailable.
ND = Not detected. The detection limits for dioxins ranged
from 0.01 to 0.53 ng/sample. For furans, the detection limits
ranged from 0.1 to 0.2 ng/sample.
5-29
-------
TABLE 5-16.
DIOXIN/FURAN CONCENTRATIONS IN THE FILTERABLE
SCRUBBER SOLIDS AT SITE SSI-B
Dioxin/Furan
Homologue
Dioxin/Furan Concentration (ODD)
Run 03 Run 05
Dioxins
2378-TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
0.002
0.05
0.03
0.14
0.15
0.44
ND (0.005)
0.11 ,
0.02
0.08
0.08
0.11
0.40
Furans
2378-TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
•
0.09
0.51
0.19
0-.16
0.12
0.03
1.1
0.54
2.6
1.2
0.8
0.13
0.02
5.3
ND - Not detected at specified minimum limit of detection.
5-30
-------
6.0 SAMPLING LOCATIONS AND PROCEDURES
Samples were collected from six different locations around the Site SSI-B
incinerator. The specific sampling locations are shown in Figure 6-1. Two of
the locations were for gaseous sampling, one was for liquid/slurry sampling,
and three were for solids sampling. The source sampling and analysis matrix
in Table 6-1 shows the sample location, the parameter measured, the sampling
method, and the analysis method.
Details on the sampling locations and methods are discussed in Sections
6.1 through 6.3. Analytical procedures for continuous monitoring samples and
molecular weight determinations are included in Section 6.1. All other
analytical procedures are discussed in Section 7.
6.1 GASEOUS SAMPLES
Two types of gaseous samples were taken during the testing: Modified
Method 5 (MM5) and continuous monitoring (CEM). The sampling locations and
methods are further discussed below.
6.1.1 Gaseous Sampling Locations
Outlet Exhaust Stack Location
The system outlet exhaust stack location is shown as Point E in
Figure 6-1. This location was used for dioxin sampling using MM5 and for gas
velocity, molecular weight, and moisture determinations using EPA Method? 1
through 4.
Exhaust gases from the incinerator and associated control equipment were
vented through a jacketed 0.8m (2.5 ft) diameter stack. Dimensions of the
outlet exhaust stack are shown in Figure 6-2. The outer stack had a 0.9m (3
ft) diameter and four 10cm (4 inch) sampling ports that extended through the
annul us between the two stacks. A fan located approximately 3.7m (12 ft)
below the sampling ports forced ambient building air through the annular
space. None of this air mixed with the incinerator exhaust gases prior to the
sampling ports. The nearest downstream flow disturbance was the stack
discharge, located 1.5m (5 ft) or 2.0 duct diameters downstream of the ports.
A total of 24 traverse points were used for velocity determination at this
location.
6-1
-------
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Due to the presence of cyclonic flow, straightening vanes had to be
installed in the inner stack to allow for valid MM5 testing. The nearest
upstream flow disturbance prior to the straightening vanes was the ID fan,
which was located 7.9m (26 ft) or 10.4 duct diameters upstream of the ports.
There is no apparent reason for the observed cyclonic flow.
The straightening vanes, which consisted essentially of a 0.3m (1 ft)
long honeycomb of 8cm (3 inch) square cells, was slipped into the stack so
that the top of the vanes was 0.6m (2 ft) below the ports. The straightening
vanes removed the cyclonic flow although the gas velocity remained low in the
center of the stack and high near the stack walls.
Incinerator Outlet Sample Location
The incinerator outlet location is shown as Point B on Figure 6-1. This
location was used for obtaining a gas sample for continuous monitoring of 02,
C0?, CO, NO , and THC. Sample acquisition was accomplished using an in-stack
t *\ - ,
filter probe and heat-traced Teflon sample line leading from the incinerator
outlet location to the continuous monitoring equipment.
6.1.2 Gaseous Sampling Procedures
Gas sampling procedures used during this program are discussed in detail
in the Tier 4 Quality Assurance Project Plan (QAPP). A brief description of
each method and any necessary deviations from the procedures outlined in the
QAPP are provided in the following sections.
Modified Method 5 (MM5)
Gas sampling for dioxins was conducted according to the latest draft
(October 1984) of the American Society of Mechanical Engineers (ASME)
chlorinated organic compound sampling protocol; This sampling method is a
modified version of EPA Method 5 that includes a solid sorbent module (XAD-2)
for trapping vapor phase organics. The MM5 sampling train was used to collect
samples at the system outlet exhaust stack. Following sample recovery, the
various parts of the sample (filter, solvent rinses, sorbent trap, etc.) were
sent to EPA's Troika laboratories to quantify the 2378-TCDD and tetra- through
octa-dioxin/furan homologues present in the samples.
A total of five MM5 test runs were conducted at the outlet exhaust stack
location with one test run being conducted per test day. The second test run
was invalidated because the filter popped up from the Teflon frit sometime
6-5
-------
during the test run. While the sample train still met all leak check
requirements, a decision was made to discard the sample because some of the
particulate matter may have bypassed the filter and entered the resin trap.
The fourth test run was aborted after completion of 13 of 24 traverse points.
The run was aborted due to large fluctuations in sludge composition and ;
moisture content that led to extended periods of non-representative
incinerator operation.
Based on the QAPP, the desired isokinetic sampling rate for the MM5 train
is 0.85 m3/hr (0.5 scfm) to provide a sample volume of 3.4 m3 (120 scf) over a
4 hour sampling period. Due to the stack gas velocity at this site and the
available nozzle sizes, isokinetic sampling had to be conducted at a sampling
rate of approximately 0.68 m3/hr (0.40 scfm). During the first run, each of
24 traverse points was sampled for 10 minutes, providing a total sample volume
of 2.7 m3 (95 scf). The sampling time at each point was increased to
15 minutes for the remaining test runs, providing total sample volumes of
approximately 4.0 m (140 scf).
A schematic diagram of the MM5 sampling train is shown in Figure 6-3,
Flue gas is pulled from the stack through a nozzle and heated gas probe.
Particulate matter is removed from the gas stream by means of a fiberglass
filter housed in a Teflon-sealed glass filter holder maintained at 120 + 14°C
(248 + 25°F). The gas passes through a sorbent trap similar to that
illustrated in Figure 6-4 for removal of organic constituents. The trap
consists of separate sections for (1) cooling the gas stream, and
(2) adsorbing the organic compounds on Amberlite XAD-2 resin (XAD). A
chilled impinger train is used to remove water from the flue gas, and a dry
gas meter is used to measure the sample ga's flow.
Volumetric Gas Flow Rate Determination |
The volumetric gas flow rate was determined during this program using
procedures described in EPA Method 2. Based on this method, the volumetric
gas flow rate1is determined by measuring the cross-sectional area of the duct
and the average velocity of the flue gas. The average flue gas velocity is
calculated from the average gas velocity pressure ( P) across the S-type
pitot, the average flue gas temperature, wet molecular weight, and the
absolute static pressure.
6-6
-------
o
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6-7
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XAO-2
Trap
28/12
Thermocouple Well
Coarse Frit
28/12
Figure 6-4. ADSORBENT SAMPLING SYSTEM
6-8
-------
Flue Gas Moisture Determination
The moisture content of the flue gas was determined using the methodology
described in EPA Method 4. Based-on this method, a known volume of
particulate-free gas is pulled through a chilled impinger train. The quantity
of condensed water is determined gravimetrically and then related to the
volume of gas sample to determine the moisture content.
Flue Gas Molecular Weight Determination
During testing, the integrated sampling technique described in EPA
Method 3 was used to obtain an integrated flue gas sample for fixed gas (CL,
C02, CO, N2) analysis. A small diaphragm pump and a stainless steel probe
were used to extract a single point flue gas sample which was collected in a
R
Tedlar bag. Moisture was removed from.the--gas-sample by a water-cooled
condenser so that the fixed gas analysis is on a dry basis.
The fixed gas composition of the gas sample was determined using a
Shimadzu Model 3BT analyzer instead of the Fyrite or Orsat analyzer prescribed
in Method 3. The Shimadzu instrument employs a gas chromatograph and a
thermal conductivity detector to determine the fixed gas composition of the
sample. Calibration of the Shimadzu analyzer was conducted according to the
procedures outlined in the QAPP, which involved analysis of one or more
standards of appropriate composition immediately before or after sample
analysis.
Continuous Monitoring
Continuous monitoring was performed at the incinerator outlet sampling
location for 02, C02, CO, NOX, and THC. The continuous monitoring was
performed throughout the 6 to 8 hour period that dioxin sampling was being
conducted each test day. The primary intent of the continuous monitoring
effort was to (1) observe fluctuations in flue gas parameters, and (2) provide
an indication of combustion conditions. Sample acquisition was accomplished
p
using an in-stack filter probe and a 30m (100-feet) heat-traced Teflon sample
line connected to a mobile laboratory. The heat-traced sample line was
maintained at a temperature of 149°C (300°F) to prevent condensation in the
sample line. The stack gas sample was drawn through the filter and sample
line using pumps located in or near the mobile laboratory. Sample gas for CO,
C02, NO , and 02 analysis was pumped through a sample gas conditioner,
6-9
-------
consisting of an ice bath and knockout trap, to remove moisture and thus .
provide a dry gas stream for analysis. A separate unconditioned gas sample
was supplied to the THC analyzer for analysis on a wet basis.
An Anarad Model 412 non-dispersive infrared (NDIR) analyzer was used to
measure CO and C02; a.Beckman Model 755 paramagnetic analyzer was used to
measure 02; a TECO Model 10 analyzer was used to measure NOX; and a Beckman
Model 402 flame'ionization analyzer was used to measure THC. Calibration of
the continuous monitors was performed according to the procedures outlined in
the QAPP. These procedures included a three point (tv/o upscale plus zero)
linearity check on the first test day, single point and zero point calibration
checks daily, and single point drift checks at the end of each test day.
6.2 LIQUID/SLURRY SAMPLES
The only liquid or slurry sample collected at Site SSI-B was scrubber
system blowdown. The sample was taken from a tap valve on a stream consisting
of the combined effluents from the venturi scrubber and the subcooler. Grab
samples of scrubber blowdown were taken hourly during each MM5 test run. The
grab samples were, either composited for weight percent solids determination or
filtered to provide composite solids and aqueous filtrate samples for
dioxin/furan analysis.
To acquire the samples, the tap valve was fitted with a 1.2 m (4 ft)
length of 1/4-inch Teflon tubing as shown in Figure 6-5.. The sample was
collected by placing the tubing in the sample jar and opening the valve to
admit a moderate flow of slurry. The conduit line was flushed before the
sample was taken and covered with hexane-rinsed foil between sampling times.
Hourly grab samples of scrubber blowdown were filtered using the
apparatus shown schematically in Figure 6-6. The apparatus consisted of a
.pressure filtration vessel, WhatmanR No. 42 filters, a tank of high-purity
nitroge'n, a two-stage regulator, and a container for filtrate collection.
Approximately 2 liters of scrubber blowdown slurry were filtered each "hour.
One liter at a time was poured into the pressure vessel and the vessel was
slowly pressurized with the nitrogen to a maximum pressure of 50 psig. The
time required to filter the two liters was approximately 20 to 30 minutes.
6-10
-------
LINE
OR
TANK
WALL
•
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lit
sx
=»:
=3=?
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(20 In.)
FIGURE 6-5. SCHEMATIC OF TAP SAMPLING
6-11
-------
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6-12
-------
The filters used to separate the scrubber solids and aqueous filtrate
have a rated collection efficiency of greater than 99 percent for particles
larger than 3 microns. To minimize the required filtering time, the filters
were replaced after every two liters of scrubber blowdown were filtered. The
used filters and collected solids were removed from the pressure device with
pre-cleaned teflon-coated tweezers and placed in a precleaned Petri dish.
6.3 SOLIDS SAMPLING
Three types of solid samples were collected at Site SSI-B: sludge feed,
incinerator bottom ash, and soils from the plant property. Sampling
procedures and locations are discussed below.
Sludge Feed Sampling
Sludge feed samples were collected from the conveyor belt feeding the
incinerator. Grab samples were'collected hourly by catching 500 mg of sludge
in a glass jar as it fell from the conveyor into the incinerator. The grab
samples were composited in a precleaned stainless steel bucket by mixing with
a potato masher. Composite sludge feed samples were analyzed for dioxin,
furan, and dioxin precursors.
Incinerator Bottom Ash Sampling
Incinerator bottom ash samples were taken hourly at the point of ash
discharge from the incinerator using a precleaned metal scoop. Hourly samples
for each MM5 test run were composited in a precleaned metal bucket and later
analyzed for dioxin and furan content.
Soil Sampling
The soil sample for Site SSI-B consisted of a composite of 10 samples.
Traditional wind patterns, as established by wind direction data provided by
the plant, and routes normally taken by trucks hauling the ash were used as
criteria for determining the soil sample location. All 10 samples were
collected from a single grassy area approximately 0.25 miles from the
incineration stacks and ash handling station. This area ran parallel to the
road normally taken by trucks hauling ash for disposal. The soil samples were
collected using a bulb planter which was pushed approximately 3 inches into
the soil. The sample was first placed in a pre-cleaned stainless steel bucket
and then transferred with hexane-rinsed aluminum foil to amber glass sample
jars.
6-13
-------
-------
7.0 ANALYTICAL PROCEDURES
Laboratory procedures used to quantify dioxins/furans and dioxin/furan
precursors in the Tier 4 samples are described in this section. MM5 train
samples were analyzed by two of EPA's Troika laboratories for dioxin/furan
content. Procedures used for these analyses are described in detail in the
Analytical Procedures and QA Plan for the Analysis of Tetra through Octa CDDs
and CDFs in samples from Tier 4 Combustion and Incineration Processes
(addendum to EPA-600/3-85-019, April 1985). These procedures are summarized
in Section 7.1.
Sludge feed .samples from Site SSI-B were analyzed by Radian to determine
concentrations of chlorinated phenols (CP), chlorobenzenes (CB), polychlor-
inated biphenyls (PCBs), and total chlorine. Procedures used for these
analyses are detailed in Section 7.2.
7.1 DIOXINS/FURANS .
The analytical procedures summarized in this section were used by Troika
for dioxin/furan analysis of MM5 train samples from Site SSI-B. Samples
consisting of organic solvents, aqueous solutions, and solids were prepared
for analysis using slightly different procedures. The organic solvent samples
consisted of rinses from the MM5 probe, nozzle, filter housing and condenser
coil. Aqueous samples consisted of impinger catch solutions, and solid
samples included filters and XAD resin. Isotopically-labeled surrogate
compounds were added to all samples prior to extraction to allow determination
of method efficiency and for quantification purposes.
Organic liquid samples (e.g., acetone and methylene chloride-based MM5
train rinses) were concentrated using a nitrogen blowdown apparatus. The
residue, which contained particulate matter from the MM5 train probe and
nozzle, was combined with the filter and handled as a solid sample. Solid
samples were extracted with benzene in a Soxhlet apparatus for a period of at
least 16 hours. The extract was. concentrated by nitrogen blowdown and
subjected to chromatographic cleanup procedures.
Aqueous solutions (e.g., MM5 train impinger samples) were extracted with
hexane by vigorous shaking for a three hour period. This extraction procedure
was repeated three times, with the organic fractions ultimately being combined
and concentrated for chromatographic cleanup.
7-1
-------
Aqueous solutions (e.g., MM5 train impinger samples) were extracted with
hexane by vigorous shaking for a three hour period. This extraction procedure
was repeated three times, with the organic fractions ultimately being combined
and concentrated for chromatographic cleanup.
The cleanup procedure involved using liquid chromatographic columns to
separate the compounds of interest from other compounds present in the
samples. Four different types of columns were used: a combination acid and
base modified silica gel column, a basic alumina column, a PX-21 carbon/eelite
545 column and a silica/did! micro column. These were used in successive
steps, with the last two being used only if necessary.
The cleaned samples were analyzed using high resolution gas
chromatography/high resolution mass spectrometry (GC/MS). Conditions for the
analyses were as follows:
Gas Chromatograph - Injector configured for capillary column, splitless
injection, injector temperature 280°C, helium carrier gas at 1.2 ml/min,
initial column temperature 100°C: final column temperature 240°C, interface
temperature 270°C.
Mass Spectrometer - Varian/MAT Model 311A, electron energy 70ev, filament
emission IMA, mass resolution 8000 to 10,000, ion source temperature 270°C.
7.2 DIOXIN/FURAN PRECURSORS
Feed samples for Site SSI-B were analyzed by Radian/RTP for chlorophenols
(CP), chlorobenzenes (CB) and polychlorinated biphenyls (PCBs) by GC/MS and
total chlorine by Parr Bomb combustion followed by ion chromatography. '.
Analytical procedures are discussed in the following sections.
7.2.1 GC/MS Analyses
The analytical procedures used for determining CP, CB, and PCB
concentrations in feed samples are modified versions of procedures typically
used for the analysis of MM5 train components. These procedures involve
initial extraction of the sample with an appropriate solvent, preliminary
separation of the compounds of interest by solvent partitioning and liquid
chromatography, and,analysis of the processed fractions. Solutions containing
7-2
-------
CB and PCB are injected directly into the GC/MS, and solutions containing CP
are derivatized prior to injection. Details on the procedures used for
Site SSI-B samples are provided in the sections below.
7.2.1.1 Sample Preparation. A flow chart for the sample preparation
procedure used for Site SSI-B feed samples is shown in Figure 7-1. The first
step in the procedure involved adding labeled surrogate compounds to provide a
measure of extraction method efficiency. The next step involved adding a
mixture of 50/50 MeCl2/Hexanes to the sample and sonicating the sample for 30
minutes. The sonicated sample was filtered and the filtrate was extracted
three times in a separatory funnel with 50 ml 0.5 N NaOH and the aqueous and
organic fractions were saved for derivatization and/or further cleanup. The
aqueous fraction (or acids portion) was acidified to pH 2.0 with 1:1 H2S04 and
then extracted three times with 50 ml MeCK. The MeClp from this extraction
was dried with anhydrous Na2S04, exchanged to benzene, and concentrated using
a nitrogen blowdown apparatus. Acetylation of any CP present in the sample
involved the following
steps:
1. 2.0 ml isooctane, 2.0 ml acetonitrile, 50 uL pyridine, arid 20 uL
acetic anhydride were added to the extract. The test tube
containing the extract was placed in a 60 C water bath for 15
minutes and was shaken 30 seconds every 2 minutes.
2. 6 ml of 0.01 N H,P04 to the test tube, and the sample was agitated
for 2 minutes on a wrist action shaker.
3. The organic layer was removed and the quantitation standard was
added. The sample was concentrated in a Reacti-Vial at room
temperature (using prepurified N2) to 1 ml prior to GC/MS analysis.
Cleanup of the organic (or base/neutrals) layer from the first 0.5 N NaOH
extraction involved successively washing the extract with concentrated H2$04
and double-distilled water. The acid or water was added in a 20 ml portion
and the sample was shaken for four minutes. After the aqueous (or acid) and
organic layers were completely separated, the .acid layer was discarded. The
acid washing procedure was repeated until the acid layer was colorless. The
organic fraction from the final wash was dried with anhydrous Na2SO.,
7-3
-------
SOg Sample
1.0ml. Baea/Neutral Surrogatea
1.0mL Acid Surrogate*
Sonicate with 30'DmL
SO/SO.MeCI^Hexanee for 30 mln.
Filter thru luchner Funnel with
Qlaaawool Cake and Filter Paper
Extract 3x with 50ml. 0.9 H
N«OH In 1.0L Separatory Funnel
Aqu«ou»
Organic
Adjust to pH2 with 1:1 H.S04,
Extract 3x wHh SOmL MeCI2
Filter with
Add 20ml. Cone. H2SO4:
Shake 4 mln; Alternate
with 20mL dlatllled H20;
Repeat until acid la clear.
Add 10ml. Benzene
Concentrate to 1mL
Finer with Na2S04
To 1mL Benzene add:
Z.OmL lao octane
a.OrnL Acetonltrlle
SOuLPyrldlne
20 uL Acetic Anlydride
I
Add 10mL Hexanea;
Concentrate to ImL
Pre-wet Column
with 20mL Hexanee
Chromatography column with:
1.0g Silica
2.0o 33% NaOH Silica
2.0g Silica
Put In «rfc Hf bath
for 15 mlnutea, Shaking
30 aeeonda every 2 mlnutea.
Bute with 90ml. Hexanea;
Concentrete to 1mL
Add ami. of 0.01 N
,PO.; Shake 2 mlnutea.
Mini-column with
I.Og Alumina
Elute with 20ml. 50/50
MeCI2/Hexanea
Add Ouentltation Standards;
Concentrate to ImL
QC/WS Anaiyalu
FIGURE 7-1. SAMPLE PREPARATION FLOW DIAGRAM FOR SITE SSI-B
PRECURSOR ANALYSIS
7-4
-------
exchanged to hexane and concentrated. Final cleanup of the sample by column
chromatography involved the following procedure.
A glass macro-column, 20 mm o.d. x 230 mm in length, tapered to 6 mm o.d.
on one end was prepared. The column was packed with a plug of silanized glass
wool, followed successively by 1.0 g silica, 2.0 g silica containing 33% (w/w)
1 N NaOH, and 2.0 g silica. The concentrated extract was quantitatively
transferred to the column and eluted with 90 ml hexane. The entire eluate was
collected and concentrated to a volume of 1 ml in a centrifuge tube.
A disposable liquid chromatography mini-column was constructed by cutting
off a 5-mL Pyrex disposable pipette at the 2.0 ml mark and packing the lower
portion of the tube with a small plug of silanized glass wool, followed by 1 g
of Woehlm basic alumina. The alumina-had-been previously activated for at
least 16 hours at 600°C in a muffle furnace and cooled in a desiccator for 30
minutes just before use. The concentrated eluate was quantitatively
transferred onto the liquid chromatography column. The centrifuge tube was
rinsed consecutively with two 0.3-mL portions of a 3 percent MeCl2: hexane
solution, and the rinses were transferred to the liquid chromatography column.
The liquid chromatography column was eluted with 20 ml of a 50 percent
(v/v) MeClg:hexane solution, and the eluate was concentrated to a volume of
approximately 1 ml by heating the tubes in a water bath while passing a stream
of prepurified Ng over the solutions. The quantitation standard was added and
the final volume was adjusted to 1.0 ml prior to GC/MS analysis.
7.2.1.2 Analysis. Analyses of the feed sample extracts for CP, CB and
PCB's present were performed with a Finnigan Model 5100 mass spectrometer
using selected ion monitoring. A fused silica capillary column was used for
chromatographic separation of the compounds of interest. Analytical
conditions for the GC/MS analysis are shown in Table 7-1.
- Tuning of the GC/MS was performed daily as specified in the Tier 4 QA
f*
Project Plan. An internal-standard calibration procedure was used for sample
quantitation. Compounds of interest were calibrated against a fixed ,
concentration of either djg-chrysene (for CB, PCB) or dg-naphthalene (for CP).
Components of the calibration solution are shown in Table 7-2. For
7-5
-------
TABLE 7-1. INSTRUMENT CONDITIONS FOR GC/MS PRECURSOR ANALYSES
Parameter
Chlorobenzenes/
Polychlorinated biphenyls
Chlorophenols
Column
Injector Temperature
Separator Oven Temperature
Column Head Pressure
He flow rate
GC program -
Emission Current
Electron Energy
Injection Mode
Mode
30 m WB DB-5 (1.0 u film
thickness) fused silica
capillary
290°C
290°C
9 psi
1 mL/min
40(4)-290°C,
10°/min & hold
0.50 mA
70 eV
Splitless 0.6 min,
then 10:1 split
Electron ionization, Selected Ion
Monitoring
290°C
290°C
9 psi
1 mL/min
40(1)-290°C,
12°/min & hold
0.50 mA :
70 eV
7-6
-------
TABLE 7-2. COMPONENTS OF THE CALIBRATION SOLUTION
Base/Neutrals
4-chlorobiphenyl
3,3'-di chlorobi phenyl
2,4',5-trichlorobiphenyl
3,3'4,4'-tetrachlorobiphenyl
2,2',6,6'-tetrachlorobiphenyl
2,2,4,5,6-pentachlorobiphenyl
2,2',4,4',5,5'-hexachlorobiphenyl
2,2',3,4,4',5',6-heptachlorobiphenyl
2,2',3,3',4,4',5,5'-octachlorobiphenyl
2,2',3,3',4,4',5,6,6'-nonachlorobiphenyl
decachlorobi phenyl
p-dichlorobenzene
1,2,4-tri chlorobenzene
1,2,3,5-tetrachlorobenzene
pentachlorobenzene
hexachlorobenzene
d^-l,4-dichlorobenzene (SS)
3-bromobiphenyl (SS)
2,2',5,5'-tetrabromobiphenyl (SS)
2,2',4,4',6,6'-hexabromobipheny1 (SS)
octachloronaphthalene (QS)
d^-phenanthrene (QS)
d^-chrysene (QS)
2,5-dichlorophenol
2,3-dichlorophenol
2,6-dichlorophenol
3,5-dichlorophenol
3,4-dichlorophenol
2,3,5-trichlorophenol
2,3,6-trichlorophenol
3,4,5-trichlorophenol
2,4,5-trichlorophenol
2,3,4-trichlorophenol
2,3,5,6-tetrachlorophenol
pentachlorophenol
dg-phenol (SS)
d.-2-chlorophenol (SS)
Cg-pentachlorophenol (SS)
dg-naphthalene (QS)
2,4,6-tribromophenol (QS)
djQ-phenanthrene (QS)
(QS)
1
Surrogate standard.
"Quantitation.standard.
7-7
-------
multi-point calibrations, this solution was injected at concentrations of 10,
50, 100, and 150 ng/ul.
Compound identification was confirmed by comparison of chromatographic
retention times and mass spectra of unknowns with retention times an.d mass
spectra of reference compounds. Since the selected ion monitoring technique
was necessary for the samples analyzed, care was taken to monitor a
sufficiently wide mass region to avoid the potential for reporting false
positives.
The instrument detection limit for the analytes of interest (i.e., CP,
CB, and PCB) was estimated to be approximately 500 pg on column. For a 50 g
sample and 100 percent recovery of the analyte, this corresponds to a feed
sample detection limit of 10 ppb.
7.3 TOTAL CHLORIDE ANALYSIS
Total chloride concentrations in feed samples were determined by Parr
Bomb combustion followed by ion chromatography (1C). A 0.5g sample was placed
in the Parr Bomb with 10 mL of a 50 g/L Na2C03 solution. After combustion of
the samples according to standard procedures (ASTM 2015), the contents of the.
bomb were rinsed into a 100 mL flask and diluted to 100 mL. The resulting
solution was analyzed for chloride concentration (Cl") by 1C using standard
anion conditions. For samples difficult to combust (such as sludges), 25
drops of paraffin oils were added to the bomb prior to combustion.
7-8
-------
8.0 QUALITY ASSURANCE/QUALITY CONTROL (QA/QC)
This section summarizes the results of quality assurance and quality
control (QA/QC) activities for Site SSI-B. The flue gas and ash dioxin/furan
data for this site were generally within the QC specifications presented in
the Tier 4 QAPP. All of the surrogate recoveries for labeled TCDD's were
within the specified limits of 50 to 120 percent. All of the surrogate
recoveries for the labeled hepta- and octa-CDD's were within the specified
limits of 40 to 120 percent. The results of the analysis of the fortified
laboratory QC sample show excellent recoveries with all values well within the
accuracy objective of 60 to 140 percent.
The dioxin/furan precursor analysis of the feed samples was not as
accurate as the dioxin/furan homologue analysis. Surrogate recoveries were
generally below the specified QC limits of + 50 percent. However, despite the
low surrogate recoveries, the dioxin/furan precursor results are considered a
reasonable approximation of the true precursor concentration in the feed
samples.
The following sections summarize the results of all Site SSI-B QA/QC
activities. Manual gas sampling methods are considered in Section 8.1 and
continuous emission monitoring and molecular weight determinations are
considered in Section 8.2. Results of QA audits and laboratory QA/QC
activities are summarized in Sections 8.3 and 8.4, respectively.
8.1 MANUAL GAS SAMPLING
Manual gas sampling methods used at Site SSI-B included Modiffed Method 5
(MM5) and EPA Methods 1 through 4. These methods are discussed in Section
6.0. Quality assurance and quality control (QA/QC) activities for the manual
methods centered around (1) equipment calibration, (2) glassware precleaning,
and (3) procedural QC checks and (4) sample custody procedures. Key
activities and QC results in each of these areas are discussed in this
section. Also discussed are problems encountered that may have affected data
quality.
Pretest calibrations or inspections were conducted on pitot tubes,
sampling nozzles, temperature sensors and analytical balances. Both pre- and
8-1
-------
TABLE 8-1. GLASSWARE PRECLEANING PROCEDURE
NOTE: USE DISPOSAL GLOVES AND ADEQUATE VENTILATION
1. Soak all glassware in hot soapy water (Alconox0) 50°C or higher.
2. H20 rinse (X3)a.
3. Distilled/deionized HgO rinse (X3).
4. ChromergeR"rinse if glass, otherwise skip to 6.
5. High purity liquid chromatography grade H20 rinse (X3).
6. Acetone rinse (X3), (pesticide grade).
7. Hexane rinse (X3), (pesticide grade). :
8. Oven dry (110°C - 2 hours).
9. Cap glassware with clean glass plugs or hexane rinsed aluminum foil
(X3) - three times
8-2
-------
post-test calibrations were also performed on the dry gas meter. All of this
equipment met the calibration criteria specified in the QAPP. The pre- and
post-test dry gas meter calibrations differed by 0.3 percent.
An extensive precleaning procedure was implemented for all sample train
glassware and sample containers. This cleaning procedure, which is outlined
in Table 8-1, was implemented to minimize the potential for sample
contamination with substances that may interfere with the analysis for dioxins
and furans. All sample train glassware was capped with foil prior to use and
stored in a dust free environment. A clean sample trailer was maintained for
train assembly and sample recovery.
Procedural QC activities during manual gas sampling focused on:
- visually inspecting equipment,
- utilization of sample train blanks,
- ensuring the proper location and number of traverse points,
- conducting pre-test, port change, and post-test sample train leak checks,
- maintaining proper temperatures at the filter housing, sorbent trap
and impinger train,
'•- maintaining isokinetic sampling rates, -and
- recording all data on preformatted data sheets.
Results of isokinetic calculations for valid MM5 test runs are shown with
EPA Method 4 results in Table 8-2. As shown in Table 8-2, the average
isokinetic sampling rate for the MM5 and sampling trains achieved the QA
objective of + 10 percent for all three test runs.
Sample custody procedures used during this program emphasized careful
documentation of the sample collected and the use of chain-of-custody records
for samples to be transported. Steps taken to identify and document samples
collected included labelling each sample with a unique alphanumeric code and
logging the sample in a master logbook. All samples shipped to Troika or
returned to Radian were also logged on chain-of-custody records that were
signed by the sampler at shipment and then by the receiving laboratory when
the samples arrived. Each sample container was also sealed with a
chain-of-custody seal so that the container could not be opened without
tearing the seal.
8-3
-------
TABLE 8-2. RESULTS OF ISOKINETIC CALCULATIONS
AND MOISTURE DETERMINATIONS
Run Number
1
3
5
Modified
Isokinetics (%)a
109
106
108
Method 5
Moisture (%)
3.38 '.
4.76
3.01
objective for isokinetics was 100 + 10 percent.
8-4
-------
8.2 CONTINUOUS MONITORING/MOLECULAR WEIGHT DETERMINATION
Flue gas'parameters monitored continuously during the M55 test runs
included CO, C02, 02, total hydrocarbons (THC) and NOX- Concentrations of
C02, 02, and N2 were also determined for integrated bag samples of stack gas.
Quality control results for these analyses are discussed in this section.
Drift check and quality control standard analyses results for the
continuously monitored flue gas parameters are summarized in Table 8-3. The
acceptance criterion for drift checks was an instrument drift within +10
percent. All data reduction was performed assuming a linear drift of
instrument response over the test day. The only calibration drift exceeding
the acceptance criterion was for C02 during Run 3. The instrument showing the
smallest drift was the 02 monitor.
The quality control standards for this program consisted of mid-range
standards that were not used for instrument calibration but were analyzed
immediately after calibration to provide data on day-to-day instrument
variability. The acceptance criterion for each control standard was agreement
with +10 percent of the running mean value. All of the instruments met this
criterion on each test day except for the CO monitor prior to Run 1 and the
NO monitor prior to Run 3. .
J\
Molecular weight was determined by analyzed integrated bag samples of
stack gas for C02, 02, and N2. Quality control for this analysis involved
duplicate analyses of calibration gases immediately before and after sample
analysis. Analysis of the calibration gases was repeated until two
consecutive analyses within +5 percent were obtained. This same criteria of
+5 percent applied to duplicate analyses required for each sample quantitation.
These criteria were met for all molecular weight determinations.
8.3 SYSTEMS AND PERFORMANCE AUDITS
Systems and performance audits of the field testing effort at Site SSI-B
were performed by one of Radian's QA coordinators for Tier 4. Results of the
audits are discussed below.
8.3.1 Systems Audit
The systems audit focused on observing the procedures and techniques used
by the sampling crew, a review of documentation for completeness, and a check
8-5
-------
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8-6
-------
of team adherence to the QC protocol prescribed by the Quality Assurance • -
Project Plan (QAPP). The completed systems audit checklist presented in •
Figure 8-1 shows the results of the systems audit for the MM5 sampling
activities. No significant problems with the MM5 procedures were observed.
An analytical problem with the apparatus used for filtering the scrubber
blowdown was discovered and corrected by the sampling crew during the systems
audit. Some of the solids in the scrubber blowdown samples were not being
removed by the apparatus because the filters were too small. The problem was
solved by obtaining properly sized filters. A potential for incomplete
documentation of testing events was also observed. The sampling task leader
typically made entries into the daily events log on the evening of the test
day with assistance from one other—sampling crew members. Due to the distance
between sampling locations and the size of the sampling effort, it may not
always have been possible for the task leader to record all of the events
that might have affected interpretation of the data. Documentation of the
events could be improved if each member of the sampling crew was required to
keep a current individual events log (pocket size) to be reviewed by the task
leader each evening.
8.3.2 Performance Audit
The performance audit consisted of challenging various components of the
sampling and analytical systems with independent standards. Gas standards
containing components representative of the flue gas were used to audit the
continuous emissions monitoring (CEM) system. The gas standards were obtained
from Scott Environmental; the standards concentrations were certified to
within +1 percent by the vendor. At least one additional standard far each
parameter was obtained from the EPA Repository as a cross check. Audit gases
were delivered through the sample conditioning system used during testing
though not through the heat-traced line between the sample probe and the
*
conditioner. The results of the CEM audit are presented in Table 8-4.
Generally, the audit results showed the CEM instrumentation to be calibrated
well within the specified program accuracy objectives. There were two
exceptions. The Anarad C0/C02 instrument exhibited a great deal of signal
noise and high bias for both channels with the CO channel exceeding the + 2%
accuracy target by a small margin. There was a degree of non-linearity below
8-7
-------
Site: SSI-B
Contract: National Dioxin Study Tier 4
Date: 11/15/84
Auditor: K. Rozacky
Yea No
Comments
Operation
1/R"
fi hrs 0 <;rfm
I ni- Q/n?fiaa
o/in/pa
an p-p Tgp<; t\ _nj
PRESAMPLING PREPARATION
1. Knowledge of process conditions.
2. Calibration of pertinent equipment
prior to each field test (especially
nozzles, dry gas meter, temperature
sensors).
3. Appropriate number and location of
sample traverse points.
4. Filter properly handled during
.. pretreatment and loading.
5. XAD traps properly handled during
pretreatment and loading.
6. Appropriate size nozzle selected
per isokinetic sampling and gas
velocity considerations.
7. Adequate identification procedures
used for filters.
8. Adequate identification procedures
for XAD traps.
9. Date of precleaning for XAD resin.
)10. Date of precleaning for filter
elements. :
11. Sampling train-properly assembled.
12. Adequate facilities, spare parts,
and support equipment available.
Figure 8-1. COMPLETED SYSTEMS AUDIT CHECKLIST
8-8
-------
Yes No
Comments
Operation
<.02 cfm
SAMPLING OPERATIONS
1. Initial leak check performed.
2. Probe maintained at proper
temperature (> 248°F).
3. Filter holder maintained at proper
temperature (248 ± 25°F).
4. Appropriate data recorded during
sampling run.
5. Proper flow rate maintained for
isokinetic samolina at each point
• (within ±10%).
6. Probe placed into and removed from
• stack with care taken to avoid
scraping port and/or duct walls.
7. Sample Grain leak checked at
conclusion of run.
POSTSAMPLING OPERATIONS
1. Sufficient sample volume
collected.
2. Nozzle rinse performed properly
(acetone, hexane x 3)
3. Proper handling procedures observed
in unloading filter holder.
4. Field blanks for filter and XAD
submitted for analysis.
5. Chain-of-custody documentation
completed for each component of
train.
6. Data and pertinent observations
properly recorded.
Figure 8-1. COMPLETED SYSTEMS AUDIT CHECKLIST (continued)
8-9
-------
Yes No Comments
COMPAQ w/MHS SOFTWARE PROGRAM
UNCAPPED
Operation
POSTSAMPLING OPERATIONS (Continued) .
7. Adequate data reduction procedures.
8. Blank train constructed, allowed to
sit for at least 3 hours,
disassembled and submitted for
analysis.
COMMENTS: Moisture determination done as part of MM5 -weight gain in implngers
1, 2. 3 as H,0 + siliga gel weight gain in 4.
Figure 8-1. COMPLETED SYSTEMS AUDIT CHECKLIST (continued)
3-10
-------
Table 8-4. CONTINUOUS EMISSION MONITORING SYSTEM (GEM) AUDIT RESULTS
Parameter
Instrument
Method
THC (as propane)
Beckman 402 FID
CO Anarad AR
400 NDIR
C02 Anarad AR
400 NDIR
QZ Beckman 755
Paramagnetic
NO Thermo
X
Electron Series
10 Chemilumi-
nescence
°2 Shimadzu
GC-3BT FID
C02 Shimadzu
GC-3BT FID
Sample
ID .
1-A
14-Aa
12-A
13-A
1-B
3-A
2-A
4-A
5 -A
6-Aa
1-B
8-A
6-Aa
ll-Aa
U-Aa
9-A
10-Aa
8-A
1-C
18-Ca
17-A
16-A
15-A
8-A
7-A
8-A
7-A
True
Concentrations
(Units)
(ppm)
0.0
9.63
20.50
80.40
(ppm)
0.0
60.5
259.0
1002.0
2491.0
2480.0
0.0.
2.01
7.61
10.50
0.0
4.015
7.99
9.96
(ppm)
0.0
51.7
100.0
225 ;0
705.0
(2)
9.96
15.10
2.01
5.10
Measured Relative Accuracy
Concentration ' Error Target
(Units) (2) (%)
(ppm)
1.11
9.84
19.50
75.16
(ppm)
-0.8
115.4
325.9
1239.5
2933.8
3048.4
0.45
2.16
8.99
12.01
—0.05
4.23
8.40
10.34
(ppm)
1.3
62.6
121.5
279.5
795.9
(2)
10.11
15.18
2.05
5.01
2.2
-4.9
-6.5
-
90.7
25.8
23.7
17.8
22.9
7.5
18.1
14.4
5.3
5.1
3.8
21.1
21.5
24.2
12.9
1.5
0.6
2.0
-1.7 '
±25
±20
±20
±20
±20
±20
±20
EPA supplied gas standard
8-11
-------
70 ppm CO; however, the majority of actual testing data was above 1000 ppm.
Also, the Thermo Electron NOX instrument also showed a high response bias
exceeding the ± 20% .accuracy target for this parameter. Both instruments did
have linear response across the scale.
The Mettler PE 360 loading analytical balance was audited using a
standard set of Class S weights. Accuracy was satisfactory. Results of the
audit are presented in Table 8-5.
The dry gas meter (DGM) in console RAC #5, used to measure volumetric
flow for the Modified Method 5 sample train, was audited by direct comparison
to a transfer DGM which had been referenced to an independent wet test meter.
A flow rate of approximately 0.4 cfm was used as a reference. Agreement ,
between the two DGM's was within + 2.7% based on three 15-minute runs :
exhibiting a coefficient of variation less than 1.3%. As part of the
performance audit, a set of sample data was submitted to the sampling team for
determination of velocity and volumetric flow rates, moisture content, and gas
molecular weight. All requested calculations were accurately performed.
In summary, the performance audit showed that the accuracy targets were
met except where noted and that those cases were not extreme. The systems
audit found the sampling team competent and knowledgeable in their tasks,
documentation complete and current, chain-of-custody procedures satisfactory,
and the prescribed QC protocol meeting the program objectives.
8.4 LABORATORY ANALYSES
QA/QC data collected for the various laboratory analyses performed on
Site SSI-B samples are discussed in this section.- Dioxin/furan QC data are
discussed in Section 8.3.1, precursor QC data are discussed in Section 8.3.2,
and total chloride data are summarized in Section 8.3.3.
8.4.1 Dioxin/Furan QC Data
Surrogate recoveries for dioxin/furan analyses performed on Site SSI-B
samples are presented in Table 8-6. All of the surrogate recoveries are
within the target ranges of 50 to 120 percent for the labeled TCDD's and 40 to
120 percent for the labeled.hepta and octa-CDD's.
Results for dioxin/furan blank samples and a QC (fortified spiked) sample
are summarized in Table 8-7. Again, surrogate recoveries were all within the
8-12
-------
TABLE 8-5. METTLER 360 (S/N C99712) BALANCE AUDIT RESULTS
Audit
Weight
(grams)
0.00
0.05
0.50
1.00
5.00
10.00
20.00
50.00
100.00
150.00
200.00
455.10
Measured
Weight
(grams)
0.00
0.05
0.50
1.00
5.00
9.99
19.99
49.97
99.87
149.82
199.78
454.80
Absolute
Error
(grams)
--
0,00
0.00
0.00
0.00
-0.01
-0.01
-0.03
-0.13
-0.18
-0.22
-0.30
Range of Error (g) -0.30 to 0.00, 95% Confidence Interval (g) -0.15 to
-0.007
8-13
-------
TABLE 8-6. SUMMARY OF SURROGATE RECOVERIES FOR DIOXIN/FURAN
ANALYSES ON SITE SSI-B SAMPLES '
Surroaate Recoveries ( percent)
Compound
37C14-TCDD
13C12-TCDD
37Cl4-Hepta-CDD
13r
c!2-Octa-CDD
Spiked3
Quantity
(ng)
5
5
20
20
Run 1
MM5
78
106
48
99
Run
MM5
92
94
!>2
79
Run 5b
MM5
(aqueous)
106
NS
53
NS
Run 5b
MM5;
(XAD resin)
NSC
102
NS
781
aAmount of compound spiked into each sample prior to extraction and analysis.
bThe aqueous and XAD resin portions of this sample were analyzed separately.
c,
'Compound not spiked into this sample.
8-14
-------
TABLE 8-7. SUMMARY OF RESULTS FOR DIOXIN/FURAN BLANK
SAMPLES AND FORTIFIED QC SAMPLES
Compound
37Cl4-TCDDa
13C12-TCDDa
37C14 Hepta-CDDb
13C12 Octa-CDDb
Field
Blank
92
102
58
99
Surrogate Recoveries,
Laboratory
Blank
98
94
78
84
Percent
Fortified
QC Sample
92
92
63
82
Amount detected, ng (Amount spiked on fortified sample, ng)
Dioxins
2378 TCDD
Other TCDD
Penta CDD
Hexa CDD
Hepta CDD
Octa CDD
Furans
2378 TCDF
Other TCDF
Penta CDF
Hexa CDF
Hepta CDF
Octa CDF
NDC
ND
ND
ND
0.3
1.0
ND
ND
ND
ND
0.1
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
0.2 (0.4)
ND (0)
ND (0)
1.1 (1.6)
2,0 (2.4)
2.4 (3.2)
0.3 (0.4)
ND (0)
0.5'(0.8)
1.0 (1.6)
1.8 (2.4)
2.4 (3.2)'
Spiked at 5 ng in each sample.
DSpiked at 20 ng in each sample.-
"ND = not detected. Detection limit ranged from 0.01 to 0.19 ng.
8-15
-------
target ranges. The field blank and the laboratory blank were found to be
clean with the exception of i.O ng of octa-CDD, 0.3 ng of Jiepta-CDD and 0.1 ng
of hepta-CDF in the field blank. Comparison of measured and spiked quantities
for the QC sample shows excellent recoveries for the unlabeled PCDD and PCDF,
with all values well within the accuracy objective of 60 to 140 percent for
this sample.
8.4.2 Precursor QC Data
Surrogate recovery efficiencies for six labeled compounds spiked into
sludge feed samples are presented in Table 8-8. The recoveries vary \
considerably depending on the particular surrogate. Recoveries for the sludge
feed samples ranged from 0 to 169 percent. With the exception of bromobiphenyl
in the Run 1 sample, the surrogate recoveries were frequently below the 50
percent objective stated in the Tier 4 QA Project Plan and were below those
generally considered achievable when analyzing for similar compounds in water
or from MM5 train components. There are no directly comparable surrogate !
recovery values reported in the literature for samples similar to those
analyzed for Site SSI-B. The cause of the high recovery for bromobiphenyl in
the Run 1 sludge sample is unknown.
There are several reasons for the comparatively low precursor surrogate
recoveries reported in the Tier 4 study for samples such as Site SSI-B feed
samples. First, the complex nature of the samples required extensive clean-up
procedures prior to GC/MS analysis, which increased the potential for losses
of the surrogate compounds (and analytes) during sample preparation. Second,
large sample sizes (25 to 50 g) were required to increase method sensitivity
for the target analytes and to ensure that representative portions of the
samples were analyzed. Due to the high cost of labeled surrogates, it was not
desirable to spike the large sample sizes with surrogates in proportion to
that normally used for smaller samples. Supplemental in-house laboratory
studies showed that when sample size was restricted to 1 g and the amount of
surrogate spiked was held fixed, surrogate recoveries improved considerably.
Surrogate recoveries for Tier 4 samples and the results for small sample sizes
are further discussed in the Tier 4 Engineering Analysis Report.
In spite of the relatively low surrogate recovery values for some of the
feed samples, the resulting analytical sensitivity for the target analytes was
8-16
-------
TABLE 8-8. SUMMARY OF SURROGATE RECOVERIES FOR DIOXIN PRECURSOR ANALYSES
Precursor Surroqate Recoveries foercent)3
Compound
d^-Di chl orobenzene
Bromobiphenyl
Tetrabromobi nhen vl
dg - Phenol
d, - Chlorophenol
Cg - Pentachlorophenol
Sludge Feed
Run 1
72
169
-- - . - 118
10
13
3
Sludge Feed
Run 3
39
110
78
10
9
5
Sludge Feed
Run 5
44
98
85
8
10
ND
Surrogates spiked at 200 ng each in 50 g sample.
ND = not detected.
8-17
-------
considered acceptable for the purpose of this study. The instrumental
detection limit ranged from about 100 to 500 picograms on-column for the T
microliter of final extract injected into the GC/MS. At a method recovery'
efficiency of 100 percent for a 50 gram solid sample cleaned up to a final
extract volume of 1 milliliter, the overall analytical sensitivity would be
approximately 2 to 10 ppb in the solid sample. For sludge samples with
surrogate recoveries as low as 3 percent, the overall analytical sensitivity
of the method would still be 600 to 3000 ppb, or 0.6 to 3.0 ppm. Thus, even
in a worst-case situation the analytical procedures used provide information
on the precursor content of the feed samples down to the ppm level.
A single matrix spike was analyzed for the Site SSI-B feed samples. This
sample showed_0_tfl. 39 percent recovery for spiked chlorobenzenes and 19 to 111
percent for spiked chlorinated biphenyls and 2 to 14 percent for spiked
chlorophenols. Results of laboratory blanks for the precursor analyses all
showed no detectable levels of the target compounds.
8.4.3 Total Chlorine PC Data
Total chloride analyses were performed by Research Triangle Institute on
three composite feed samples. Blank analysis values obtained for the Parr
bomb combustion/ion chromatography technique were 36, 0, 56, and 18 ppm
chloride. Data presented in Section 5 are blank corrected. A LECO coal
sample containing 2600 ppm chloride was analyzed as a daily QC standard.
Reported values were 2500, 2500, 2500, and 2400 ppm.
8-18
-------
9.0 REFERENCES
1. Radian Corporation. National Dioxin Study Tier 4 - Combustion Sources,
Draft Final Report prepared for U.S. Environmental Protection Agency,
Research Triangle Park, N.C. EPA 450/4-84-014e, April 1985.
9-1
-------
-------
APPENDIX A
FIELD RESULTS
-------
-------
APPENDIX A-l
MODIFIED METHOD 5 AND EPA METHODS 1-4 FIELD RESULTS
A-l
-------
-------
R
E
(
PLANT
PLANT
SAMPL
TEST
DATE
TEST
A 0
P A
R A
SI
ING
#
PER
I A N
M E
W D
TE
LOCAT
IOD
T
A
ON
S
H
T
C
C
/
) U R C E
) D 2-5
V )
DIOX1N SI
UNIT
03-MM5-01
1 1/15/84
0946-1358
TEST
TE #03
EXHAUST
(0946-1 1
46
/ 1158-1358)
PARAMETER
VALUE
Sampling time (min.) 240
Barometric Pressure (In.Hg) 29.18
Sampling nozzle diameter (in.) .12
Meter Volume (cu.ft.) 90.001
Meter Pressure (fn.H20) .445
Meter Temperature (F) 42.26
Stack dimension (sq.in.) 671.9588
Stack Static Pressure (in.H20) -.9
Stack Moisture Collected (gm) 68.1
Absolute stack pressureUn Hg) 29.11382
Average stack temperature (F) 169.4894
Percent C02 4.66
Percent 02 17.85
Percent N2 77.49
Delps Subroutine result 38.20479
DGM Factor " .9945
Pitot Constant .84
A-3
-------
R
E
F
PLANT
PLANT
SAMPL
TEST
DATE
TEST
A D
P A
1 N
SI
ING
#
PER
1 A N
• M E
A L
TE-
LOCAT
IOD
T
R
ON
S (
H (
E «
) U R C E
) D S 2 -
3 U L T S
D I OX 1 N SI
UNIT
03-MM5-01
11/15/84
0946-1358
TEST
5
TE #03
EXHAUST
(0946-11
46
/ 1158-1358)
PARAMETER
RESULT
VmCdscf)
Vm(dscm)
Vw gas(scf)
Vw gas (scm)
% moisture
Md
MWd
MW
Vs(fpm)
Vs (mpm).
FIow(acfm)
Flow(acmm)
FIow(dscfm)
Flow(dscmm)
% I
% EA
91.86876
2.601723
3.210915
9.093311E-02
3.377078
,,9662292
29.4596
29.0726
5658.119
1725.036
26402.94
747.7312
20821.67
589.6698
109.2916
684.6008
Program Revision:1/16/84
A-4
-------
RADIAN SOURCE TEST
EPA METHOD 2-5
(RAW DATA)
PLANT ,
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
DI OX IN SITE #03
UNIT ' EXHAUST
03-MM5-03
11/17/84
10-1556 (0940-1235 / 1237-1242 / 1256-1556)
PARAMETER
VALUE
Sampling time (mln.) 360
Barometric Pressure (In.Hg) 29.48
Sampling nozzle diameter (In.) .12
Meter Volume (cu.ft.) 142.921
Meter Pressure (In.H20) .501
Meter -Termfrerature (F) 64.53
Stack dimension (sq.In.) 671.9588
Stack Static Pressure (ln.H20) -.9
Stack Moisture Collected (gm) 149.5
Absolute stack pressureUn Hg) 29.41382
Average stack temperature (F) 169.4861
Percent C02 4.98
Percent 02 . 15.62
Percent N2 . 79.4
Delps Subroutine result 40.53412
DGM Factor .9945
PItot Constant .84
A-5
-------
IAN S 0 U R C
RESULTS
RAD
EPA METHODS
FINAL
PLANT
PLANT SITE
SAMPLING LOCATION
TEST &
DATE
TEST PERIOD
E
2 -
TEST
5
DIOXIN SITE '#03
UNIT EXHAUST
03-MM5-03
11/17/84
0940-1556 (0940-1235 / 1237-1242 / 1256-1556)
PARAMETER
RESULT
Vm(dscf)
Vm(dscm)
Vw gas(scf)
Vw gas (scm)
% moisture
Md
MWd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flow(acmm)
Flow(dscfm)
Flow(dscmm)
% I
% EA
141 .1473
3.997292
7.048925
,,1996256
4.75648
,,9524351
29.4216
28.87833
5992.457
1826.969
27963.09
791 .9146
21961 .31
621.9441
106.1348
292.4218
Program Rev Ision:1/16/84
A-6
-------
R
E
(
PLANT
PLANT
SAMPL
TEST
DATE
TEST
A D
P A
R A
SI
ING
f
PER
1 A N
M E
W D
TE
LOCAT
IOD
T
A
ON
S C
K C
T /
) U R C E
) D 2-5
\ )
DIOXI N SI
UNIT
03-MM5-05
11/19/84
0845-1503
TEST
TE #03
EXHAUST
(0845-1 1
45
/ 1203-1503)
PARAMETER
VALUE
Samp I Ing
Barometr
Samp I Ing
Meter Vo
Meter
Meter
Stack
Stack
Stack
t ime (mIn.)
ic Pressure (in.Hg)
nozzle diameter (in.)
ume (cu.ft.)
Pressure (fn.H20)
Temperature (F)
d imens f on (sq . i n .)
Static Pressure (In.H20)
Moisture Collected (gm)
Absolute stack pressure(in Hg)
Average stack temperature (F)
Percent C02
Percent 02
Percent N2
Delps Subroutine result
DGM Factor
P.itot Constant
360
29.72
.12
120.726
.36
52.93
671.9588
-.9
80.9
29.65382
173.1528
4.89
15.69
79.4
34.33359
.9945
.84
A-7
-------
R A D I
EPA
F I N A
PLANT -
PLANT SITE
SAMPLING L
TEST #
DATE
TEST PERIOD
AN S C
M E T H C
L R E <
CATION
)URCE TEST
) D S 2-5
3 U L T S
DIOXIN SITE #03
UNIT EXHAUST
03-MM5-05
11/19/84
0845-1503 (0845-1
145
/ 1203-1503)
PARAMETER
Vm(dscf)
Vm(dscm)
Vw gas(scf)
Vw gas (scm)
% moisture
Md
MWd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Fl.ow(acmm-) •
Flow(dscfm)
Flow(dscmm)
% I
% EA
RESULT
122.8727
3.479754
3.814435
.1080248
3.010911
.9698909
29.4044
29.06102
5039.289
1536.369
23515.24
665.9516
18850.24
533.8387
107.642
2.97.6326
Program Rev Ision:1/16/84
A-8
-------
APPENDIX A-2
CONTINUOUS EMISSION MONITORING RESULTS
A-9
-------
-------
CEM RESULTS - SITE 03 - TEST 1
TIME
1005
1010
1015
1020
1025
1030
1035
1040
1045
1050
1055
1100
1105
1110
1115
1120
1125
1130
1135
1140
1145
1200
1205
1210
1215
1220
1225
1230
1235
1240
1245
1250
1255
1300
1305
1310
1315
1320
1325
1330
1335
1340
1345
1350
1355
NO. PTS.
MEAN-
STD. DEV,
02
(35V)
= ====
13.3
13.5
13.5
13.6
13.8
13.9
13.9
14.1
14.4
15.2
15.6
15.1
15.1
14.5
15.0
14.8
14.7
14.7
14.6
14.4
14.6
14.3
14.3
14.4
14.4
14.5
14.6
14.4
14.4
14.4
14.6
14.5
14.9
14.7
14.9
14.7
14.7
14.4
14.5
14.5
14.2
14.8
14.3
14.7
14.8
' = = = = = =
45
14.5
0.5
CO
(PPMV)
=======
5561.5
5203.4
5585.0
5594.4
5640.8
6176.5
6490.1
6610.9
7039.4
6798.1
6002.3
5744.4
5483.8
5346.8
5722. 5
6071.2
5618.7
6378.3
6607.8
6419.7
6219.9
6497.1
6673.4
' 7059.4
7022.6
7153.0
7358.8
6699.4
6816.7
6502.2
7126.9
6258.8
7987.7
7061.9
6443.6
7123.7
6377.7
5649.6
6226.6
5994.6
5272.4
6638.8
5692.0
6727.4
6487.6
=========
45
6337.0
627.3
C02
(*V)
ESSS
18.9
23.5
21.7
22.6
21.8
20.2
22.8
22.9
23.2
20.9
21.0
17.8
17.5
21.9
23.2
20.6
18.7
17.9
22.2
19.7
22.0
21.0
21.3
20.4
21.8
20.9
20.5
19.1
17.4
22.3
21.7
19.4
19.5
18.9
20.7
17.5
20.5
19.8
18.3
21.0
16.9
19.7
16.3
18.6
18.5
= = = = =
45
20.3
1.9
NO-X
(PPMV)
=======
^
799.3
803.0
825.1
828.9
825.0
810.2
786.9
727.2
726.8
641.8
763.2
750.4
743.8
727.6
757.4
712.0
766.1
853.0
804.1
855.3
848.7
836.0
843.5
845.0
858.3
829.1
890.4
849.2
889.9
861.5
890.3
831.9
848.0
775.9
795.9
787.4
767.2
807.2
770.4
834.5
807.9
S3SS3SSSSSS2
41
804.3
53.2
THC
(PPMV)
= = = = = s'=
5.8
8.2
6.3
5.9
5.2
5.7
5.5
5.8
5.3
10.5
20.4
19.9
19.5
17.5
18.7
20.2
20.4
17.5
16.9
18.1
18.6
SSS3SSSS
2]
12.?
6.t
A-ll
-------
GEM RESULTS - SITE 03 - 'TEST 3
TIME
945
950
955
1000
1005
1010
1015
1020
1025
1030
1035
1040
1045
1050
1055
1100
1105
1110
1115
1120
1125
1130
1135
1140
1145
1150
1155
1200
1205
1210
1215
1220
1225
1230
1235
1240
1300
1305
13 1C
1315
1320
1325
1330
1335
1340
1345
1350
1355
1400
1405
02
CSV)
ss==
11.2
11.3
11.3
11.2
11.3
11.3
11.4
10.9
10.8
11.4
11.2
11.6
12.1
12.4
11.9
12.3
11.8
11.8
11.7
11.8
12.4
11.6
12.4
11.7
12.3
12.5
11.6
12.9
12.2
11.4
11.9
11.8
11.8
11.7
12.0
11.7
11.6
12.0
11.7
11.7
11.9
11.9
11.7
11.8
11.8
11.9
11.6
11.6
11.5
11.3
CO
(PPKV)
ss s s ss = s
1213.2
1960.8
1547.9
1226.0
1788.0
1350.5
1248.7
1375.4
1225.7
1498.6
1400.2
1380.5
1672.3
1744.1
1746.2
1849.5
1381.7
1524.1
1374.0
1490.6
2247.7
1495.6
2230.3
1411.7
1618.9
2598.9
1483.9
2962.3
1708.9
1641.4
2105.8
1951.4
1846.5
2408.1
2045.1
2014.4
2081.8
2366.2
2573.3
2661.1
2295.8
2508.1
2358.8
2824.9
2258.2
2504.1
1904.1
1952.9
2223.5
2777.6
C02
(55V)
19.2
19.6
19.7
18.6
16.2
18.8
15.5
17.2
14.4
16.7
14.5
14.9
21.1
17.2
18.3
22.1
17.4
15.6
17.7
18.9
16.0
15.3
18.4
17.2
18.1
18.1
15.9
17.7
18
NOX
(PPMV)
677.8
.2
.3
5
17.4
16.5
17.9
18.2
14.5
17.5
16.0
16.8
18,
15,
16.0
16.9
17.1
19.9
20.5
15.2
18.4
14.6
15.7
17.0
17.4
,1
,2
.7
.1
768
695
691.9
784.8
787.2
737
705
708.9
786.0
815.2
739.9
810.0
955.9
806.6
783.1
740.6
808.5
777»4
673.4
930.9
712.3
804.1
857.3
651.5
935.7
740.0
749.9
724.5
725.6
890.2
631.9
792.8
846.6
780.7
748.1
738.7
750.7
767.7
800.0
681.2
725
700,
750.0
713.7
745.2
708.5
728.7
705.8
767.7
.0
.3
THC
(PPMV)
18.9
10.8
8.6
7.7
7.5
7.2
7.1
6.7
6.6
7.0
9.4
8.7
8.0
7.9
7.5
8.0
9.8
6.8
5.9
6.3
7.0
5.8
6.9
6.4
5.9
7.2
6.4
7.8
7.5
6.0
7.6
-5.0
5.9
6.1
6.4
6.0
5.3
5.7
5.7
5.8
5.6
6.6
5.5
5.3
5.4
9.6
5.3
5.0
5.3
5.1
A-12
-------
GEM RESULTS - SITE 03 - TEST 3
TIME
02
CO
(PPKV)
C02
NOX
(PPMV)
THC
(PPMV)
=======
======= ===:
141C
1415
1420
1425
1430
1435
1440
1445
1450
1455
1500
1505
1510
1515
1520
1525
1530
1535
1540
1545
1550
1555
11.7
11.7
11.4
11.1
11.2
11.6
11.4
11.5
11.7
11.8
11.4
11.7
11.5
11.4
11.8
11.3
11.6
11.4
11.3
11.9
11.4 •
11.7
1982.6
2123.5
2089.6
1203.9
1444.0
1259.9
1292.4
1116.5
1342.5
18S1.5
878.6
1484.2
1662.1
1234.3
1191.5
1078.6
1334.4
1114.7
1062.0
1076.0
793.7
1897.5
17.5
16.9
15.6
17.6
22
17
18
21
18
20.4
17.9
19.1
19.1
18.6
19.4
16.4
16.6
16.4
20.9
21.5
20.7
16.0
673
687
726,
635
687.4
823.1
770.4
694.6
790.6
906.4
747.2
722.9
830.8
737.1
774.2
755.8
899,
740,
740,
900.0
691.0
822.5
,5
,2
.2
5.4
4.8
10.8
4.7
4.6
3.8
5.8
5.7
5.7
5.1
5.3
4.1
5.0
4.3
5.2
4.2
6.6
3.5
3.9
4.3
4.3
3.3
NO. PTS.
MEAN
STD. DEV
72
11.7
0.4
7-2
1744.6
507.4
72
17.7
1.9
72
761.3
70.3
72
6.4
2.2
A-13
-------
GEM RESULTS - SITE 03 - TEST 5
TIME
845.00
850.00
855.00
900.00
905.00
910.00
915.00
920.00
925.00
930.00
935.00
940.00
945.00
950.00
955.00
1000.00
1005.00
1010.00
1015.00
1020.00
1025.00
1030.00
1035.00
1040.00
1045.00
1050.00
1055.00
1100.00
1105.00
1110.00
1115.00
1120.00
1125.00
1130.00
1135.00
1140.00
1145.00
1205.00
1210.00
1215.00
1-220.00
1225.00
1230.00
1235.00
C2
CSV)
3 SS =
18.0
18.2
18.3
18.2
18.3
18.2
18.4
18.5
18.3
18.5
18.2
18.4
18.5
18.3
18.5
18.3
18.2
18.3
18.5
18.3
18.4
18.3
18.5
18.5
18.4
18.3
18.4
18.5-
18.5
18.4
18.7
18.5
18.5
18.8
18.4
18.7
18.5
18.3
18.6
18.4
18.5
18.4
18.5
18.4
CO
(PPMV)
=======
6028.9
6540.4
6057.2
6507.9
6192.8
5191.9
6004.8
6652.2
5646.1
6751.3
5074.3
3601.4
5089.8
5534.6
5742.8
5510.6
5912.9
5801.0
7301.2
6313.1
5995.5
5971.2
. 6742.4
6762.0
5658.4
6499.6
5922.4
7660.4
8651.2
5145.3
6234.6
6278.3
6469.0
5224.0
6702.0
5424.1
4702.9
6950.2
6691.1
7486.4
8124.2
5877.9
7517.0
4599.2
C02
(SV)
19.1
17.4
22.1
16.7
29.8
22.2
16.
20,
13,
13.9
23.3
14.3
14.7
17.9
25,
18,
NOX
(PPNW)
THC
(PPKV)
,1
.1
.3
,5
.1
22.5
20.5
24.4
17.9
20.0
17
16,
22.2
20.2
20,
25
.2
,5
,3
.7
21.6
17.7
20.4
20.0
16.5
17.4
20.7
20.9
20.1
16.9
15.8
14.8
13.7
18.6
11.1
20.3
15.9
623.9
862.8
866.4
713.7
959.9
723.1
745.3
812.9
782.0
797.9
797.5
820.1
829.6
830.0
805.5
955.2
,2
.3
.1
706
822
781
703.4
851.4
714.0
845.2
833.4
844.2
839.9
904.4
764.0
927.1
779.6
954
894
845
892
869.6
801.1
908.8
737.5
727.7
840.3
733.9
692
839
.7
,1
727.9
18.35
18.53
19.65
22.83
17.79
16.37
21.25
15.97
21.26
27.62
23.45
21.82
20.32
21.53
29.24
29.45
34.93
3 2'. 04
59.60
33.02
38.02
45.10
46.51
42.36
41.89
45.97
44.12
35.81
23.22
39.92
40.28
45.22
39.98
52.52
61.40
68.51
68.64
74.16
A-14
-------
GEM RESULTS - SITE 03 - TEST 5
TIME
=======
1240.00
1245.00
1250.00
1255.00
1300.00
1305.00
1310.00
1315.00
1320.00
1325.00
"1330.00"
1335.00
1340.00
1345.00
1350.00
1355.00
1400.00
1405.00
141C.OO
1415.00
1420.00
1425.00
1430.00
1435.00
1440.00
1445.00
1450.00
1455.00
1500.00
NO. PTS.
MEAN
STD. DEV.
02
( S V )
=======
18.4
18.5
16.5
18.6
18.3
18.5
lfi.8
18.3
18.4
18-. 4
18.7
18.6
18.4
18.3
18.3
.18.2
18.2
18.3
18.2
18.5
17.8
18.4
18.4
18.3
18.2
18.3
18.6
18.3
18.2
5========
73
18.4
0.2
CO
(PPMV)
=======
7540.3
6639.6
641C.9
5295.6
5111.2
6727.2
6904.5
5913.0
6268.4
4915,7
7584.4
5491.1
5113.5
6520.5
6609.1
5348.0
4912.8
5797.2
6374.7
6299.2
3252.6
6983.6
4959.1
2069.0
4668.1
4560.9
5844.3
3575.9
5691.7
73
5946.9
1095.6
C02
(SV)
18.5
17.5
22.8
16.5
11.0
12.4
22.8
13.8
23.9
12.3
24.9
14.2
28.0
14.1
24.1
11.1
28.0
14.0
14.0
21.5
14.4
24.6
15.3
34.2
14.6
15.7
19.3
11.9
16.2
s is 'st = sz =:
73
18.7
4.7
MOX
(PPMV)
• — — • — — gg
821.6
715.8
829.9
751.0
698.9
767.6
671.1
795.6
784.5
823.7
857.4
817.0
774.7
734.8
769.9
605.0
793.9
755.4
.793.6
774.9
746.0
786.1
762.6
766.2
700.8
830.6
891.0
822.1
733.8
=========:
73
798.9
71.3
THC
(PPMV)
80.15
62.12
72.34
74.16
64.16
87.21
59. 85
60.72
56.93
60.05
64.38
60.42
56.01
46.52
47.44
46.11
54.30
58.14
62.18
52.18
60.55
======
59
48.82
18.73
A-15
-------
-------
APPENDIX A-3
EPA METHOD 3 FIXED GAS RESULTS
A-17
-------
-------
FIXED GAS ANALYSIS RESULTS FOR SSI-Be
Run Sample,
Number Number
1 le
2
average
3 1
2
5 1
2
.
Fixed Gas Concentrations'1
°2
19.2
17.9
17.9
15.1
16.1
15.6
15.5
15.9
15.7
co2
3.42
4.66
4.66
5.43
4.52
4.98
4.88
4.90
4.89
N2
82.2
84.7
84.7
80.5
77.7
79.1
80.2
82.7
81.4
Total
Percentages"
104 .8
106.1
106.1
101.0
98.3
99.7
100.6
103.5
102.1
Analysis by gas chromatograph/thermal conductivity detector.
Represents Tedlar bags of stack gas collected according-to EPA Method 3.
Concentrations presented represent average values from duplicate sample
analysis.
Sum of fixed gas concentrations. Difference from 100 percent are due to
analytical error.
Q
Leak suspected in bag sampling system for first bag.
First bag sample not included in average.
A-19
-------
-------
APPENDIX A-4
MODIFIED METHOD 5 AND EPA METHODS 1-4 SAMPLE CALCULATIONS
A-21
-------
-------
RADIAN SOURCE TEST
EPA METHOD 2-5
SAMPLE CALCULATION
• PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
DIOXIM SITE #03
UNIT EXHAUST
03-MM5-01
11/15/84
0946-1358 (0946-1146 / 1158-1358)
) Volume of dry gas sampled at standard conditions (68 deg-F ,29.92 in. Hg)
Y x Vm x CT(std) + 460] x TPb -KPm/13.6)]
P(std) x (Tm + 460)
Vm(std) =
.9945 x 90.001 x 528 x C 29.18 + ( .445 /13 .6) ]
Vm(std) =
29.92 x ( 42.26 + 460)
Vm(std) = 91.869dscf
Volume of water vapor at standard conditions:
Vw(gas) = 0.04715 cf/gm x W(l) gm •
Vw(gas) = 0.04715 x 68.1 = 3.211, scf
3) Percent Moisture in stack gas :
100 x Vw(gas)
Vm(std) " + Vw(gas)
100 x 3.211
= 3.38 55
91.869 +3.211
4) I'.ole fraction of dry stack gas :
100 - 3M * 100 - 3.38
100 100
3 M =
Md =
.9662292
A-23
-------
SAMPLE CALCULATION
PAGE TWO
5)Average Molecular Weight of DRY stack gas :
MWd - (.44 x SC02) + (.32 x !?02) + (.28 x ?N2)
MWd = (.44 x 4.66 ) + (.32 x 17.85 ) + (.28 x 77.49 ) = 29.4595
6)Average Molecular Weight of wet stack gas s
KW s KWd x Md + 18(1 - Md)
MW = 29.4596 x .9662292 + 18(1 - .3.662292 ) = 29.0726
7) Stack gas velocity in feet-per-rainute (fprn) at stack conditions :
Vs - KpxCp x CSQRT (dP)]§avet x SORT [Ts Savgt] x SORT [1 / (PsxMV.') ] x;60sec/mi
Vs s 85.49 x .34 x 60 x 38.20479 x SQRT[1/( 29.11382 X 29.0726 )]
V.s « 5653.1 19 FPM . ;
8) Average stack gas dry volumetric flow rate (DSCFM) :
Vs x As x Md x T(std) x Ps
144 cu. in./cu.ft. x (Ts +460) x P(std)
5658.119 x 671.9588 x .9662292 x528x 29.11382
144 x 629.4894 x 29.92
Qsd - 20321.67 dscfm
Osd
Osd
A-24
-------
SAMPLE CALCUL-ATION
PAGE THREE
3)lsokinetic sampling rate (?5) :
Dimensional Constant C = K4 x 60 x 144 x P / (Pi /4)]
K4 = .0945 FOR ENGLISH UNITS
<* =
C x Vm(std) x (Ts + 460)
Vs x Tt x Ps x Md x (Dn)e2
1039.574 x 91.86876 x 629.4894
5658.-119 x 240 x 29.11382 x .9662292 x( .12 )°2
109.2916
10) Excess a i r (%) :
100 x 302 100 x 17.85
P/> _ »•••«,«,«,«,••«.••«.-, = — — — — — — — ___ _ _ _ — —
(.264 x SN2) - 302 (.264 x 77.49 ) - 17.85
EA = 684.60
11) Participate Concentration :
Cs = ( grams part.) / Vm(.std) = 0 / 91.86876
Cs =
0.0000000 Grams/DSCF
T(std) x Md x Ps x Cs
P(std) x Ts
528 x .9662292 x 29.11382 x 0.0000000
29.92 x 629_.4394
0.0000000 Grarns/ACF
LBS/HR = Cs x 0.002205 x Os d x 60
LBS/HR = O.OOOOOOOx 0.002205 x 20821.7 x 60
LBS/HR = 0
Ca =
Ca =
Ca =
Program Revision:1/15/34
A-25
-------
PARAMETER
RADIAN SOURCE TEST
EPA METHODS 2-5
DEFINITION OF TERMS
DEFINITION
Tt(min.)
Dn( in.)
Ps(in.H20)
Vm(cu.ft.)
Vw(gm.)
Pm(In.H20)
Tm(F)
Pb( In.Hg.)
% C02
? 02
f5 N2
SQR(DELPS)
As(sq.in.)
Ts(F)
Vm(dscf)
Vm(dscm)
Vw gas(scf)
" moisture
Fid
MW d
f!W
Vs(fpm)
FIow(actm)
FIow(acnm)
FIow(dscfm)
F I ow(dscnjrc)
;$ I
1 EA
DGM
Y
Cp
dH
dP
*** EPA
STANDARD
CONDITIONS
TOTAL SAMPLING TIME
SAMPLING NOZZLE DIAMETER
ABSOLUTE STACK STATIC GAS PRESSURE
ABSOLUTE VOLUME OF GAS SAMPLE MEASURED BY DGM
TOTAL STACK MOISTURE COLLECTED
AVERAGE STATIC PRESSURE OF DGM
AVERAGE TEMPERATURE OF DGM
BAROMETRIC PRESSURE.
CARBON DIOXIDE CONTENT OF STACK GAS
OXYGEN CONTENT OF STACK GAS
NITROGEN CONTENT OF STACK GAS .
AVE. SQ. ROOT OF S-PITOT DIFF. PRESSURE-TEMP. PRODUCT!
CROSS-SECTIONAL AREA OF STACK(DUCT)
TEMPERATURE OF STACK
STANDARD VOLUME OF GAS SAMPLED ,Vm(std),AS DRY STD.
STANDARD VOLUME OF GAS SAMPLED,Vm(std),AS DRY STD. CM
VOLUME "OF WATER VAPOR IN GAS SAMPLE,STD
WATER VAPOR COMPOSITION OF STACK GAS
PROPORTION, BY VOLUME,OF DRY GAS IN GAS SAMPLE
MOLECULAR WEIGHT OF STACK GAS,DRY BASIS LG/LB-MOLE
MOLECULAR WEIGHT OF 'STACK GAS, WET BASIC LB/LB-MOLE
AVERAGE STACK GAS VELOCITY .
FLOW RATE(ACTUAL STACK COND.)
FLOW RATECACTUAL STACK COND.)
VOLUMETRIC FLOW RATE(DRY BASIS)
VOLUMETRIC FLOW RATE(DRY BASIS)
AVERAGE
AVERAGE
AVERAGE
AVERAGE
PERCENT
PERCENT
DRY GAS
DRY GAS
STACK
PI TOT
STACK
STACK
STACK
STACK
GAS
GAS
GAS
GAS
ISOKI NET 1C
EXCESS AIR
METER
METER CORRECTION FACTOR
STATIC GAS PRESSURE
COEFFICIENT
IN STACK GAS
ORIFICE PLATE DIFF. PRESS.
PITOT D IFF. PRESS. VALUE
VALUE
Temperature = 68 deg-F (528 deg-R)
Pressure- =• 29.92 in. Hg.
A-26
-------
APPENDIX B
PROCESS DATA SUMMARY
B-l
-------
-------
APPENDIX B
PROCESS DATA TABLE
Definition of Terms
FEED RATE = sludge feed rate to incinerator, wet basis, ton/hr
ID INLET = induced draft fan inlet temperature, °F
STEAM PROD = waste heat boiler steam production, Ib/hr
VENTURI HLO FLOW = venturi scrubber water flow, gpm
venturi scrubber pressure drop, in. H?0
\2Q
VENTURI DP
SUBCOOLER DP = subcooler pressure drop, in.
SUBCOOLER H20 FLOW = subcooler water flow, gpm
SUBCOOLER TEMP = subcooler gas outlet temperature, °F
CYCLONE DP * cyclone pressure drop, in. H?0
VENTURI TEMP * venturi scrubber gas outlet temperature, °F
SCRUBBER
FLOW = total water flow to venturi scrubber plus subcooler, gpm
B-3
-------
-------
DATE
111584
111584
111584
111584
111584
111584
111584
111584
111584
111584
111534
111584
111584
111584
111584
111584
111584
111584
111584
111584
111584
111584
111584
111584
111584
111784
111784
111734
111784
111784
111784
111784
111784
111784
111784
111784 -
111784
111784
111784
111784
111784
111784
111784
111784.
111784
111784
U1784
111784
111784
111784
111884
111884
111884
TIME
800.
900
1000
1100
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
100
200
300
400
500
600
700
800
300 '
900
1000
1100
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
100
200
300
400
500
600
700
aoo
800
900
iOOO
FEED
RATE
7
7.4
7.'1
8.1
7
6.7
7.3
7.9
7.8
7.7
7.1
7.5
6.2
6.4
6.1
6.4
7.3
6.9
6.9
7.2
7.9
7.8
6.6
8.1
8.9
9
8.9
8.4
"a, 5
9.1
9
9
8.4
7.9
3.5
9.1
3.1
8.9 .
5.3
9
8.8
8.5
8.7
9.4
7.7
6.7
7.9
0
,
7.6
7.8
7.8
ID
INLET
135
140
140
135
135
135
135
135
135
135
135
135
135
135
135
140
140
135
140
• 135
135
135
135
130
130
135
135
135
135
135
130
130
130
130
135
135
135
135
135
135
135
135
140
135
140
140
135
135
135
.
130
130
130
.STEAM VENTURI VENTURI 3UBCOQLR SUBCOOLR SUBCOOLR CYCLONE VENTUftI SCRUBBER
PROD H20 FLOM
8800 '
8200
9100
9600
9400
12160
8200
10120
.
9560
9000
.
10080
9520
8800
9200
7400
6200
10800
8000
8600
9600
11400
10600
9200
14960
15160
14080
14600
14520
14000
13080
13560
14040
13360
13280
12360
12400
13200
12000
8400
13600
11600
14000
12000
15000
12800
12400
11400
0
11040
9960
11080
190
190
190
190
190
190
0
190-
190
190'
190
190.
190
190
190
190
190
190
190
190
190
190
190
180
1BO
180.
190
185
180
180
180
190
190
190
190
190
180
190
190
190
180
180
190
190
190
190
190
0
190
190
190
190
190
DP TEMP H2Q FLQH
24
25
24
25
25
25
.
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
27
26
25
nc
i5
25
25
26
26
26
26
25
26
30
20
20
32
32
32
32
32
32
27 '
,
25
25
25
27
•28.
68
68
68
68
70
70
,
70
70
70
70
70
70
70
69
70
70
70
70
69
69
70
'70
70
70
74
74
74
74
74
74
76
76
76
76
74
76
76
65
65
75
72
75
76
76
76
72
,
70
70
70
74
79
980
980
980
980
980
980
0
930
980
980
980
980
980
980
980
980
980
980
980
980
980
980
980
1000
1000
960
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
960
0
980
980
980
980
980
DP
4.5
3.5
4
5
5.75
5
.
4
3.5
5
4.5
5
5.5
5
4.5
4.5
4.5
4.5
5
5
4.5
4.5
5
5
5
6
5.5
6
6
6
6
6
6
6
6
6
6
7
2
6
1
t
5.5
5.5
7
7
7
6.5
.
6 '
6
6
•7
I
1
DP
3.3
3.6
3.4
3.2
4.2
4.2
.
4
4
3.5
4
2.5
3
3
2.5
2.5
2
2.4
1.5
1.8
2
2
2.4
2.4
2.4
7.6
7.2
8
7.6
7
7.6
7.6
7.4
7.4
7.2
7.4
7.4
7.4
6.8
1.4
1.8
1.3
1.3
6.3
7
7
,
.
4.2
4.4
4.4
4.2
4
TES1P H2Q FLOS
140
140
140
140
140
140
140
140
140
140
140
140
140
135
140
140
140
140
140
140
140
140
140
140
140
150
150
150
150
150 .
150
150
150
150
150
150
150
125
125
150
150
150
150
• 150
150
150
140
,
140
140
140
150-
150
1170
1170
1170
1170
1170
1170
0
1170
1170
1170
1170
1170
1170
1170
1170
1170
1170
1170
1170
1170
1170
1170
1170
1180
1180
1140
1190
1185
1180
1130
1180
1190
1190
1190
1190
1190
1180
1190
1190
1190
1180
1130
1190
1190
1190
1190
1150
0
1170
1170
1170
1170
1170
B-5
-------
111934
111984
111984
111984
111984
111984
111984 '
111984
111984
111984
1U984
111984
111984
111984
111984
111984
111984
111984
111984
111984
111984
111984
111984
111984 .
111984
111984
1 100
800
900
1000
1100
1200
1300
1400
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
100
200
300
4QO
500
600
700
800
7.6
6.9
9
4.8
6.7
6.6
7.2
7
6.9
7.2
7.9
7.6
7.2
6.7
7.7
7.8
7.2
7.2
7.8
7.8
7.2
7.7
7
6.4
6.1
6.6
135
130
130
-130
130
130
130
130
135
135
130
130
140
140
130
130
130
130
130
130
130
130 '
130
130
135
135
14200
11500
11500
10120
9200
10040
9440
9360
10600
7720
10000
•10440
10520
8080
8080
11200
10400
10800
11600
10800
9200
11200
8200
11200
10120
8440
190
190
190
0
0
190
190
190
190
190
190
190
190
190
190
190
190
190
190
190
190
190
190
190
190-
190
25
24
25
.
•
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
25
70
68 '
68
.
.
68
68
68
68
63
68
68
68
65
68
68
68
68
70
70
70
70
70
70
64
64
980
960
960
0
0
960
960
960
960
860
960
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
960
960
6
3.5
3.4
•
.
4.5
4.5
4
4
4.5
4.5
5
4.5
3
4.5
5
5
5
5
5
4.5
4.5
4.5
4.5
3
3.5
, 3
.-l
L
2
•
-
3.2
3.2
3.4
2.5
3
2.5
3
3
2.5
2
3
i. a
2
2.3
2.6
3
2.8
3
2.6
0
0
140
130
"130
•
•
140
140
140
140
135
135
135
135
130
135
140
140
140
140
140
140
140
140
140
130
130
1170
1150
1150
0
0
1150
1150
1150
1150
1050
1150
1190
1190
1190
1190
1190
1190
1190
1190
1190
1190
1190
1190
1190
1150
1150
B-6
-------
APPENDIX C
SAMPLE SHIPMENT LETTER
C-l
-------
-------
, AD TAN
-crporat i an
.November 19,'1934
I. 3. EPA Toxicant Analysis Center
luild.ing 11G5-
lay St. Louis, MS 39529
ittention: Danny McDaniel
Subject: Tier 4 - Analysis Instructions
kaar Sir:
The objective of this letter is to clarify instructions and prior-
ti-es—f-ar individual samples from specific Tier 4 combustion sites.
'his instruction letter is No. 3 and pertains to EPA Site No. 03.
The episode No. is 2494, and SCC numbers assigned to this site were
umbers DQOOO3O1 through DQOO0324.
•SCC numbers DQOOO3O1 through DQOOO306 have been assigned to Troika
or internal QA/QC purposes. Number DQ000324 was not used and all
emaining numbers have been assigned to samples as .described below.
The sample shipment for EPA Site No.
antaining samples.
.03 consists of
boxes'
Instructions for extraction and analysis follow.
The following samples require IMMEDIATE EXTRACTION and analysis
(Priority #1 samples).
Radian Run tt 03-MM5-01 .
(Total of 6 train components)
SCC tt
Container
Fracti on
DQGG0311.
DQOOO311
DQGOG311
DQOOQ311
DQOO0311
OQO00311
1
6
Filter
XAD Module
Probe Rinse
Back Half /
Coil Rinse
Condensate
Impinger Solution
C-3
-------
'J. 3. EPA ECC Toxicdant Analysis Center
-=»ae two
No/ember 19, 19S4
Radian Run # O3-MM5-03
(Total of 6 train components)
SCC #
Container
Fracti on
DQQQ0303
DQ000308
DQOOO3OS
DQ0003QB
DQOOO30S
DQQ0030S
1
6
Filter
XAD Module
Probe Rinse
Back Half /
Coil Rinse
Condensate
Impinger Solution
Radian Run # O3-MM5-Blank
(Total o-f 6 train components)
SCC
Container
Fracti on
DQ000312
DQOOO312
DQOOO312
DQ000312
DQ000312
DQ000312
1
6
Filter
XAD Module
Probe Rinse
Back Half /
Coi'l Rinse
Condensate
Impinger- Solution
Radian Run tt 03-MM5-04
(Total of 6 train components)
SCC #
Contai ner
hracti on
DQ00031.S
DQGOO313
DQ00031S
DQ00031S
DQ00031S
DQ000313
1
6
Filter
XAD Module
Probe Rinse
Back Half /
Coil Rinse
Condensate
Impinger Solution
C-4
-------
5,. EPA ECC Toxicant Analysis Center
chree
amber 19., 1984
Bottom Ash -
SCC ft
Process Sample
Sampl i
DQ000309
DQ000317
DQ000322
Ash
Ash
Ash
Scrubber Slowdown Solids - Process Sample
SCC tt
Sample
======
DQOOO315
DQOOO316
DQ000321
Scrubber blowdown solids
Scrubber blowdown solids
Scrubber blowdown solids
Scrubber Slowdown Filtrate - Process Sample
SCC # . . . Sample
DQOO0313
DQOOO314
DQOO032O
Scrubber blowdown -Filtrate
Scrubber blowdown -filtrate
Scrubber blowdown filtrate
The -Following Priority #2 samples -For this site should be held
-For analysis pending the results o-F Priority #1 analyses:
SCC tt
Sample
DQO003O7
DQO0031O
DQOOO319
Sewage sludge -Feed
Sewage sludge feed
Sewage sludge feed
The soil sample is the only Priority #3 sample. It will be
held at Radian for analysis pending the results of Priority ttl and
Priority #2 samples. The SCC number for the soil sample
is DQOOO323.
If there are any questions concerning this sample shipment, please
tact either Dave Savia, Mike Palazzolo, or Andrew Miles at Radian
p o r a t i cn (919) 541-910O.
Si ncsrely,
05
TEST TEAM LEADER
-------
-------
APPENDIX D
DIOXIN/FURAN ANALYTICAL DATA FOR GASEOUS SAMPLES
D-l
-------
-------
TABLE D-l. -DIOXIN/FURAN ANALYTICAL DATA
FOR MM5 TRAINS - SITE SSI-B
Isomer/
Homologue
Dioxins
2378 TCDD
Other TCDD
Penta CDD
Hexa CDD
Hepta CDD
Octa CDD
Total PCDD
Furans
2378 TCDF.
Other TCDF
Penta CDF
Hexa CDF
Hepta CDF
Octa CDF
Total PCDF
Amount Detected,
Run 01
ND (30.0)
500
ND (50.0)
N.D (480)
300
800
1,600
1,900
19,500
5,400
2,200
ND (620)
100
29,100
Picograms per Sample Train
Run 03
ND (240)
ND (240)
ND (180)
ND (410)
ND (270)
700
700
1,000
6,100
ND (180)
ND (230)
ND (290)
ND (50)
7,100
(Detection limit)
Run 05
ND (40)
100
ND (200)
ND (30)
ND (140)
600
700
.
1,400
9,300 .
2,500
ND (740)
ND (70)
ND (60)
13,200
Spiked at 5 ng in each sample.
3Spiked at 20 ng in each sample.
•*
"ND = not detected. Detection limit ranged from 0.01 to 0.19 ng.
D-3
-------
-------
APPENDIX E
RUN-SPECIFIC DIOXIN/FURAN EMISSIONS DATA
-------
-------
APPENDIX E-l
RUN-SPECIFIC DIOXIN/FURAN EMISSIONS DATA
(As-Measured Concentrations)
E-l
-------
TABLE E-l. DIOXIN/FURAN EMISSIONS DATA FOR RUN 1, SITE SSI-B
Dioxin/Furan
Isomer
Isomer Concentration
In Flue Gas
(ng/dscm)
Isomer Concentration
In Flue Gai»
(ppt)
Isomer Hourly
Emissions Rate
(ug/hr)
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
1
1
3
6
7
7
2
8
3
1
ND (
.92E-01(
ND (
ND (
.15E-01(
.08E-01(
.15E-01
.31E-01(
.50E+00(
.08E+00(
.46E-01(
ND (
.85E-02(
.12E+01
1.15E-02)
N/A )
1.92E-02)
1.85E-01)
N/A )
N/A )
N/A )
N/A )
N/A )
N/A )
2.38E-01)
N/A )
1
6
1
3
5
5
1
• 5
2
8
ND (
.44E-02(
ND (
ND (
.53E-03(
.61E-02(
.70E-02
.74E-02(
.90E-01(
.47E-OH
.43E-02(
ND (
.08E-03(
.50E-01
8.62E-04;
N/A
1.30E-03
1.14E-02
N/A
N/A
N/A
N/A
N/A
N/A
1.40E-02
N/A
-
I- ND
6
ND
ND
1 4
1 1
2
> 2
) 2
7
2
ND
1 1
3
( 4.08E-01)
.80E+00
( 6.80E-01)
( 6.53E+00)
.08E+00
.09E+01
.18E+01
..
.59E+01
.65E+02
.35E+01
.99E+01
( 8.44E+00)
.36E+00
.96E+02
NOTE: Isomer concentrations shown are at as-measured oxygen conditions.
ND » Not detected (detection limit in parentheses).
N/A » Not applicable. QA samples indicate the method capabilities and
minimum limits of detection values when values are positive.
ng » •1.0E-09g
ug - 1.0E-06g
ppt - parts per trillion, dry volume basis
8760 operating hours per year
E-3
-------
TABLE E-2. DIOXIN/FURAN EMISSIONS DATA FOR RUN 3, SITE SSI-B
Dioxin/Furan
Isomer
Isomer Concentration
In Flue Gas
(ng/dscm)
Isomer Concentration
In Flue Gas
(ppt)
Isomer Hourly
Emissions Rate
(ug/hr)
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
ND
ND
ND
ND
ND
1.75E-01(
1.75E-01
6.00E-02)
6.00E-02)
4.50E-02)
1.02E-01)
6.75E-02
N/A
ND
ND
ND
ND
ND
9.15E-03(
4.48E-03)
4.48E-03)
04E-03)
( 6.31E-03)
( 3.82E-03)
" N/A )
( 3,
9.15E-03
ND ( 2.24E+00)
ND ( 2.24E+00)
ND ( 1.68E+00)
ND ( 3.82E+00)
NO ( 2.52E+00)
6.53E+00
6.53E+00
2378 TCDF
Other TCDF-
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
2.50E-01
1.52E+00
ND
. ND
ND
ND ( 1.25E-02)
1.77E+00
N/A.
N/A
4.50E-02
75E-02)
25E-02)
) 1.97E-02(
1.20E-01(
ND (
ND (
ND (
ND (
1.40E-01
N/A
N/A
18E-03)
3.69E-03)
4.26E-03)
6.77E-04)
ND
ND
ND
ND
9.33E+00
5.69E+01
68E+00)
15E+00)
71E+00)
4.66E-01)
6.62E+01
NOTE: Isomer concentrations shown are at as-measured oxygen conditions.
ND = Not detected (detection limit in parentheses).
N/A = Not applicable. QA samples indicate the method capabilities and
minimum limits of detection values when values are positive.
ng = 1.0E-09g
ug = 1.0E-06g
ppt = parts per trillion, dry volume basis
8760 operating hours per year
E-4
-------
TABLE E-3. DIOXIN/FURAN EMISSIONS DATA FOR RUN 5 , SITE SSI-B
Dioxin/Furan
Isomer
Isomer Concentration
In.Flue Gas
(ng/dscm)
Isomer Concentration
In Flue Gas
(ppt)
Isomer Hourly
Emissions Rate
(ug/hr)
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
NO (
2.87E-02(
ND (
ND (
ND (
1.72E-01(
2.01E-01
1.15E-02)
N/A )
5.75E-02)
8.62E-03)
4.02E-02)
N/A )
ND ( 8.59E-04)
2.15E-03
ND
ND
ND
9.02E-03
N/A )
3.88E-03)
5.30E-04)
2.28E-03)
[ N/A )
1.12E-02
ND ( 3.68E-01)
9.20E-01
ND ( 1.84E+00)
ND ( 2.76E-01)
ND ( 1.29E+00)
5.52E+00
6.44E+00
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
4.02E-01(
N/A )
N/A )
N/A )
2.13E-01)
2.01E-02]
ND ( 1.72E-
67E+00(
18E-OH
ND (
ND (
. V/ A /
:-o2)
:-02)
3.
2.
5.
16E-02(
10E-01(
08E-02(
ND (
ND (
N/A )
N/A )
N/A )
1.36E-02)
1.18E-03).
ND ( 9.34E-04)
3.79E+00
2.93E-01
1.29E+01
8.56E+01
2.30E+01
ND ( 6.81E+00)
ND ( 6.44E-01)
ND ( 5.52E-01)
1.21E+02
*
NOTE: Isomer concentrations shown are at as-measured oxygen conditions.
ND
N/A
ng
ug
ppt
Not detected (detection limit in parentheses).
Not applicable. QA samples indicate the method capabilities and
minimum limits of detection values when values are positive.
1.0E-09g
1.0E-06g
parts per trillion, dry volume basis
8760 operating hours per year
E-5
-------
APPENDIX E-2
RUN-.SPECIFIC DIOXIN/FURAN EMISSIONS DATA
(Corrected to 3% Oxygen)
E-7
-------
-------
TABLE E-4- DIOXIN/FURAN EMISSIONS DATA FOR RUN 1
Concentrations Corrected to 3% Oxygen
SITE SSI-B
Dioxin/Furan
Isomer
Isomer Concentration
In Flue Gas
-(ng/dscm @ 3% oxygen)
Isomer Concentration
In Flue Gas
(ppt @ 3% oxygen)
Isomer Hourly
Emissions Rate
(ug/hr)
DIOXINS
2378 TCDD
Other TCDO
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
• NO |
1.10E+00
ND
ND
6.59E-01
1.76E+00
3.52E+00
4.18E+00
4.29E+01
1.19E+01
4.84E+00
ND
2.20E-01
6.40E+01
k 6.59E-02)
N/A )
1.10E-01)
1.05E+00)
N/A )
N/A )
(N/A )
; N/A
( N/A )
( N/A )
( 1.36E+00)
( N/A )
ND (
8.21E-02(
ND (
ND (
3.73E-02(
9.19E-02(
2.11E-01
3.28E-01(
3.37E+00(
8.40E-01(
3.10E-01(
ND (
1.19E-02(
4.86'E+OO
4.93E-03)
N/A )
7.43E-03)
6.49E-02)
N/A )
N/A )
N/A )
N/A )
N/A )
N/A )
8.01E-02)
N/A )
ND ( 4.08E-01)
6.80E+00
ND ( 6.80E-01)
ND ( 6.53E+00)
4.08E+00
1.09E+01
2.18E+01
2-.59E+01
2..65E+02
7.35E+01
2.99E+01
ND ( 8.44E+00)
1.36E+00
3.96E+02
NOTE: Isomer concentrations shown are corrected to 3% oxygen.
ND = Not detected (detection limit in parentheses).
N/A = Not applicable. QA samples indicate the method capabilities and
minimum limits of detection values when values are positive.
ng = 1.0E-09g
ug = 1.0E-06g
ppt = parts per trillion, dry volume basis
8760 operating hours per year
E-9
-------
TABLE E-5. DIOXIN/FURAN EMISSIONS DATA FOR RUN 3
Concentrations Corrected to 3% Oxygen
SITE SSI-B
Dioxin/Furan
Isomer
Isomer Concentration
In Flue Gas
(ng/dscm @ 3% oxygen)
Isomer Concentration
In Flue Gas
(ppt @ 3% oxygen)
Isomer Hourly
Emissions Rate
(ug/hr)
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
ND
NO
ND
ND
ND <
5.86E-01I
2.01E-01
2.01E-01
1.51E-01
3.43E-01
k 2.26E-01
k N/A )
5.86E-01
NO
ND
ND
NO
ND
3.06E-02i
[ 1.50E-02)
1.50E-02)
1.02E-02)
2.11E-02)
1.28E-02)
k N/A )
3.06E-02
ND ( 2.24E+00)
ND ( 2.24E+00)
ND ( 1.68E+00)
ND ( 3.82E+00)
ND ( 2.52E+00)
6.53E+00
6.53E+00
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
8.36E-01(
5.10E+00(
ND (
NO (
NO (
ND (
5.94E+00
N/A )
N/A )
1.51E-01)
1.92E-01)
2.43E-01)
4.18E-02)
6.58E-02(
4.01E-01
NO
NO
NO
ND I
4.67E-01
N/A . )
N/A )
1.07E-02)
1.23E-02)
1.43E-02)
2.27E-03)
9.33E+00
5.69E+01
ND ( 1.68E+00)
ND ( 2.15E+00)
ND ( 2.71E+00)
ND ( 4.66E-01)
6.62E+01
NOTE: Isomer concentrations shown are corrected to 3% oxygen.
ND
N/A
Not detected (detection limit in parentheses).
Not applicable. QA samples indicate the method capabilities and
minimum limits of detection values when values are positive.
1.0E-09g
1.0E-06g
parts per trillion, dry volume basis
8760 operating hours per year
ng
ug
E-10
-------
TABLE E-6. DIOXIN/FURAN EMISSIONS DATA FOR RUN 5, SITE
Concentrations Corrected to 3% Oxygen
S'SI-B
Dioxin/Furan
Isomer
Isomer Concentration Isomer Concentration
In Flue Gas In Flue Gas
(ng/dscm @ 3% oxygen) (ppt @ 3% oxygen)
Isomer Hourly
Emissions Rate
(ug/hr)
DIOXINS
2378 TCDD
Other TCDO
Penta-CDD
Hexa-CDD
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
ND (
9.74E-02(
ND (
ND (
ND (
5.84E-01(
6.82E-01
3.90E-02)
N/A )
1.95E-01)
2.92E-02)
1.36E-01)
N/A )
ND (
.28E-03(
2.91E-03)
N/A
ND (
ND (
3.06E-02(
3.78E-02
NO ( 1.32E-02
1.80E-03)
7.72E-03)
N/A )
ND ( 3.68E-01)
9.20E-01
ND ( 1.84E+00)
ND ( 2.76E-01)
ND ( 1.29E+00)
5.52E+00
6.44E+00
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF.
1.36E+00(
9.06E+00(
2.44E+00(
ND (
ND (
ND (
1.29E+01
N/A )
N/A )
N/A )
7.21E-01)
6.82E-02)
5.84E-02)
,07E-01(
.12E-01I
1.72E-01(
ND (
ND (
ND (
9.92E-01
N/A .)
N/A )
N/A )
4.62E-02
4.01E-03
3.17E-03)
1.29E+01
8.56E+01
2.30E+01
ND ( 6.81E+00)
ND ( 6.44E-01)
ND ( 5.52E-01)
1.21E+02
NOTE: Isomer concentrations shown are corrected to 3% oxygen.
ND = Not detected (detection limit in parentheses).
N/A = Not applicable. QA samples indicate the method capabilities and
minimum limits of detection values when values are positive
ng = 1.0E-09g
ug = 1.0E-06g
ppt = parts per trillion, dry volume basis
8760 operating hours per year
E-ll
-------
-------
APPENDIX F
RUN-SPECIFIC RISK MODELING INPUT DATA
F-l
-------
-------
TABLE F-I. RISK MODELING PARAMETERS FOR RUN i, SITE SSI-B
Stack Height (From Grade level) = 27
Stack Diameter (ID) = 0.74
Flue Gas Flow Rate (Dry Standard) = 590
Flue Gas Exit Temperature = 349
Flue Gas Exit Velocity (Actual) = 1725
Dioxin/Furan
Isomer
I some r
Concentration
In Flue Gas
(ng/dscm)
Isomer Hourly
Emissions
Rate
(ug/hr)
Relative
Potency
Factor
2,3,7,8 - TCDD
Equivalent
Emissions
(mg/yr)
2378 TCDD
Other TCDD
2378 TCDF
Other TCDF
.Penta-CDD
Penta-CDF
Hexa-CDD
Hexa-CDF
Hepta-CDD
Hepta-COF
Octa-CDD
Octa-CDF
ND
NO
ND
ND
( 1.15E-02)
1.92E-01
31E-01
50E+00
1.92E-02)
08E+00
( 1.85E-01)
8.46E-01
1.15E-01
( 2.38E-01)
3.08E-01
3.85E-02
7.
7.
2.
ND ( 4.08E-01)
6.80E+00
2.S9E+01
2.65E+02
ND ( 6.80E-01)
7.35E+01
ND ( 6.53E+00)
"2.99E+01
4.08E+00
ND ( 8.44E+00)
1.09E+01
1.36E+00
Net 2378 TCDD Equivalent Atmospheric Loading
1.000 ND ( 3.58E+00)
.010 5.96E-01
.100 2.26E+01
.001 2.32E+00
.500 ND ( 2.98E+00)
.100 6.44E+01
.040 ND ( 2.29E+00)
.010 2.62E+00
.001 3.58E-02
.001 ND ( 7.39E-02)
.000 .OOE+00
.000 .OOE+00
9.26E+01
ND = not detected (detection limit in parentheses).
N/A = detection limit not available
ng = 1.0E-09g
ug = 1.0E-06g
mg - 1.0E-03g
Standard conditions: 293 K (20 C) temperature and 1 atmosphere pressure.
8760 operating .hours per year
F-3
-------
TABLE F-2. RISK MODELING PARAMETERS FOR RUN 3, SITE SSI-B
Stack Height (From Grade Level) = 27
Stack Diameter (ID) - 0.74
Flue Gas Flow Rate (Dry Standard) - 622
Flue Gas Exit Temperature = 349
Flue Gas Exit Velocity (Actual) - 1827
Dioxin/Furan
Isomer
2378 TCDD
Other TCDD
2378 TCDF
Other TCDF
Penta-CDD
Penta-CDF
Hexa-CDD
Hexa-CDF
Hepta-CDD
Hepta-CDF
Octa-CDD
Octa-CDF
Isomer
Concentration
In Flue Gas
(ng/dscm)
ND ( 6.00E-02)
ND ( 6.00E-02)
2.50E-01
1.52E+00
ND ( 4.50E-02)
ND ( 4.50E-02)
ND ( 1.02E-01)
ND ( 5.75E-02)
ND ( 6.75E-02)
ND ( 7.25E-02)
1.75E-01
ND ( 1.25E-02)
Isomer Hourly
Emissions .
Rate
(ug/hr)
ND ( 2.24E+00)
ND ( 2.24E+00)
9.33E+00
5.69E+01
ND ( 1.68E+00)
ND ( 1.68E+00)
ND ( 3.82E+00)
ND ( 2.15E+00)
ND ( 2.52E+00)
ND ( 2.71E+00)
6.53E+00
ND ( 4.66E-01)
Relative
Potency
Factor
1.000
.010
.100
.001-
.500
.100
.040
.010
.001
.001
.000
.000
2,3,7,8 - TCDD
Equivalent
Emissions
(mg/yr)
ND ( 1.96E+01)
ND ( 1.96E-01)
8.17E+00
4.99E-01
ND ( 7.36E+00)
ND ( 1.47E+00)
ND ( 1.34E+00)
ND ( 1.88E-01)
ND ( 2.21E-02)
ND (.2.37E-02)
.OOE+00
ND ( .OOE+00)
Net 2378 TCDD Equivalent Atmospheric Loading
8.67E+00
ND - not detected (detection limit in parentheses).
N/A » detection limit not available
ng » 1.0E-09g
ug * 1.0E-06g
mg » 1.0E-03g
Standard conditions: 293 K (20 C) temperature and 1 atmosphere pressure.
8760"operating hours per year
F-4
-------
TABLE F-3. RISK MODELING PARAMETERS FOR RUN- 5 , SITE SSI-B
Stack Height (From Grade Level) = 27
Stack Diameter (ID) = 0.74
Flue Gas Flow Rate (Dry Standard) = 534
Flue Gas Exit Temperature * 351
Flue Gas Exit Velocity (Actual) = 1536
Dioxin/Furan
Isomer
2378 TCDD
Other TCDD
2378 TCDF
Other TCDF
Penta-CDD
Penta-CDF
Hexa-CDD
Hexa-CDF
Hepta-CDD
Hepta-CDF
Octa-CDD
Octa-CDF
Isomer
Concentration
In Flue Gas
(ng/dscm)
ND ( 1.15E-02)
2.87E-02
4.02E-01
2.67E+00
ND ( 5.75E-02)
7.18E-01
ND ( 8.62E-03)
ND ( 2.13E-01)
ND ( 4.02E-02)
ND ( 2.01E-02)
1.72E-01
ND ( 1.72E-02)
Isomer Hourly
Emissions
Rate
(ug/hr)
ND ( 3.68E-01)
9.20E-01
1.29E+01
8.56E+01
ND ( 1.84E+00)
2.30E+01
ND ( 2.76E-01)
ND ( 6.81E+00)
ND ( 1.29E+00)
ND ( 6.44E-01)
5.52E+00
ND ( 5.52E-01)
Relative
Potency
Factor
1.000
.010
.100
..001
.500
.100
.040
.010
.001
.001
.000
.000
2,3,7,8 - TCDD
Equivalent
Emissions
(mg/yr)
ND ( 3.23E+00)
8.06E-02
1.13E+01
7.50E-01
ND ( 8.06E+00)
2.02E+01
ND ( 9.68E-02)
ND ( 5.97E-01)
ND ( 1.13E-02)
ND ( 5.64E-03)
.OOE+00
ND ( .OOE+00)
Net 2378 TCDD Equivalent Atmospheric Loading
3.23E+01
ND = not detected (detection limit in parentheses).
N/A = detection limit not available
ng = 1.0E-09g
ug = 1.0E-06g
mg = 1.0E-03g
Standard conditions: 293 K (20 C) temperature and 1 atmosphere pressure.
8760 operating hour-s per year
F-5
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TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
EPA-450/4-84-014/
riTLE AND SUBTITLE
3. RECIPIENT'S ACCESSION NO.
National Dioxin Study Tier 4 - Combustion Sources
Final Test Report - Site 3
Sewage Sludge Incinerator SSI - B
5. REPORT DATE
April 1987
i. PERFORMING ORGANIZATION CODE
'. AUTHOR(S)
Michael A. Palazzolo, D. Blake Bath,
Martha H. Keating
8. PERFORMING ORGANIZATION REPORT NO.
87-231-056-12-46
I. PERFORMING ORGANIZATION NAME AND ADDRESS
Radian Corporation
Post Office Box 13000
Research Triangle Park, NC 27709
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
68-03-3148
12. SPONSORING AGENCY NAME AND ADDRESS
U.S. Environmental Protection Agency, OAQPS
Research Triangle Park, NC 27711
Office of Research and Development
Washington, DC 20460
13. TYPE OF REPORT AND PERIOD COVERED
Final
14. SPONSORING AGENCY CODE
5. SUPPLEMENTARY NOTES
EPA Project Officers:
Donald Oberacker, ORD
William B. Kuykendal, OAQPS
This report summarizes the results of a dioxin/furan emissions test of a sewage sludge
incinerator equipped with a wet scrubber system for particulate matter emissions
control. The test was the third in a series of thirteen dioxin/furan emissions
tests conducted under Tier 4 of the National Dioxin Study. The primary objective of
Tier 4 is to determine if various combustion sources are sources of dioxin and/or
furan emissions. If any of the combustion sources are found to emit dioxin or furan,
the secondary objective of Tier 4 is to quantify these emissions.
Sewage sludge incinerators are one of eight combustion source categories tested in
the Tier 4 program. The tested sewage sludge incinerator, hereafter referred to as
incinerator SSI-B, was selected for this test after an initial information screening
and a one-day pretest survey visit.
Data presented in the report include dioxin (tetra through octa horaologue + 2378 TCDD)
and furan (tetra through octa homologue + 2378 TCDF) results for both stack samples
and ash samples. In addition, process data collected during sampling are also
presented.
7.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
c. COSATI Field/Group
Air Emissions
Combustion Sources
Dioxin
Furans
2,3,7,8 Tetrachlorodibenzo-p-dioxin
.Sewage Sludge Incinerator
Incineration
Air Pollution Emissions
Data
8. DISTRIBUTION STATEMENT
Release Unlimited
19. SECURITY CLASS f This Report/
Unclassified
21. NO. OP PAGES
170
20. SECURITY CLASS (This page>
TTnr* 1 23 c Q *? f i o/^
22. PRICE
EPA Form 2220-1 (R*v. 4-77) PRevious EDITION is OBSOLETE
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