EPA-450/4-84-014n
NATIONAL DIOXIN STUDY
TIER 4 — COMBUSTION SOURCES
Final Test Report — Site 5
Black Liquor Boiler BLB — B
By
Michael A. Palazzolo
Winton E. Kelly
Donna Holder
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
Research 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 reflect the views and
policies of the Agency, neither does mention of trade names or commercial products
constitute endorsement or recommendation for use.
EPA-450/4-84-014n
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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 Title
J_LL!g Page
1.0 Introduction , ,
2.0 Summary „
2.1 Test Description. ...!.*!'.* «"}
2.2 Summary of Results o"i
2.2.1 ESP Inlet Data ?\
2.2.2 ESP Outlet Data o~7
2.2.3 Inlet/Outlet Comparison '!".'.''.'''' 2-8
3.0 Process Description. . . . - ,
3.1 Facility Description. ....... 3 }
3.2 Black Liquor Recovery Boiler Description! .' 3 ?
3.3 Electrostatic Precipitator Description. ...'.'.'.'.'.'.'. 3-2
4.0 Test Description .
4.1 Field Sampling '. T":
4.2 Process Data Collection . . . '. J"i
4.3 Laboratory Analyses '. Tj.
4.3.1 Dioxin/Furan Analyses. . . . . [ J"|
4.3.2 Dioxin/Furan Precursor Analyses. . . *~l
4.3.3 Total Chloride Analyses '""'"'! Jly
5.0 Test Results
5.1 Process Data * "!*.'!". c"{
5.1.1 Black Liquor Boiler'operating*Data '.'.'. 51
R o ci 2^ E1ectrostatic Precipitator Operating Data. !.'*'* 5.1
5.2 Flue Gas Parameter Data 2 i
5.3 Continuous Emissions Monitoring Data I 7
5.4 Dioxin/Furan Emissions Data . . r"(q
5.4.1 Electrostatic Precipitator Inlet '.'.'.'. \ 5~ia
5.4.2 Electrostatic Precipitator Outlet. . . ' ' ' 5 ?R
5.4.3 Reduction of Dioxin/Furan Concentrations Due to* * '
c e , the ESPfor Site BLB-B r ,n
5.5 Black Liquor Precursor Data . . ........ o-ju
5.6 Auxiliary Process Sample Analyses . ! .' i",S
5.7 HC1 Train Chloride Emissions Data . . 2,0
5.8 Soil Sampling Data '.'.'.'.'.'.'.''' sl^
6.0 Sampling Locations and Procedures. * ,
6.1 Gaseous Sampling ! ! ! ! ! 61
6.1.1 Gaseous Sampling Locations .' p~\
6.1.1.1 ESP Outlet fi~}
6.1.1.2 ESP Inlet '.'.'.'. g 1
6.1.1.3 Recovery Boiler Outlet. .........'. 6-4
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Section
TABLE OF CONTENTS
(cont'd.)
Title
6.1 Gaseous Sampling (cont'd.)
6.1.2 Gaseous Sampling Procedures 6-4
6.1.2.1 Modified Method 5 (MM5) 6-4
6.1.2.2 HC1 Determination 6-11
6.1.2.3 Volumetric Gas Flow Rate Determination . . . 6-12
6.1.2.4 Flue Gas Moisture Weight Determination . . . 6-12
6.1.2.5 Flue Gas Molecular Weight Determination. . . 6-12
6.1.2.6 Continuous Monitors 6-13
6.2 Liquid Sampling 6-13
6.2.1 Strong Black Liquor Circuit Sampling 6-14
6.2.2 Auxiliary Black Liquor Circuit Sampling 6-14
6.3 Solid Sampling 6-15
6.3.1 By-product Saltcake Sampling 6-15
6.3.2 Soil Sampling 6-15
7.0 Analytical Procedures 7-1
7.1 Dioxin/Furan Analyses 7-1
7.2 Dioxin/Furan Precursors 7-2
7.2.1 GC/M5 Analyses 7-2
7.2.1.1 Sample Preparation . 7-2
7.2.1.2 Analysis 7-5
7.3 TOX Analysis 7-7
7.4 Total Chloride Analyses 7-7
8.0 Quality Assurance/Quality Control (QA/QC) 8-1
8.1 -Manual Gas Sampling 8-1
8.1.1 Equipment Calibration and Glassware Preparation ... 8-2
8.1.2 Procedural QC Activities/Manual Gas Sampling 8-2
8.1.3 Sample Custody 8-5
8.2 Continuous Monitoring/ Molecuar Weight Determination .... 8-5
8.3 Laboratory Analysis >. 8-7
8.3.1 Dioxin/Furan Analyses 8-7
8.3.1.1 Surrogate Recoveries of the Test Samples . . 8-7
8.3.1.2 Sample Blanks 8-7
8.3.2 Precursor Analyses 8-10
8.3.3. Total Chloride Analysis 8-10
Appendix A Field Sampling Data
A.I Modified Method 5 and EPA Methods 1-4 Field Results A-l
A.2 Continuous Emission Monitoring Results A-25
A.3 HC1 Train Results A-33
A.4 Modified Method 5 Sample Calculations A-45
Calculations - Definitions of Terms and Sample Calculation. . . . A-51
Appendix B Sample Shipment Letter „ B-l
VI
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TABLE OF CONTENTS
(cont'd.)
Section r-mo
-LLLLe Page
Appendix C Dioxin/Furan Analytical Data for Modified Method 5 Trains. C-l
Appendix D Run-Specific Dioxin/Furan Emissions Data
D.I As-Measured Concentrations n ,
D.2 Concentrations Corrected to 3 Percent'Oxygen .'!.'!!!!! D-7
Appendix E Run-Specific Risk Modeling Input Data
E.I ESP Inlet _ ,
E.2 ESP Outlet •" i .' 1 1 I.'!.'!.'! E-7
Appendix F Compound-Specific Precursor Results p.j
Appendix G Research Triangle Institute (RTI) Audit Report G-l
Appendix H Process Monitoring Data
8'2 5?anJyrnV6rage JtalUe? °£ 5°11er °P«««ns Parameters .... H-l
H.2 Plant Computer Output of Process Data. H 7
H.3 Electrostatic Precipitator Electrical Data .' .' ! .' ! '.'.'.'.
Appendix I Field D.ata Sheets
Appendix J Project Participants
Appendix K Volumetric Flowrate: Blocked Duct Corrections
Appendix L Error Analysis of Control Device Efficiency Calculations .
H-37
1-1
J-l
K-l
L-l
vi i
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LIST OF FIGURES
Figure
Page
2-1 Simplified Flow Diagram of Black Liquor Recovery Boiler BLB-B . . .2-2
2-2 Data Summary for Site BLB-B
4-1 Process Flow Diagram and Sampling Location for Site BLB-B 4.4
5-1 Hourly Boiler Operating Data for Run 1 5.3
5-2 Hourly Boiler Operating Data for Run 2 5.4
5-3 Hourly Boiler Operating Data for Run 3 5.5
5-4 Volume Percent Oxygen versus Volume Percent C0? in the Flue
' n " 5-11
5-5 Oxygen Concentration versus Test Time, Site BLB-B 5_13
5-6 Carbon Dioxide Concentration versus Test Time, Site BLB-B 5-14
5-7 Carbon Monoxide versus Test Time, Site BLB-B 5_16
5-8 Total Hydrocarbon Concentration versus Test Time 5.!7
5-9 Sulfur Dioxide Concentration versus Test Time, Site BLB-B 5-13
5-10 Nitrogen Oxides Concentration versus Test Time, Site BLB-B 5-20
5-11 Dioxin and Furan Homologue Distributions of the Electrostatic
DMA/* ir\4-^n4>Av* T M n «*x r* • • *» »»• • w wi^wi*iwoi»ciul\*
rrecipitator Inlet Emissions for Site BLB-B 5.75
5-12 Dioxin and Furan Homolgue Distributions of the Electrostatic
Precipitator Outlet Emissions for Site BLB-B. . .5.33
6-1 ESP Outlet Port Location, Site BLB-B. c -
o-d
6-2 Sample Point Layout, ESP Outlet Site BLB-B. . 6.3
6-3 ESP Inlet Sample Port Location, Site BLB-B 6.5
6-4 Sample Point Layout, ESP Inlet Ducts, Site BLB-B 5.5
6-5 Modified Method 5 Train
6-6 Adsorbent Sampling System . . - ,n
' ' o-lO
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LIST OF FIGURES
(cont'd.)
Figure Title page
6-7 Soil Sampling Locations, Site BLB-B 6-17
7-1 Sample Preparation Flow Diagram for Site BLB-B Precursor Analyses .7-3
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LIST OF TABLES
Clll
2-1
2-2
2-3
2-4
3-1
4-1
5-1
5-2
5-3
5-4
5-5
5-6
5-7
5-8
5-9
5-10
5-11
Page
Source Sampling and Analysis Overview for Site BLB-B 2-3
Summary of Mean Dioxin/Furan Emissions Data for Site BLB-B
(ESP Inlet) * r
Summary of Mean Dioxin/Furan Emissions Data for Site BLB-B
(ESP Outlet) « 7
ESP Inlet/Outlet Dioxin/Furan Emissions Data Summary 2-9
Chlorine Contents and Flow Rates for Various Pulo Mill
Process Streams at Site BLB-B 3.3
Source Sampling and Analysis Matrix for Site BLB-B 4-2
Mean Values for Boiler Operation Parameters During Dioxin
Testing at Site BLB-B 7 . . 52
ESP Operating Data for Site BLB-B. . c c
3-D
Flue Gas Parameters at Site BLB-B 5.8
Summary of Oxygen and Carbon Dioxide Results . 5.9
Mean Values and Standard Deviations of Continuously Monitored
Combustion Gases at the Recovery Boiler Outlet 5-12
Overview of Dioxin/Furan Emissions Concentrations Data for
Site BLB-B (Electrostatic Precipitator Inlet 5_2i
Summary of Dioxin and Furan Emissions Rate Data for Site BLB-B
(Electrostatic Precipitator Inlet) ? ? ? . . .5-22
Summary of Dioxin/Furan Emissions Data for Site BLB-B Inlet
(As-measured concentration) 5.23
Summary of Dioxin/Furan Emissions Data for Site BLB-B Inlet
(Concentrations corrected to 3% Oxygen) 5_24
Dioxin/Furan Emission Factors for Site BLB-"B Inlet 5-27
Overview of Dioxin and Furan Emissions Concentrations Data for
. Site BLB-B (Electrostatic Precipitator Outlet) 5-28
XI
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LIST OF TABLES
(cont'd.)
Table Title Page
5-12 Summary of Dioxin and Furan Emissions Rate Data for Site BLB-8 . . .5-29
5-13 Summary of Dioxin/Furan Emissions Data for Site BLB-B Outlet. . . . 5-31
5-14 Summary of Dioxin/Furan Emissions Data for Site BLB-B
{Concentrations corrected to 3% Oxygen) . , 5-32
5-15 Dioxin/Furan Emission Factors for Site BLB-B Outlet 5-34
5-16 ESP Removal Efficiencies at Site BLB-B 5-36
5-17 Summary of Dioxin Precursor Data for Site BLB-B Feed Samples. . . . 5-37
5-18 Total Chloride Analyses of Black Liquor Samples for Site BLB-B. . . 5-38
5-19 Summary of Total Chloride Data for Site BLB-B 5-40
5-20 HC1 Chloride Emissions Data for Site BLB-B at Electrostatic
Precipitator Outlet 5-41
6-1 Summary of Gas Sampling Methods for Site BLB-B 6-7
6-2 Description of Soil Sampling Locations at Site BLB-B 6-16
7-1 Instrument Conditions for GC/MS Precursor Analyses 7-6
•
7-2 Components of the Calibration Solution 7-8
7-3 Analytical Conditions for TOX Analysis .7-9
8-1 Glassware Precleaning Procedure 8-3
8-2 Summary of Isokinetic Rate Results for MM5 Sampling, Site BLB-B. . .8-4
8-3 Summary of Drift Check and Control Standard Results 8-6
8-4 Percent Surrogate Recoveries for Site BLB-B Dioxin/Furan Analyses. .8-8
8-5 Analysis Results'for Quality Control Samples 8-9
8-6 Field Blank Dioxin/Furan Data for Site BLB-B MM5 Samples 8-11
8-7 Percent Surrogate Recoveries for Site BLB-B Feed Samples 8-12
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1.0 INTRODUCTION
This report summarizes the results of a dioxin/furana emissions test of a
black liquor recovery boiler equipped with a dry-bottom electrostatic
precipitator for particulate emissions control. Black liquor recovery boilers
are used at Kraft pulp mills to produce process steam and to reclaim inorganic
chemicals from spent wood pulping liquors. This test is the fifth in a series
of several dioxin/furan emissions tests being conducted under Tier 4 of the
National Dioxin Study. The primary objective of Tier 4 is to determine if
various combustion processes 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.
Black liquor recovery boilers are one of 8 combustion source categories
that have been tested in the Tier 4 program. After an initial information
screening and .one-day pre-survey visit, this site (BLB-B) was selected
partially because of the higher chloride content of the black liquor (3.5 wt.
%, dry) compared to other black liquor recovery boiler sites surveyed in the
Tier 4 study (approximately 0.2 to 1.0 wt %, dry). However, the Site BLB-B
chloride content of the black liquor was determined to be 0.53 wt%, dry,
during the field testing. Also, the weak black liquor concentrating
evaporators use direct contact of the hot boiler combustion gases with the
weak black liquor, which is a common practice for black liquor boilers
installed prior to the early*1970's. The other two black liquor boilers
tested in the Tier 4 study (i.e., BLB-A and BLB-C do not use direct contact
evaporation).
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,
description 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" as used in this report refers to the polychlorinated
dibenzo-p-dioxin and dibenzofuran isomers with four or more chlorine atoms.
1-1
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2.0 SUMMARY
The host plant (Site BLB-B) is a Kraft pulp mill that produces pulp and
paper products. Black liquor recovery boiler BLB-B combusts strong black
liquor from the pulping process and recovers the inorganic chemicals used to
produce pulp from wood chips. Particulate emissions from black liquor boiler
BLB-B are controlled by a dry bottom electrostatic precipitator. A simplified
process flow diagram of the system is shown in Figure 2-1.
2.1 TEST DESCRIPTION
The gaseous, liquid, and solid sampling performed during the test program
is summarized in Table 2-1. Sampling for dioxin/ furan was performed
simultaneously at the electrostatic precipitator outlet exhaust stack and
electrostatic precipitator inlet location (i.e., black liquor boiler outlet)
in each of a series of three test runs conducted on February 26 through 28,
1984. The dioxin/furan sampling followed the October 1984 draft of the
Modified Method 5 (MM5) procedure recommended by the American Society of
Mechanical Engineers (ASME) for measuring emissions of chlorinated organic
compounds. This protocol was strictly followed for Site BLB-B except for the
modifications discussed in Section 6.1.2.1 (solvent change and condenser
orientation). MM5 train components and train rinses were analyzed for
dioxins and furans by EMSL-RTP and ECL-Bay St. Louis, two of three EPA
laboratories collectively referred to as Troika. The dioxin/furan analysis
quanti fi ed 2,3,7,8-tetrachlorodi benzo-
p-dioxin (TCDD) and the tetra- through octa- dioxin/furan homoloques present
in the samples.
Dioxin/furan precursor and TOX analyses were performed by Radian on
samples of the concentrated black liquor fed to the boiler. The specific
dioxin precursors analyzed for were chlorophenols, chlorobenzenes, and
polychlorinated biphenyls. Total chlorine analyses were performed by RTI on
concentrated liquor samples. Samples of the black liquor circuit
intermediates (white liquor and weak black liquor) and the major chlorine
inputs to the system (R2 C102 plant neutralized spent acid, R3 C102 plant
byproduct saltcake, and process makeup water) were collected and analyzed by
Radian for total chlorine.
2-1
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TABLE 2-1. SOURCE SAMPLING AND ANALYSIS OVERVIEW FOR SITE BLB-B
Item
Item Description
1. Number of test runs
2. Gaseous sampling
3. Liquid sampling
4. Solids sampling
- Three identical test runs (Runs 1, 2, 3).
- MM5 sampling at black liquor boiler outlet
and ESP outlet exhaust stack (Runs 1, 2, 3).
Dioxin analysis.
- EPA Reference Methods 2 and 4 at black liquor
boiler outlet and ESP outlet exhaust stack
(Runs 1, 2, 3). Gas velocity and moisture.
- Integrated bag sampling at black liquor
boiler outlet and ESP outlet exhaust stack
(Runs 1, 2, 3). CO-, 0,, N2, analysis for
molecular weight determination.
- HC1 sampling at ESP outlet exhaust stack
(Runs 1, 2, 3).
- Continuous monitoring of CO, CO-, 0-, NO ,
SO-, total hydrocarbons at blacR liquor
bofler outlet (Runs 1, 2, 3).
- Strong black liquor sampling (Runs 1, 2, 3).
Dioxin analysis, dioxin precursor analysis,
total chlorine analysis.
- White liquor sampling (Runs 1, 2, 3). Total
chlorine analysis.
- Weak black liquor sampling (Runs 1, 2, 3).
Total chlorine analysis.
- C102 system waste acid sampling.
(Runs 1,2,3). Total chlorine analysis.
- Well water sampling (Runs 1, 2, 3). Total
chlorine analysis.
- Soil sampling3 (one composite sample from
10 locations). Potential dioxin analysis.
- CIO- system byproduct salt cake sampling.
(Runs 1, 2, 3). Total chlorine analysis.
Sample(s) to be analyzed pending evaluation of the dioxin/furan emission
data from the MM5 sampling train.
2-3
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The total chlorine analyses for these streams were performed to provide
information on the major chlorine inputs to the black liquor circuit (see
Table 3-1).
Continuous emission monitoring (CEM) was performed by Radian at the black
liquor boiler outlet for CO, C02, NOX, S02, total hydrocarbons (THC), and 02-
The continuous monitoring data will be used in conjunction with the process
data to relate dioxin emissions to combustion conditions.
A single set of soil samples was collected by Radian and may be analyzed
for dioxin by Troika. The soil sample results would provide information on
the dioxin content of soils near the plant.
2.2 SUMMARY OF RESULTS
Figure 2-2 summarizes the data obtained at Site BLB-B during the Tier 4
test program. The black liquor boiler and electrostatic precipitator (ESP)
were operated under conditions representative of normal operation during the
sampling periods. Detectable quantities were found for roughly two-thirds of
all dioxin and furan species analyzed for in the stack gas emissions.
2.2.1 ESP Inlet Data
As shown in Table 2-2, average as-measured stack gas concentrations of
2378 TCDD, total PCDD, and total PCDF were not detected, 15.1, and .93
•
ng/dscm, respectively. This corresponded to hourly mass emission rates of
.004 g/hr total PCDD, and .0002 g/hr total PCDF. Emissions of 2378 TCDD,
other TCDD, and Penta-CDD were not detected for any of the runs. The octa-CDD
homologue was significantly more prevalent than the hexa- and
hepta-chlorinated dioxins.
2.2.2 ESP Outlet Data
As shown in Table 2-3, average as-measured stack gas concentrations of
2378 TCDD, total PCDD, and total PCDF were not detected, 1.02, and .60
ng/dscm,~respectively. This corresponded to hourly mass emission rates of
.0002 g/hr total PCDD, and .0001 g/hr total PCDF. Emissions of 2378 TCDD,
other TCDD, and penta-CDD were non-detectable among runs. The octa-CDD
homologue was significantly more prevalent than the hexa- and
2-4
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TABLE 2-2. SUMMARY OF MEAN DIOXIN/FURAN EMISSIONS DATA
" FOR SITE BLB-B (ESP INLET)
Parameter
2378 TCDD
Total PCDD Total PCDF
Emissions Concentration (ng/dscm)
As Measured
Corrected to 3% 02
Emissions Rate fug/hr)
NO
NO
ND
15.1
17.1
3383
.93
1.07
209
ND - not detected.
2-6
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TABLE 2-3. SUMMARY OF MEAN DIOXIN/FURAN EMISSIONS
DATA FOR SITE BLB-B (ESP OUTLET)
Parameter
2378 TCDD Total PCDD Total PCDF
Emissions Concentration fnq/dscm)
As-Measured
Corrected to 3% 0«
Emissions Rate (uo/hr^
NO
NO
NO
1.02
1.19
230
.60
.71
136
ND = not detected.
2-7
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hepta-chlorinated dioxins. Total furan emissions were fairly evenly
distributed with the-exception of the penta-chlorinated furan homologue which
was consistently non-detectable among runs. Table 2-4 compares dioxin/furan
emission before and after the ESP.
2.2.3 ESP Dioxin/Furan Emissions Reduction
As shown in Table 2-4, the total PCDD concentration in the stack gas was
reduced by 93 percent across the ESP. The total PCDF concentration decreased
by 35 percent.
Figure 2-2 summarizes the additional data obtained at Site BLB-B. Strong
black liquor feed was analyzed for chlorinated benzenes, chlorinated
biphenyls, and chlorinated phenols, but only trace levels of pentachlorophenol
were found. There were no total organic halides (TOX) found in the strong
black liquor. The boiler was operated similarly during the individual test
runs with the exception of a slightly lower flue gas oxygen content for Run 02
compared with Runs 01 and 03. There were no process upsets during any of the
runs that resulted in sampling interruptions. Boiler load during the test
periods averaged 343.4 (1,000 Ib/hr of steam at 900 psi, 820°F), and the black
liquor feed temperature to the boiler averaged 259°F. The ESP power
consumption in the north and south compartments averaged 6.5 and 11.8 KW,
respectively. The average ESP outlet temperature was 328°F.
Average flue gas concentrations measured in the exhaust stack by the
Radian continuous emission monitoring system were: Og, 12.2 vol.%; COg, 17.4
vol.%; CO, 10,900 ppmv; THC, 57.7 ppmv (C3); S02, 830 ppmv; and NOX, 42.6
ppmv, all corrected to 3% 0«» on a dry basis except for THC. Total chloride
emissions concentrations measured using the HC1 train at the ESP outlet
exhaust stack were 2.1 ng/dscm (as-measured), and the total HC1 emission rate
was .44 Kg/hr. The front half of the HC1 train (i.e., probe rinse and filter)
accounted for roughly 90 percent of the total chloride emissions and the back
half (i.e., impingers and back half rinse) accounted for the remaining 10
percent. The total chloride content measured for the various process samples
was neutralized spent acid, 805 ug/g; by-product salt cake, 1,200 ug/g; white
liquor, 6,150 ug/g; and make-up water, 230 ug/g, expressed as Cl".
2-3
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TABLE 2-4. ESP INLET/OUTLET DIOXIN/FURAN EMISSIONS DATA SUMMARY
Parameter
Inlet
Outlet
% Emissions
Reduction
Emission Concentration. As-measured (nq/dscm)
2378 TCDD ND
Total PCDD 15.1
Total PCDF .93
Emission Rate fug/hr)
2378 TCDD
Total PCDD
Total PCDF
ND
3383
209
ND
1.02
.60
ND
230
136
0
93
36
0
93
35
ND = Not Detected
2-9
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The composite soil sample obtained at Site BLB-B is currently being
analyzed by a non-Tier 4 EPA group for dioxin/furan content.
2-10
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3.0 PROCESS DESCRIPTION
This section describes the host site and the black liquor recovery
boiler/electrostatic precipitator system tested. Data summarizing the
operation of the boiler and the precipitator during the test periods are
presented in Section 5.0.
3.1 FACILITY DESCRIPTION
The host plant, (Site BLB-B), is a Kraft pulp mill with a rated capacity
of 1725 Mg/day (1900 TPD) of air-dried pulp. The plant maintains two black
liquor recovery boilers with rated capacities of 725 Mg/day (800 TPD) and 1000
MG/day (1100 TPD) of air-dried, unbleached pulp. The dioxin/furan emissions
tests were conducted on the 725 Mg/day (800 TPD) boiler.
Both soft and hard woods (pine and gum) are processed at Site BLB-B.
Wood and wood chips are transported to the plant by truck. None of the wood
processed in the pulping circuit has been stored in salt water or, to the best
knowledge of plant personnel, treated with pentactilorophenol (PCP). -•
Approximately 120 digester batches per day are processed in the 17 digesters
at the pulping plant. Each batch consists of 64 Mg (70 tons) of wood chips,
34 to 54 cubic meters (1200 to 1900 cuft) of white liquor, and a small amount
of weak black liquor.
The contents of the finished digester batches are sent to a "blow tank"
for intermittent storage and then to a countercurrent "brown stock washer"
system. Pulp is separated from the rest of the finished digester batch in the
brown stock washers. Dirty water from the brown stock washers (i.e., weak
black liquor) is sent to an evaporator system for solids concentration prior
to being fired in the black liquor boiler.
Cleaned pulp from the brown stock washer is bleached, pressed, and
spooled for off-site production into a variety of paper products. Bleaching
is performed using chlorine dioxide (C102), which is produced on-site using
the R2 and R3 processes. Neutralized spent acid (predominately sodium
sulfate).from the R2 process is fed to the black liquor circuit at the rate of
38 cubic meters (1340 cu ft) per day. Approximately 36 Mg/day (40 TPD) of
by-product salt cake from the R3 process is also fed to the black liquor
circuit. These two by-product or waste streams provide make-up sodium and
sulfur for the pulping process.
3-1
-------
3.2 BLACK LIQUOR RECOVERY BOILER DESCRIPTION
Black liquor recovery boiler BLB-B is a Combustion Engineering recovery
boiler with a rated capacity of 725 Mg/day (800 TPD) unbleached pulp. The
boiler, which was installed in 1962, is typically base loaded and operates at
a steady black liquor firing rate.
The solids content of the concentrated black liquor fired in Boiler BLB-B
is approximately 70 percent by weight. Concentration of the weak black liquor
produced by the brown stock washers is accomplished using a four-stage
multiple effect evaporator system and cascade direct contact evaporators.
Particulate matter from combustion of the black liquor is collected dry in an
electrostatic precipatator. The dry precipitator catch and fresh make-up salt
cake are mixed with the strong black liquor before the liquor is fired in the
boiler.
The chloride content of the concentrated black liquor fed to boiler BLB-B
is typically .53% on a dry basis. The majority of chlorine entering the black
liquor circuit comes from one of three sources: the neutralized spent acid
(R2), the by-product saltcake (R3), and well water used for process make-up.
Chlorine contents arid flow rates for these three streams and for the weak
black liquor, strong black liquor and white liquor are shown in Table 3-1.
Other potential sources of chlorine entering the black liquor circuit include
small amounts of calcined lime (CaO) used in converting green liquor to white
liquor, fresh makeup saltcake (Na2 S04) added to the strong black liquor, and
wood chips fed to the process.
Concentrated black liquor is sprayed into the combustion zone of boiler
BLB-B at a temperature of approximately 127°C (260°F) using four oscillating
"guns". Primary and secondary combustion air are suppled to the boiler by
forced draft fans. The primary: secondary air ratio is approximately 0.8:1.
The combustion air supply is computer controlled using flue gas oxygen
monitoring and black liquor feed rate monitoring. Oxygen is continuously
monitored at the economizer section of the boiler.
a*
3.3 ELECTROSTATIC PRECIPITATOR DESCRIPTION
Exhaust gases from black liquor recovery boiler BLB-B pass through a
two-chamber Flakt electrostatic precipitator (ESP) for particulate removal.
3-2
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3-3
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Particulate matter is removed from the ESP hopper by drag and screw type
conveyors. Participate matter is recycled directly back into the pulping
liquor circuit (resulting in an inaccessible sampling location). Each chamber
of the ESP handles approximately half of the total boiler exhaust gas of
290,000 acfm at 330 F. The ESP has a design specific collection area of 0.4
ft2/acfm and a design particulate removal efficiency of 99.6 percent.
3-4
-------
4.0 TEST DESCRIPTION
This section describes the field sampling, process monitoring, and
analytical activities that were performed for test Site BLB-B. The purpose of
the section is to provide sufficient descriptive information about the test so
that the test results presented in Section 5.0 can be easily understood.
Descriptions of the sampling locations and sampling procedures are presented
in Section 6.0.
The remainder of 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 test Site
BLB-B. Three dioxin/furan emissions tests (Runs 01, 02, 03) were performed
simultaneously at the electrostatic precipitator inlet location and the
electrostatic precipitator outlet exhaust stack. These locations are shown as
Points D and E on Figure 4-1. Dioxin/furan sampling followed the Modified
Method 5 (MM5) sampling protocol developed by the American Society of
Mechanical Engineers (ASME) for measuring emissions of chlorinated organic
compounds with two minor modifications (see section 6.1.2.1 for details).
Testing was performed at the electrostatic precipitator outlet exhaust stack
for a period corresponding to 240 minutes of on-line sampling. Testing was
performed during the same time period at the electrostatic precipitator inlet
location. The on-line sampling period was from 160 to 200 minutes. The
recovery boiler flue gas is divided between two identical, parallel direct
contact evaporator-ESP systems. Dioxin/furan tests were performed only on the
South Inlet Duct. The two ESP inlet ducts were physically separated so that
both ducts could not be tested using the same sampling train. Additional
personnel and equipment would have been required to sample at both ESP inlet
streams. Since the direct contact evaporators contact the same gas stream
with the same black liquor stream, and the two ESP sections are identical, the
dioxin/furan content should be similar in each ESP inlet stream. In order to
4-1
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demonstrate that the parallel direct contact evaporators were operating
similarly, the flue fas temperature and gas velocity were measured at the
North Inlet Duct during each test run.
Concentrations of HC1 in the flue gas were determined for each test day
at the electrostatic precipitator outlet exhaust stack using another
modification of EPA Method 5. The sampling train was identical to that of
Method 5 except that water in the impingers was replaced with 0.1 M KOH. The
impinger solution was changed to potassium hydroxide at the suggestion of the
National Council for Air and Stream Improvement (NCASI). The substitution of
KOH in the impinger was performed in an effort to eliminate sodium chloride
(NaCl) interferences in the HC1 measurement (to avoid overestimating chloride
content).
Continuous emissions monitoring (CEM) of 02, CO, C02, S02, NOX, and total
hydrocarbons (THC) was performed during the three MM5 test runs. These data
were obtained to assess variations in combustion conditions during the
sampling periods. Instantaneous concentration values for each species
monitored were recorded every five minutes by the CEM data system.
Six types of process samples were taken during the MM5 test periods:
strong black liquor, white liquor, weak black liquor, R2 C102 generator spent
acid, well water, and R3 C102 generator by-product saltcake. The strong black
liquor samples were taken to characterize dioxin-furan and dioxin/furan
precursor contents of the material fed to the boiler. Three identical
composites of hourly strong black liquor samples were prepared: one for
dioxin/furan analysis by Troika, one for dioxin/furan precursor analysis by
Radian/RTP, and one for total chloride analysis by'Research Triangle
Institute. The white liquor, weak black liquor, well water and C102 generator
spent acid and by-product saltcake samples were taken to indicate the major
contributors of chloride to the mill liquor circuit. These samples were taken
twice during each test day, and a single sample composite for each test run
was sent to Radian/Austin for total chloride analysis.
Soil samples were collected from ten locations at the plant site. The
ten samples were combined into a single composite, which was held for
potential dioxin/furan analysis pending evaluation of the MM5 dioxin/furan
emissions data.
4-5
-------
4.2 PROCESS DATA COLLECTION
Process data were collected to characterize the operation of the black
liquor boiler and electrostatic precipitator during the MM5 test periods. A
copy of the daily status report for the recovery boiler system was provided by
the host site. This report includes an hourly listing of the recovery furnace
operating variables. These variables include black liquor characteristics
furnace drafts and air flow furnace and ESP temperatures steam flow, and flue
gas and green liquor compositions. Electrostatic precipitator voltage and
current data were recorded manually at intermittent times throughout the test
period. The process data will be used in Section 5.1 with the CEM data to
evaluate and compare combustion conditions during the three MM5 test periods.
4.3 LABORATORY ANALYSES
Laboratory analyses performed on samples from test Site 05 included
dioxin/furan analyses, dioxin/furan precursor analyses and total chloride
analyses. Samples analyzed for dioxin/furan are discussed in Section 4.3.1
and samples analyzed for dioxin precursors are discussed in Section 4.3.2.
Samples analyzed for chloride are discussed in Section 4.3.3.
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, two of three EPA laboratories collectively
referred to as Troika.
Dioxin/furan analyses were performed by gas chromatography/mass
spectroscopy. Specific isomers identified included 2378 TCDD and 2378 TCDF.
Other dioxin/furan compounds were quantified in groups according to the number
of chlorine atoms per molecule. The tetra-through octa-chlorinated homologues
were quantified.
4.3.2 Dioxin/Furan Precursor Analysis
Dioxin/furan precursor analyses of strong black liquor samples were
performed by Radian using gas chromatography/mass spectroscopy. The specific
dioxin/furan precursors to be analyzed for included chlorophenols,
chlorobenzenes, and PCB's. Composite feed samples were also analyzed for
4-6
-------
total chlorine by Parr Bomb combustion followed by ion chromatography and for
total organic halide-by gas chromatography and Hall detector
4.3.3 Total Chloride Analysis
Chloride analysis was performed on the combined probe rinse/filter sample
and on the back half-rinse/impinger solution sample for each HC1 train (i.e.,
front half and back half analysis). Chloride analysis only was also performed
on the strong black liquor, white liquor, weak black liquor, by-product
saltcake, neutralized spent acid, and the make-up water (well-water) by
Radian/Austin.
4-7
-------
-------
5.0- TEST RESULTS
The results of the Tier 4 dioxin/furan emissions test of black liquor
boiler BLB-B are presented in this section. The individual test runs are
designated as Runs 1-3.
Process data obtained during the test runs are presented in Section 5.1,
and continuous monitoring results for 0-, CO, CCL, NO , SO-, and THC are
presented in Section 5.2. The dioxin/furan emissions data are contained in
Section 5.3. Results of HC1 train sampling at the precipitator outlet and
chlorine analysis of various process samples are presented in Section 5.4.
Strong black liquor dioxin/furan analysis and dioxin/furan precursor analysis
are presented in Section 5.5.
5.1 PROCESS DATA
Process data were obtained to document black liquor boiler and
electrostatic precipitator operation during the test runs . The boiler
operating data are summarized in Section 5.1.1, and the electrostatic
precipitator operating data are summarized in Section 5.1.2.
5.1.1 Black Liquor Boiler Operating Data
Plant-maintained data summarizing the mean operating conditions of black
liquor boiler BLB-B during the three MM5 test runs are shown in Table 5-1.
Hourly data for boiler load, flue gas oxygen content in the economizer section
of the boiler, strong black liquor solids flow, and primary and secondary, air
flow are shown for each test run in Figures 5-1, 5-2 and 5-3. The data show
that the boiler was operated similarly during the individual test runs with
the exception of a slightly lower flue gas oxygen content for Run 2 compared
to Runs 1 and 3. There were no process upsets during any of the runs that
resulted in sampling interruptions.
5.1.2 Electrostatic Precipitator Operating Data
Electrostatic precipitator operating data maintained by the host plant
are summarized in Table 5-2 for test runs 1, 2, and 3. The data show similar
5-1
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Figure 5-1. Hourly Boiler Operating Data for Run 1.
5-3
-------
20Or
Black Liquor
SoNdaHow
(100O Ib/hr)
Bofter Load
(10OO t>/hr
Steam)
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Local Time
Teat
End
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Local Time
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nd
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Figure 5-2. Hourly Boiler Operating Data for Run 2.
5-4
-------
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Stock Liquor -
SofcteFtow
(1000 fc/hr)
100
Bo tor Load
(1OOOt>/hr
Steam)
300
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oa
Test
Start
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(% by Voknw)
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Flgur* 5-3. Hourly 8oil«r Operating Data for Run 3.
5-5
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5-6
-------
ESP operation during the three runs, with the exception of some variability in
the south ESP compartment power consumption.
5.2 FLUE GAS PARAMETER DATA
Table 5-3 summarizes flue gas temperature, moisture, volumetric flowrate,
and oxygen concentration data obtained at Site BLB-B. These parameters were
fairly consistent among test runs. The average flue gas temperature and
moisture content measured at the ESP inlet and outlet were 164°C, 32.4%, and
157°C, 32.0%, respectively. The average gas flowrates for the ESP inlet and
outlet under actual stack temperature and moisture conditions were 8,200
(287,300 ascf) and 8,100 (282,500 ascf) acmm, respectively. The average dry
standard flowrate was 3,700 dscmm (129,500 dscfm) for the inlet and 3,800
dscmm (132,100 dscfm) for the outlet. Standard EPA conditions are 20°C (68°F)
and 1 atm.
5.3 CONTINUOUS EMISSIONS MONITORING DATA
The continuous emissions monitoring system that was used to measure the
combustion products in the black liquor flue gas did not operate in a fully
successful manner during this test. A significant difference was observed
between the oxygen value reported by the CEM system and the values reported by
the plant 02 analyzer and the Reference Method 3 tests. The average results
reported by the three measurements are summarized in Table 5-4. As can be
observed, the C*EM system reported consistently high results.
The oxygen concentration measured by the Radian CEM system ranged from
10.9 to 13.1 percent by volume. The values reported by the host site
instruments (Table 5-l)were about 2.3% by volume. The EPA Method 3 results
for samples collected at the ESP,Inlet ranged from 3.9 to 5.2 percent. The
cause for the difference in results was a leak in the pump in the gas
conditioning system that could not be repaired in the field. Because of the
leak, the results cannot be used for direct comparison of combustion
conditions. However, the oxygen results can be used to normalize the CO, CCL,
NOX and S02 results to the 3% 02 basis that has been selected for the Tier 4
5-7
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5-8
-------
TABLE 5-4. SUMMARY OF OXYGEN AND CARBON DIOXIDE RESULTS
ESP Inlet
Method 3
Run No. y n 0/rn
7o Up /oLU«
1 3.9 16.3
2 4.7 15.1
3 5.2 15.1
ESP Outlet
Method 3
V A
/, o2
5.9
5.4
5.3
%co2
14.1
14.6
15.3
CEM System Plant 0?
02 Analyzer
o/ f\ ot r\
A U2 A U2
13.1 3.6
12.7 2.4
10.9 3.2
Notes: 1. Volume % concentration on a dry basis
2. Plant 02 results adjusted to dry basis using 25% H20.
5-9
-------
data base. The leak was equivalent to dilution with clean ambient air, which
can be confirmed using the carbon dioxide results. For a combustion process
that uses air as the source of combustion oxygen, the relationship between the
oxygen and carbon dioxide concentration in the flue gas is linear. The oxygen
and carbon dioxide results from the Method 3 tests and the CEM system are
plotted in Figure 5-4. The average CEM result (normalized to 3% 02 and "as
measured") and random, individual data points are presented in the plot.
Although there is some scatter in the results, a linear relationship is
confirmed. This linear relationship demonstrates that simple dilution was
occuring and that there were no secondary calibration errors. Therefore, the
species measurements normalized to 3% 02 are valid and can be used to compare
combustion conditions among test runs for C02, CO, S02, and NOX.
The total hydrocarbon sample was collected through a separate sample line
and pump system and leakage did not occur in this system. The flue gas oxygen
concentration measured by the host site was essentially 3% on a dry basis,
thus the THC results as measured are essentially on the same basis as the
other species normalized to 3% CL.
The mean value and standard deviation of the gas concentration for each
of the species that was measured continuously at the recovery boiler outlet
are presented in Table 5-5. A complete listing of the CEM data is included in
Appendix A-2. A dilution correction for oxygen concentration cannot be
calculated because there is no independent basis for computing an adjustment
factor. However, the results as measured can be used to indicate the relative
variation between runs.
The average oxygen concentration for Runs 1-3 ranged from 10.9 to 13.1
volume percent, dry basis with an average result of 12.2 percent. The
concentrations are plotted versus test time in Figure 5-5. The oxygen
measurements were relatively stable during each test run, and did not change
significantly between runs. As discussed previously, the reported oxygen
results are biased high, and are presented only to show the relative variation
with time.
The carbon dioxide results are plotted versus time in Figure 5-6. The
average carbon dioxide concentration on a dry basis, adjusted to 3% 02, ranged
5-10
-------
30-
(0
X
O
25-
20-
15-
10-
0 ESP Inlet, Method 3
Q ESP Outlet, Method 3
Average GEM Result
<§>3% O2
Uncorreeted Average
GEM Result
5-
25
% CO2 in Flue Oas
Figure 5-4. Volume Percent Oxygen Versus Volume Percent CO2
in the Flue Gases, Site O5.
5-11
-------
TABLE 5-5. MEAN VALUES AND STANDARD DEVIATIONS OF CONTINUOUSLY
MON.ITORED COMBUSTION GASES AT THE RECOVERY BOILER OUTLET
Species
Run 01
Average Concentration
(Standard deviation)
Run 02 Run 03
Average
02 (% vol , dry)
CO (ppmv @ 3% 02, dry)
C02 (% vol @ 3% 0£, dry)
S02 (ppmv @ 3% 02, dry)
NOX (ppmv @ 3% 02, dry)
THC (ppmv as propane
as measured, wet)
13.1
(1.4)
10607.8
(2357.8)
17.0
(1.2)
948.6
(272.8)
41.6
(15.7)
66.9
(43.7)
12.7
(0.4)
12926.0
(1918.8)
19.2
(0.9)
976.8
(264.6)
42.3
(11.2)
59.2
(27.8)
10.9
(0.5)
9210.4
(2795.7)
16.1
(2.4)
565.3
(143.9)
44.0
(9.1)
46.9
(46.8)
12.2
10,900
17.4
830
42.6
57.7
NOTES: 1. The mean concentration is presented as the upper entry, and the
standard deviation is presented in parenthesis.
2. The THC sample was collected through a separate sample line/pump
system and was not corrected for leakage on the same basis as the
other measured species.
5-12
-------
SITE 05 — TEST 1
HE AN: IZ. 17. 02
3TO. CSV.: 1.4V.
INSTRUMENT RANGEi a-23V. 02
TOT TIMC (nouns)
SITE 05 - TEST 2
•nem.c
neont
STO. O
12. 7X 02
a.«y.
RANGE: 3-:3V. 02
TCIT TIMC (wouits)
SITE 05 - TEST 3
nCANt ia.=>v. 02
STO. oev.i a.3%
INSTRunENT RANGEi a-2SX 02
TEST TIMC (HOURS)
Figure 5-5. Oxygen Concentration Versus Test Time,
Site OS.
5-13
-------
SITE 05 - TEST 1
oiowot f*ar\\JL
MEANi 17.3?. C02
STO. 06V.! 1.2V.
INSTmjP€NT RONQEl 3-IB'/. C02
TOT T1MC (HOUNS)
SITE 05 - TEST 2.
OAION oioxioe »i«sini.e
3* -
31-
33-
3O-
nEANl If. IX C02
STO. DEV. I a. 9%
INSTRUFiENr RANOCt a-IOX C02
TOT TIMC
SITE 05 - TEST 3
so-
31-
II -
34-
22-
3O -
13-
10-
nEANi 14. IV. C02
iTO. 06V.i 2.4X
[NSTRUFIENT SflfJGEl a-2»X CQ2
Terr TIMC (nouns)
Figure 5-6.
Carbon Dioxide Concentration Versus
Test Time, Site 05.
5-14
-------
from 16.1 to 19.2 volume percent. The factor that is used to normalize the
results to a 3% 02 basis is:
20.9 - 3% 0,
correction factor
20.9 - measured % 0,
This factor was calculated for each 5 minute average data point.
The carbon dioxide results are relatively stable except for a short
period in Run 3 where there were two outlying data points. The points
(identified as 1400 and 1415) were plotted on Figure 5-4 to test the validity
of the values. The two points are significantly displaced from the
theoretical CO- vs. 0- line. This suggests that the cause for the low results
is not combustion related, but due to some other reason. A possible
explanation is that the two low data points are averages that were measured
during a gas conditioner cleaning cycle or, when the probe was removed from
the flue to collect a bag sample. The response time of the 02 analyzer is
significantly longer than the C02 analyzer, and the two averages could be a
result of the 02 analyzer not seeing the same sample as the C02 analyzer
during a blowback period. Because of this uncertainty, the two low CCL
concentrations will not be treated as a real occurrence.
The carbon monoxide and total hydrocarbon results are presented
graphically in Figures 5-7 and 5-8 respectively. The total hydrocarbon
results are presented on an as-measured basis since the THC sample was
collected through a separate pump system. Dilution by leakage did not occur
in the THC sample. There was a relatively large variation in the
concentration of carbon monoxide and total hydrocarbons during each run, but
the averages between runs was similar. Also the CO and THC variations tend to
track each other, as would be expected. The average results for CO and THC
are not directly proportional for all three test runs. However, this is
probably due to the absence of about 1 1/2 hours of THC data during Run 1.
The sulfur dioxide concentration results for each run are presented in
Figure 5-9. The average S02 concentration was essentially the same for Runs 1
and 2, (949 and 977 ppm by volume dry at 3% 02), but was significantly less
5-15
-------
SITE 05 - TEST 1
MONOXIQC
B
M;
a
R
52!
13607.3 ogmv CO
STO. osv. i :T37.a OB'"*
INSTRUnENT RftNGEl 3-4303 gamv CO
SITE 05 - TEST 2
: »«orn.e
nEANl 11926.3 PD«V CO
STO. OEV.: 1919.9 PQAV
INSTRUMENT RONGEl 3-6329 DP«v CO
TOT TIMC (Mourn)
SITE 05 - TEST 3
MONOXIQC rn.t
nEANl •'213. « g0mv CO
STO. 06V.I 2793.7 ooi«v
INSTRUMENT RflNGEl 3-6309 gomv CO
TOT TIUC
-------
SITE 5 - TEST 1
i \
JB,V-!|
Mean: 66.9 ppmv THC
Std. Oev.: 43.7 ppmv
Instrument Range: 0-500 ppm THC
SITE 5 - TEST 2
ret*!. mmc&mH B»or«.c
Mean: 59.2 ppmv THC
Std. Oev.: 27.8 ppmv
Instrument Range: 0-500 ppm THC
TEST TIMC ONOU«>
SITE 5 - TEST 3
amom.lt
i
J^" ? rKi '
^""' \*\ ,<*~\.^
I »r JJ. • a
\
\
". «jrVV
*~ \**
Mean: 46.9 ppmv THC
Std. Oev.: 46.3 ppmv
Instrument Range: 0-500 ppm THC
Figure 5-8. TotaS Hydrocarbon Concentration Versus
Test Time, Site OS.
5-17
-------
-SITE 05 - TEST 1
QIOXIOC
nEANi 948.6 ooi"v 302
STO. OEV.t 27C.S ooniv
INSTRUFCNT RANGEI 3-1338 oomv SOI
rar nuc (HOURS)
SITE 05 - TEST 2
*76.a BP«lv S02
STO. SEV.t 36«.6 opmv
INSTFHj-ENT RANQEl a-l88« op»v 302
TOT Time (HOURS)
SITE 05 - TEST 3
autnjR oioxiot RROFILC
SC. 'J-
MEAN!
STO. 06V.I
363.1 ppmv S02
143.9 gonv
a-lSOO ppmv 302
rar nuc (HOURS)
Figure 5-9.
Sulfur Dioxide Concentration Versus
Test Time, Site 05.
5-18
-------
during Run 3 (565 ppmv). The reason for the reduced SO* emission is not
apparent from the recorded process data.
The NO results are presented in Figure 5-10. For all three runs, the NO
A A
concentration was steady and essentially the same value of 42-44 ppm by
volume, dry at 3% 02.
5.4 DIOXIN/FURAN EMISSIONS DATA
5.4.1 Isomer and Homoloque Specific Data at the ESP Inlet
Tables 5-6 and 5-7 present emission concentrations and emissions rate
data measured at the electrostatic precipitator inlet for the 2378 TCDD,
isomer and total PCDD and total PCDF homologues. The data include dioxin and
furan collection in the entire MM5 train, including filter, XAD sorbent trap,
impingers, and sample train clean-up rinses.
/
Average as-measured emissions concentrations of total PCDD, and PCDF
species were not-detected 2378 TCDD; 15.1 ng/dscm total PCDD; and .93 ng/dscm
total PCDF. When corrected to 3% 02 using the EPA Method 3 oxygen
concentration data, these values correspond to 17.1 ng/dscm @ 3% 02; and 1.07
ng/dscm @ 3% 02, respectively. Average emission rates for the three species
were 0.003 g/hr total PCDD, and 0.0002 g/hr total PCDF. Emissions of 2378 .
TCDD were consistently not detected for any of the runs. The total PCDD and
PCDF emissions were much less consistent between runs which indicates
significant variability. The maximum deviation of any individual run from the
overall average was approximately 94 percent for total PCDD emissions and 70
percent for total PCDF emissions.
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/dscm and parts-per-
trillion units and homologue emission rates in ug/hr units are included in
Appendix D. Detectable quantities were found for roughly two-thirds of the
isomers and homologues analyzed for at the electrostatic precipitator inlet of
Site BLB-B. Figure 5-11 is a histogram that shows the relative distributions
of the 2378 TCDD/TCDF isomers and the tetra-through octa PCDD/PCDF homologues
in the inlet electrostatic precipitator emissions (mole basis). The
5-19
-------
SITE 05 - TEST 1
oxioes or xmeoeN a«oni.g
I
S soo-t-
rar TIMC (HOURS)
nEANt «t.6 ppmv HOx
STO. OEV. i 13.7 oomv
[NSTRUMENT RflNSEl
SITE 05 - TEST 2
OXTOCI of MimootN »xoni.e
a * . •
TOT Tiue (HOURS)
MCANl 42.3 OP«v N0»
STO. DEV.I 1t.2 ppnv
tNSTRUnEMT RONSgl 8-3B9 pp«v NO»
SITE 05 - TEST 3
OX1QC3 Of MITHOaOt "ROItt
T8ST TIMC (MOUIW)
FIEAMt 44.3 po«v HO*
STO. OEV.l 9.I apnv
INSTBUnENT KANGEt 3-39* ppnv NOx
Figure 5-1O. Nitrogen Oxides Concentration Versus
Test Time, Site 05.
5-20
-------
Table 5-6. Overview of Dioxin/Furan Emissions Concentration Data
for Site BLB-B (Electrostatic Precipitator Inlet)
Run Number
2378 TCDD
Total PCDD Total PCDF
Emissions Concentration
(as .measured), ng/dscm
Run 01
Run 02
Run 03
Average
ND
NO
ND
.88
3.1
41.3
15.1
.26
.69
1.84
.93
Emissions Rate Concentration
(corrected to 3% 02), ng/dscm
3%
Run 01
Run 02
Run 03
Average
ND
ND
ND
— •
.92
3.37
47.0
17.1
.28
.77
2.10
1.07
ND = Not Detected
5-21
-------
Table 5-7. Summary of Dioxin and Furan Emissions Rate Data
for Site BLB-B (Electrostatic Precipitator Inlet)
Dioxin/Furan Emission Rate, uq/hr
Run Number
Run 01
Run 02
Run 03
Average
2378 TCDD
ND
NO
ND
--
Total PCDD
193
687
9270
3383
Total PCDF
58
156
413
209
ND » Not Detected
5-22
-------
TABLE 5-8. SUMMARY OF DIOXIN/FURAN EMISSIONS DATA FOR SITE BLB-B INLET
(As-Measured Concentrations)
Dioxin/Furan
Isomer
Isomer Concentration in Flue Gas
(ng/dscm)
Run 01 Run 02 Run 03
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( 3.95E-02)
ND( 3.95E-02)
ND( 3.95E-02)
ND( 3.95E-02)
1.75E-01
7.02E-01
8.77E-01
•
4.39E-02
4.39E-02
ND( 1.05E-01)
8.77E-02
4.39E-02
4.39E-02
2.63E-01
ND 6.25E-02)
ND 6.25E-02)
ND 6.94E-03)
ND( 8.68E-02)
7.29E-01
2.33E+00
3.06E+00
ND( 6.25E-02)
ND( 6.25E-02)
ND( 3.47E-02)
1.04E-01
3.47E-01
« 2.43E-01
6.94E-01
ND( 2.43E-02)
ND( 2.43E-02)
ND( 8.68E-02)
2.08E-01
6.81E+00
3.42E+01
4.13E+01
6.94E-02
4.51E-01
ND( 8.68E-02)
2.43E-01
6.25E-01
4.51E-01
1.84E+00
.OOE+00
.OOE+00
.OOE+00
6.94E-02
2.57E+00
1.24E+01
1.51E+01
3.78E-02
1.65E-01
.OOE+00
1.45E-01
3.39E-01
2.46E-01
9.33E-01
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
5-23
-------
TABLE 5-9. ' SUMMARY OF DIOXIN/FURAN EMISSIONS DATA FOR SITE BLB-B INLET
JConcentrations Corrected to 3% Oxygen)
Dioxin/Furan
Isomer
Isomer Concentration in Flue Gas
(ng/dscm @ 3% oxygen)
Run 01 Run 02 Run 03
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
Avg.
DIOXINS
2378 TCDD ND
Other TCDD ND
Penta-CDD ND
Hexa-CDD ND
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF ND
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
4.15E-02)
4.15E-02)
4.15E-02)
4.15E-02)
1.84E-01
7.37E-01
9.22E-01
4.61E-02
4.61E-02
( 1.11E-01)
9.22E-02
4.61E-02
4.61E-02
2.77E-01
ND( 6.90E-02)
ND( 6.90E-02)
ND( 7.67E-03)
ND( 9.59E-02)
8.05E-01
2.57E+00
3.37E+00
ND( 6.90E-02)
ND( 6.90E-02)
ND( 3.83E-02)
1.15E-01
3.83E-01
2.68E-01
7.67E-01
ND( 2.77E-02)
ND( 2.77E-02)
ND( 9.89E-02)
2.37E-01
7.75E+00
3.90E+01
4.70E+01
7.91E-02
5.14E-01
ND( 9.89E-02)
2.77E-01
7.12E-01
5.14E-01
2.10E+00
.OOE+00
.OOE+00
.OOE+00
7.91E-02
2.91E+00
1.41E+01
1.71E+01
4.17E-02
1.87E-01
.OOE+00
1.61E-01
3.81E-01
2.76E-01
1.05E+00
5-24
-------
o
Ui
DIOXIN MONOLOGUES AT THE INLET
1
~
0.9 -
o.a -
0.7 -
o.s -
0.5 -
O.4. -
0.3 -
0.2 -
O.I -
8L8-B
V/
2378 TCDD Qi^mr TCOD »«nte-CDD H«xa-COD Hapla-CDO Qata-COD
DICXIN HQMCLOGUE
ITT! RUN O1 g??vl RUN O2 P£%] RUN O3
FURAN HCMOLOGUES AT THE INLET
9L3-3
237B TCDF O*h«r TCOF P«o«a-CDF Huxa-CDF H«p-Na-CDF Oaia-CDF
FURAH HOMOLOGUC '
RUN O1 &77X RUN O2 IX?3 RUN O3
FIGURE 5-11. DIOXIN AND FURAN HOMOLOGUE DISTRIBUTIONS OF THE ELECTRO-
STATIC PRECIPITATOR INLET EMISSIONS FOR SITE BLB-B
5-25
-------
distribution of dioxin species was extremely non-uniform among the various
homologues. Only the hepta- and octa- CDD homologues were detectable in the
electrostatic precipitator inlet emissions. The octa-CDD homologue accounted
for roughly 80 percent of the total dioxins found. The hepta-CDD homologues
accounted for the remaining 20 percent of the total dioxins found in the
electrostatic precipitator inlet emissions. The furan species were more
uniformly distributed than the dioxin species, with the hepta-CDF homologue
being the largest single contributor to the total PCDF emissions. The
contributions of the tetra- through octa-chlorinated furan homologues to the
total PCDF were: tetra, 0-49%; penta, 0%; hexa, 12-28%, hepta, 13-50%, and
octa, 11-33%.
Emission factors based on black liquor dry solids feed rate for the
electrostatic precipitator inlet at site BLB-B are shown in Table 5-10.
Average emission factors for 2378 TCDD, total PCDD, and total PCDF were 0 g
2378 TCDD emitted per Kg feed; .06 ug total PCDD emitted per Kg feed; and .004
ug total PCDF emitted per Kg feed. Emission factors for the various dioxin
and furan homologues varied considerably between test runs.
5.4.2 Isomer and Homoloque Specific Data at the ESP Outlet
Emission concentrations and emissions rate data measured at the
electrostatic precipitator outlet are shown in Tables 5-11 and 5-12 for the
2378 TCDD, total PCDD, and total PCDF species. The data include dioxin and
furan collection in the entire MM5 train, including filter, primary XAD
sorbent trap, impingers, and sample train clean-up rinses.
Average as-measured emissions concentrations of the 2378 TCDD, total
PCDD, and PCDF species were 1.02 ng/dscm total PCDD; and .60 ng/dscm total
PCDF. When corrected to 3% 02 using the EPA Method 3 oxygen concentration
data, these values correspond to 1.19 ng/dscm 9 3% 02; and .71 ng/dscm @ 3%
02, respectively. Average emission rates for the three species were 0.0002
g/hr total PCDD, and 0.0001 g/hr total PCDF. Emissions of 2378 TCDD were
non-detectable for all three runs. The total PCDD emissions were consistent
for runs 2 and 3; however, run 1 emissions were a factor of 2 greater for
total PCDD. PCDF emissions were less consistent between runs which indicates
considerable variability. The maximum deviation of any individual run from
5-26
-------
TABLE 5-10. DIOXIN/FURAN EMISSION FACTORS FOR SITE BL8-B INLET
Dioxin/Furan
Isomer
Dioxin/Furan Emission Factors (ug/kg)
Run 01 Run 02 Run 03
ND = 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( 1.53E-04)
ND( 1.53E-04)
ND( 1.53E-04)
ND( 1.53E-04)
6.81E-04
2.72E-03
3.40E-03
1.70E-04
1.70E-04
ND( 4.09E-04)
3.40E-04
1.70E-04
1.70E-04
1.02E-03
ND( 2.47E-04)
ND( 2.47E-04)
ND( 2.74E-05)
ND( 3.43E-04)
2.88E-03
9.19E-03
1.21E-02
ND( 2.47E-04)
ND( 2.47E-04)
ND( 1.37E-04)
4.11E-04
1.37E-03
9.60E-04
2.74E-03
ND( 9.60E-05)
ND( 9.60E-05)
ND( 3.43E-04)
8.23E-04
2.69E-02
1.35E-01
1.63E-01
2.74E-04
1.78E-03
ND( 3.43E-04)
9.60E-04
2.47E-03
1.78E-03
7.27E-03
.OOE+00
.OOE+00
.OOE+00
2.74E-04
1.01E-02
4.90E-02
5.94E-02
1.48E-04
6.51E-04
.OOE+00
5.70E-04
1.34E-03
9.71E-04
3.68E-03
5-27
-------
Table 5-11.
Overview of Dioxin and Furan Emissions Concentration Data
for Site BLB-B (Electrostatic Precipitator Outlet)
Run Number
2378 TCDD
Total PCDD Total PCDF
Emissions Concentration
(as measured), ng/dscm-
Run 01
Run 02
Run 03
Average
ND
ND
ND
1.58
0.71
0.77
1.02
1.32
.12
.36
.60
Emissions Rate Concentration
(corrected to 3% 02), ng/dscm Q 3% 02
Run 01
Run 02
Run 03
Average
ND
ND
ND
•• •"
1.88
.81
.90
1.19
1.57
0.14
.42
.71
ND - Not Detected
5-28
-------
Table 5-12— Summary of Dioxin and Furan Emissions Rate Data
for Site BLB-B (Electrostatic Precipitator Outlet)
Dioxin/Furan Emission Rate, ua/hr
Run Number
Run 01
Run 02
Run 03
Average
2378 TCDD
NO
NO
NO
--
Total PCDD
355
156
179
230
Total PCDF
296
26.1
84.4
136
NO - Not Detected
5-29
-------
the overall average was approximately 35 percent for total PCDD emissions and
80 percent for total-PCDF emissions. Therefore, the between run variability
is within the range expected given the analytical uncertainty.
Isomer- and homologue specific emission concentration data are summarized
in Tables 5-13 and 5-14 for the three test runs. Run-specific data tables
showing homologue emission concentrations in both ng/dscm and
parts-per-trillion units and homologue emission rates in ug/hr units are
included in Appendix D. Figure 5-12 is a histogram that shows the relative
distributions of the 2378 TCDD/TCDF isomers and the tetra- through octa
PCDD/PCDF homologues in the electrostatic precipitator outlet emissions (mole
fraction basis). The distribution of dioxin species was non-uniform among the
various homologues. Only the hexa, hepta, and octa-CDD homologues were
detectable in the electrostatic precipitator outlet emissions. The octa-CDD
homologue accounted for roughly 70 percent of the total dioxins found. The
contributions (on a mole-basis) of the hexa- and hepta-CDD dioxin homologue to
the total TCDD were: hexa, 0-13%; and hepta, 20-25%. The total PCDD and PCDF
emissions were more evenly distributed than the dioxin species with the
contributions of the tetra- through octa-chlorinated furan homologues to the
total PCDF as follows: tetra, 10-35%; penta, 0%; hexa, 0-53%; hepta, 18-62%;
and octa, 5-38%.
Emission factors for the electrostatic precipitator outlet at site BLB-B
are shown in Table 5-15. Average emission factors for 2378 TCDD and total
PCDD, and total PCDF were 0.004 ug total PCDD emitted per Kg feed; 0.002 ug
total PCDF emitted per Kg feed. Emission factors for the various dioxin and
furan homologues were fairly consistent between test runs.
5.4.3 Reduction of Dioxin/Furan Concentrations Due to the ESP
The dioxins/furans which condense on parti oil ate in the stack gas are
removed from the stack gas along with the particulate by the pollution control
device (ESP). The dioxin/furan removal efficiency of the control device is
calculated from the difference of the inlet and outlet concentration of each
dioxin/furan homlogue divided by the inlet concentration of each homlogue.
Each value is considered to have an analytical uncertainty of +50%. An
analysis of the uncertainty of the control device efficiency (contained in
5-30
-------
TABLE 5-13. SUMMARY OF DIOXIN/FURAN EMISSIONS DATA FOR SITE BLB-B OUTLET
Dioxin/Furan
Isomer
Isomer Concentration in Flue Gas
(ng/dscm)
Run 01 Run 02 Run 03
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( 3.01E-02)
ND( 3.01E-02)
ND( 4.51E-02)
1.88E-01
3.38E-01
1.05E+00
1.58E+00
ND( 3.76E-02)
2.63E-01
ND( 2.74E-01)
7.14E-01
2.63E-01
7.52E-02
1.32E+00
ND( 1.18E-02)
ND( 1.18E-02)
ND( 3.29E-02)
ND( 8.47E-02)
1.65E-01
5.41E-01
7.06E-01
ND( 4.00E-02)
ND( 4.00E-02)
ND( 3.29E-02)
ND( 1.36E-01)
7.06E-02
4.71E-02
1.18E-01
ND( 2.49E-02)
ND( 2.49E-02)
ND( 1.36E-01)
6.79E-02
1.58E-01
5.43E-01
7.69E-01
2.26E-02
6.79E-02
ND( 1.36E-01)
1.36E-01
9.05E-02
4.52E-02
3.62E-01
.OOE+00
.OOE+00
.OOE+00
8.53E-02
2.20E-01
7.12E-01
1.02E+00
7.54E-03
1.10E-01
.OOE+00
2.83E-01
1.41E-01
5.58E-02
5.98E-01
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
5-31
-------
TABLE 5-14.
SUMMARY OF DIOXIN/FURAN EMISSIONS DATA FOR SITE BLB-B OUTLET
(.Concentrations Corrected to 3% Oxygen)
Dioxin/Furan
Isomer
Isomer Concentration in Flue Gas
(ng/dscm @ 3% oxygen)
Run 01 Run 02 Run 03
NOTE: Isomer concentrations shown are corrected to 3% oxygen.
NO = not detected (detection limit in parentheses).
ng - 1.0E-09g
8760 operating hours per year
Avg.
DIOXINS
2378 TCDD
Other TCDD
Penta-CDD
Hexa-CDO
Hepta-CDD
Octa-CDD
Total PCDD
FURANS
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
ND( 3.59E-02)
ND( 3.59E-02)
ND( 5.38E-02)
2.24E-01
4.03E-01
1.25E+00
1.88E+00
ND( 4.48E-02)
3.14E-01
ND( 3.27E-01)
8.51E-01
3.14E-01
8.96E-02
1.57E+00
ND( 1.36E-02)
ND( 1.36E-02)
ND( 3.80E-02)
ND( 9.77E-02)
1.90E-01
6.24E-01
8.14E-01
ND( 4.62E-02)
ND( 4.62E-02)
ND( 3.80E-02)
ND( 1.57E-01)
8.14E-02
5.43E-02
1.36E-01
ND( 2.85E-02)
ND( 2.85E-02)
ND( 1.56E-01)
7.78E-02
1.82E-01
6.23E-01
8.82E-01
2.59E-02
7.78E-02
ND( .1.56E-01)
1.56E-01
1.04E-01
5.19E-02
4.15E-01
.OOE+00
.OOE+00
.OOE+00
1.01E-01
2.58E-01
8.34E-01
1.19E+00
o
8.65E-03
1.31E-01
.OOE+00
3.36E-01
1.66E-01
6.53E-02
7.06E-01
5-32
-------
It.
w
DIOXIN HOMOLOGUES AT THE OUTLET
1
8L8-8
0.9 -
o.a -
O.7 -
o.s -
0.5 -
O..* -
O.3 -
0.2 -
O.I -
2378 TCDD Qihmr TCDD P«nHa-CDD H»«a-CDO H»pia-CDD Oofa-CDD
___ plOXIM MOMOLOGUE
iXXI HUN O1 V77X RUN O2 j^^! RUN O3
Ui
FURAN HOMOLOGUES AT THE OUTLET
3L8-3
O.9 -
O.8 -
O.7 -
O.S -
0.5 -
O.4. -
0.3 -
0.2 -
O.I -
0 -
1
F?l ' /
1
F^
1
/ s
I
1
—r
'%
m
%
\
S3
1
V
F
1
&
2378 TCDF Oih.r TCDF
£VJ RUN 01
Mexd-COF H«pte- CDF Oala—CDF
RUN 03
-IRAN HOMOLOGUC
^ RUN O2
FIGURE 5-12. DIOXIN AND FURAN HOMOLOGUE DISTRIBUTIONS OF THE ELECTRO-
STATIC PRECIPITATOR OUTLET EMISSIONS FOR SITE BLB-B
5-33
-------
TABLE 5-15. DIOXIN/FURAN EMISSION FACTORS FOR SITE BLB-B OUTLET
Dioxin/Furan
Isomer
Dioxin/Furan Emission Factors (ug/kg)
Run 01 Run 02 Run 03
ND - 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( 1.19E-04)
ND( 1.19E-04)
ND( 1.79E-04)
7.46E-04
1.34E-03
4.18E-03
6.27E-03
ND( 1.49E-04)
1.04E-03
ND( 1.09E-03)
2.83E-03
1.04E-03
2.98E-04
5.22E-03
ND( 4.58E-05)
ND( 4.58E-05)
ND( 1.28E-04)
ND( 3.30E-04)
6.42E-04
2.11E-03
2.75E-03
ND( 1.56E-04)
ND( 1.56E-04)
ND( 1.28E-04)
ND( 5.32E-04)
2.75E-04
1.83E-04
4.58E-04
ND( 1.02E-04)
ND( 1.02E-04)
ND( 5.56E-04)
2.78E-04
6.49E-04
2.22E-03
3.15E-03
9.27E-05
3.71E-04
ND( 5.56E-04)
5.56E-04
3.71E-04
1.85E-04
1.58E-03
.OOE+00
.OOE+00
.OOE+00
3.41E-04
8.78E-04
2.84E-03
4.06E-03
3.09E-05
4.72E-04
.OOE+00
1.13E-03
5.63E-04
2.22E-04
2.42E-03
5-34
-------
Appendix L) indicated that with a measured efficiency of greater than 66.7%,
the removal efficiency is most likely positive. With measured efficiencies
between 66.7% and -200%, a definite conclusion cannot be drawn concerning the
true removal efficiency is most likely negative.
The measured ESP removal efficiencies for each dioxin/furan homlogue at
Site BLB-B are summarized in Table 5-16-. In general, the average removal
efficiencies for all homologues indicated positive true removal efficiency for
the ESP. However, some of the homologues had measured removal efficiencies in
the inconclusive range.
5.5 BLACK LIQUOR PRECURSOR DATA
As discussed in Section 4.3.2, the strong black liquor was sampled at
Site BLB-B. These samples were analyzed for chlorinated benzenes, chlorinated
biphenyls, and chlorinated phenols.
Table 5-17 summarizes the results of the compound-specific precursor
analyses. Trace levels of pentachlorophenols were detected for Run 02, but
overall the specific precursors analyzed for (i.e., chlorobenzenes,
chlorophenols, and chlorinated biphenyls) were not detected. The phenol
surrogate recovery data supports the problems (extraction and cleanup
encountered with the dirty field samples (see Table 8-7).
Table 5-18 presents the results of the strong black liquor and weak black
liquor total chloride analyses. The chloride concentration was consistent
among the three test runs. The greatest deviation of any run from the overall
average was 12 percent for the strong black liquor and 6 percent for the weak
black liquor. As seen from Table 5-17, the strong black liquor was about
three times as concentrated as the weak black liquor with respect to total
chloride content. This increase in chloride content follows directly from the
process since the dirty water from the brown stock washers (i.e., weak black
liquor) is sent to an evaporation system for solids concentration prior to
being fired into the boiler.
Total organic halide (TOX) analysis of an hourly composite sample of
black liquor from test Run 01 showed no presence of TOX in the boiler feed.
(Nondetected; Detection Limit). The detection limit of the analysis was
approximately 4 ppm (4 ug/g). The data is inconclusive due to the "dirty"
5-35
-------
TABLE 5-16. ESP REMOVAL EFFICIENCIES AT SITE BLB-B
Homo! ogue
Dloxins
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
ESP
Run 01
-
a
a
a
b
-93.1
-49.6
-80.2
100.0
-497.7
a
-711.4
-497.9
-70.5
-396.2
Removal
Run 02
a
a
a
b
77.4
76.8
76.9
a
a
a
100.0
79.8
80.7
83.1
Efficiency
Run 03
a
a
a
67.3
97.7
98.4
98.1
68.1
84.9
a
44.0
85.6
90.0
80.4
Average
a
a
a
67.3
27.3
41.8
31.6
84.0
-206.4
a
-189.1
-110.8
33.4
-77.6
aNone detected
Efficiency could not be determined; ND at the inlet, concentration
reported at the outlet.
5-36
-------
TABLE 5-17. SUMMARY OF DIOXIN PRECURSOR DATA FOR' SITE BLB-B FEED SAMPLES
Precursor Concentration, ua/a (oom)
Black Liauor Feed
Precursor Categories
Total Chlorinated
Total Chlorinated
Total Chlorinated
Benzenes
Biphenyls
Phenol s*
Run 01
ND
ND
ND
Run 02
ND
ND
trace
Run 03
ND
ND
ND
Average
--
--
--
ND = not detected. Detection limit - 4 ppm.
* Cleanup problems with acids fraction. See Table 8-7 for surrogate
recoveries.
5-37
-------
Table 5-18. Total Chloride Analyses of the Black Liquor Samples
?or Site BLB-B
Liquor
Run No.
Total Chloride
Concentration
(ug/g)
Strong Black Liquor
Weak Black Liquor
01
02*
03
Average
01
02
03
Average
4604.9
5329.8
5910
5281
1714.0
1893.7
1725.0
1777.6
*The average value reported for duplicates.
5-38
-------
nature of the samples. Table 8-7 shows the problems found with surrogate
recoveries for phenols.
5.6 AUXILIARY PROCESS SAMPLE ANALYSES
In addition to the chloride analysis performed on each HC1 train.
chloride analysis was also performed on the strong black liquor, weak black
liquor, white liquor, by-product saltcake, neutralized spent acid, and the
make-up water (well water) samples collected at Site BLB-B. The results of
the strong and weak black liquor chloride analyses are presented in Section
5.4, Precursor Data. Table 5-19 summarizes the data obtained from the total
chloride analyses of the other process samples mentioned above. The majority
of the chlorine entering the black liquor circuit comes from the neutralized
spent acid, the by-product salt cake, and the well water used for process
make-up with each contributing 9.67, 13.9, and 911 g chlorine/mg of solids
burned, respectively.
5.7 HC1 TRAIN CHLORIDE EMISSIONS DATA
Table 5-20 summarizes HC1 train chloride emissions data measured at the
electrostatic precipitator outlet sampling location. The data are reported as
"front half," "back half," and."train total" chloride emissions. The front
half emissions represent chlorides captured in the probe rinse/filter fractio.n
of the HC1 train, which may include metal chlorides contained in the
particulate matter. The back half emissions represent chlorides captured in
the HC1 sample train impingers, which would include HC1 and any metal
chlorides that pass through the sample train filter. The train total
emissions represent the sum of the front half and back half emissions.
As shown in Table 5-20, the average as-measured train-total chloride
emissions concentration was approximately 2.1 mg/dscm (0.001 grains/dscf).
Corrected to 3% 02 using the EPA Method 3 data, this corresponds to
approximately 2.5 mg/dscm @ 3% 02 (.001 gr/dscf @ 3% 02). The train total
chloride mass emission rate from the electrostatic precipitator outlet exhaust
stack was about 0.44 Kg/hr (0.968 Ib/hr). Chloride emissions were
non-uniformly distributed between the front half and back half of the HC1
sample train.
5-39
-------
Table 5-19,. Summary of Total Chloride Data for Site BLB-B
Test Run
01
02
03
Average
Neutralized
Spent Acid
820
NAb
790
805
By- Product
Salt Cake
1200
1100
1300
1200
White
Liquor
NAb
7800
4500
6150
Make-Up Water
(Well Water)
240
230
230
230
All concentrations expressed as ug/g as Cl".
DThe sample was Parr-bombed and the result was invalid.
5-40
-------
TABLE 5-20. HC1 TRAIN CHLORIDE EMISSIONS DATA FOR SITE BLB-B
- AT THE ELECTROSTATIC PRECIPITATOR OUTLET
Parameter
Run 01
Run 02
Run 03 Average
Total Chloride Concentration
(mg/dscm, as measured)
Front Half
Back Half
Train Total
Total Chloride Concentration
(mg/dscm, corrected to 3% Oxygen)
Front Half
Back Half
Train Total
Total Chloride Mass Emission Rate
(Kg/hr)
Front Half
Back Half
Train Total
2.69
ND
2.69
3.21
ND
3.21
0.537
ND
0.537
0.63
0.58
1.21
0.75
0.69
1.44
0.138
0.128
0.266
2.40
ND
2.40
2.86
ND
2.86
0.514
ND
0.514
' 1.91
0.58
2.10
2.27
0.69
2.50
0.40
0.128
0.44
Concentration corrected to 3% 0- using the equation:
[Cl~] @ 3% 02 = [Cl~], as measured x (20.9 - 3)/(20.9 - %02)
5-41
-------
Compared with other Tier 4 test sites, Site BLB-B showed relatively low
chloride emissions based on the total train catch. The corrected
concentration range for all test sites for which HC1 sampling was performed
was 2.4 to 8800 mg/dscm @ 3% 02 (0.001 to 3.8 gr/dscf @ 3% 02), while the Site
BLB-B average was 2.5 mg/dscm @ 3% 02 (.001 gr/dscf @ 3% 02).
5.8 SOIL SAMPLING DATA
Dioxin/furan analyses are currently being performed on the soil sample
obtained at Site BLB-B.
5-42
-------
6.0 SAMPLING LOCATIONS AND PROCEDURES
Samples were collected from ten different locations at Site BLB-B. Three
of the locations were for gaseous sampling, five were for liquid sampling, and
two were for solid sampling. The source sampling and analysis matrix in Table
4-1 lists the sample locations, measured parameters, sampling methods, and
analytical methods that were used.
Details on the sampling locations and methods are discussed in Section
6.1 through 6.3. Analytical procedures for continuous monitoring of CO, C02,
02, NO , S02, and THC are included in Section 6.1. All other analytical
procedures are discussed in Section 7.
6.1 GASEOUS SAMPLING
Four types of gaseous samples were collected during this test program:
Modified Method 5 (MM5), HC1, EPA Method 3, and continuous monitoring (CEM).
The sampling locations and methods are further discussed in this section.
6.1.1 Gaseous Sampling Locations
6.1.1.1 ESP Outlet. The electrostatic precipitator outlet sampling location
is identified as point "E" in Figure 4-1. The sampling ports are located in
the 12 .ft. diameter exhaust stack serving the ESP. Four ports at 90°
orientation are located approximately 24 ft. (2 duct diameters) downstream of
the induced draft fan and over 48 ft. (4 duct diameters) upstream of the stack
exhaust to atmosphere. A total of 24 traverse points, 12 on each of 2
diameters, were used for stack gas velocity measurements and MM5 sampling.
The location of the sampling ports and the traverse point layout are shown in
Figures 6-1. and 6-2, respectively.
6.1.1.2 ESP Inlet. The electrostatic precipitator inlet sampling location is
identified as point D in Figure 4-1. The ESP inlet gas stream flows through
two similar ducts, designated as the North and South ducts. Sampling ports
6-1
-------
50'
24'
-12'0*
From
ESP
-5
ID Fan
-\\
Furnace Building
Flgur* 6-1. ESP Outlet Port Location, Site BLB-B
6-2
-------
B
3 1/2"-»
•\ 654321
12'*
Roof
Figure 6-2. Sample Point Layout, ESP Outlet Site 05.
6-3
-------
are located similarly in each of the two horizontal 7.5 ft. diameter ducts.
Two ports at 90° orientation are located 25 ft (3.3 duct diameters) downstream
of a bend in the ductwork, and 18 ft. (2.4 duct diameters) upstream of the
entrance to the ESP.
A total of 24 traverse points (12 on each of two diameters) were to be
used for velocity measurements and MM5 sampling. However, a dust accumulation
was present in the bottom of each duct. The clear depth measured through the
top port at the North and South ducts was 83 1/2 inches as compared to the
stack diameter of 89 1/2 inches. In order to avoid collection of re-entrained
dust, sampling was not conducted at the lower four points on the vertical
traverse. The remaining 20 traverse points were used to measure gas velocity
at the North duct, and to measure gas velocity and for MM5 sampling in the
South duct. The port locations and traverse point layouts are given in
Figures 6-3 and 6-4 respectively.
6.1.1.3 Recovery Boiler Outlet.
The sampling location at the recovery boiler outlet was located between
the furnace and the direct contact evaporator outlet. This location is
identified as point C in Figure 4-1. The single sampling port is located in a
rectangular duct. The continuous monitoring probe was located 2 feet into the
duct.
6.1.2 Gaseous Sampling Procedures
Gaseous sampling procedures used during the testing are listed in
Table 6-1. These procedures 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 section.
6.1.2.1 Modified Method 5 (MM5K
Gas sampling for dioxins and furans was conducted according to the
October 1984 draft of the ASME chlorinated organic compound sampling protocol.
6-4
-------
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to
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a
E
a
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-------
CM
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a
a
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-------
TABLE 6-1. SUMMARY OF GAS SAMPLING METHODS FOR SITE 05
Sample Location
Sample Type
or Parameter
Sample
Collection Method
ESP Outlet, Point E,
Figure 4-1
ESP Inlet, Point D,
Figure 4-1
South Duct
North Duct
Recovery Boiler
Outlet, Point C,
Figure 4-1
Dioxin/furan
Volumetric Flow
Gas Molecular Weight
Moisture
HC1
Dioxin/furan
Volumetric flow
Molecular Weight
Moisture
Volumetric flow
CO, C02, 02, S02, NO..
and THC monitoring
Modified EPA Method 5
EPA Method 2
EPA Method 3
EPA Method 4
HC1 train
Modified Method 5
EPA Method 2
EPA Method 3
EPA Method 4
EPA Method 2
Continuous monitors
6-7
-------
Minor deviations from the ASHE protocol are discussed later in this section.
This sampling method-is a modified version of EPA Method 5 that includes a
solid sorbent module for trapping vapor phase organics. The MM5 sampling
train was used to collect samples at the electrostatic precipitator outlet
exhaust stack and at the black liquor boiler outlet sampling location.
Following sample recovery, the various parts of the sample (filter, solvent
rinses, sorbent trap, etc.) were sent to the EPA's Troika laboratories to
quantify 2, 3, 7, 8-TCDD, tetra-through octa-dioxin homolgues, 2,3,7,8-TCDF,
and tetra- through octa- furan homologues. A total of three MM5 test runs
were conducted simultaneously at the two sampling locations, with one test run
being conducted at each location per test day. The MM5 samples were collected
isokinetically over a 240-minute on-line sampling period at the electrostatic
precipitator outlet with a sample flow rate of approximately 0.50 scfm.
Sampling was performed during the same time period at the electrostatic
precipitator inlet location. The actual on-line sampling period was 160-200
minutes. Multiple filter changes were required at this location because of
the high particulate loading. A complete traverse was not completed during
Run 01. The sample box suspension system failed after the top three points on
the vertical diameter were sampled. The probe was bent and a replacement was
not readily available. The sampling train was successfully leak checked after
the partial traverse. The sample flow rate at the electrostatic precipitator
inlet was approximately 0.5 scfm.
A schematic diagram of the MM5 sampling train is shown in Figure 6-5.
Flue gas is pulled from the stack through a nozzle and a heated glass probe.
Particulate matter is removed from the gas stream by means of a glass fiber
filter housed in a teflon-sealed glass filter holder maintained at 248 ± 25°F.
The gas passes through a sorbent trap similar to that illustrated in Figure
6-6 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-2R resin (XAD). A chilled impinger train following
the sorbent trap is used to remove water from the flue gas, and a dry gas
meter is used to measure the sample gas flow.
6-8
-------
Ifl
•o
o
o
5
•
o
in
i
3
6-9
-------
JT
28/12
Condenser Coll
ra,
28/12
XAO-2
Trap "*
_ cfc-Th
Co«r«« Frit
Thermocouple Well
28/12
Figure 6-6: Adsorbent Sampling System
6-10
-------
Modifications'to the ASME protocol that were instituted for this test
site include the following:
1. Sample recovery was modified to include methylene chloride in the
sample train rinsing scheme. Water, acetone, and methylene chloride
were used in series to recover the probe, back half-coil, and first
impinger samples. Previous black liquor sampling experience has
shown that water is necessary because the black liquor boiler
particulate is soluble in water but insoluble in acetone.
2. The probe brush is specified in the ASME protocol as being inert
material with a stainless steel handle. To ensure cleanliness, a
separate precleaned nylon bristle brush attachable to a stainless
steel handle was used for each probe cleaning.
3. The condenser was oriented horizontally instead of vertically.
6.1.2.2 HC1 Determination.
HC1 concentrations in the electrostatic precipitator outlet exhaust stack
were determined using another modification fo EPA Method 5. The sample train
components and operation were identical to those of Method 5 with the
following exceptions:
1. No knockout impinger was utilized.
2. Water in the first two impingers was replaced with.O.lM KOH. As
discussed in Section 4.1, the substitution of KOH in the impingers
was performed to eliminate NaCl interferences in the determination
of HC1 emissions by utilizing sodium, sulfate, carbonate and chloride
material balances on the impinger solutions. These interferences
would lead to overestimates of HC1 due to the chlorine from NaCl.
Upon further study of this issue, it was determined that several
additional chemical analysis would be needed to remove the potential
NAC1 interference. The uncertainty of the final result would be
increased according to the uncertainty of each additional analysis.
As a result, the plan to remove NaCl interferences was dropped and
only the total chloride analysis results are reported.
3. Sampling was single-point isokinetic with the nozzle placed at
points in the stack with approximate average velocity.
6-11
-------
4. .The moisture/KOH in the impingers was saved for laboratory analysis
by ion chromatography for total chlorides. The impinger catch was
analyzed by Radian's Austin, Texas laboratory.
Recovery of the HC1 train provided a sample consisting of three components:
probe rinse, filter, and back-half rinse/impinger catch.
A total of three HC1 train runs were performed at the electrostatic
precipitator outlet stack sampling location. The HC1 samples were collected
over on-line sample times of 100 to 175 minutes at a sample flow rate of
approximately 0.4 scfm.
6.1.2.3 Volumetric Gas Flow Rate Determination.
The volumetric gas flow rate was determined at the electrostatic
precipitator inlet (corrected for one partially blocked duct, see Appendix L)
and'outlet sampling locations using EPA Method 2. Based on this method, the
volumetric gas flow rate was determined by measuring the average velocity of
the flue gas and the cross-sectional area of the duct. The average flue gas
velocity was calculated from the average of the velocity pressure differential
•
( P) measurements at each traverse point, the average flue gas temperature,
the gas molecular weight, and the absolute static pressure.
\
6.1.2.4 Flue Gas Moisture Determination.
The moisture content of the flue gas was determined at the electrostatic
precipitator inlet and outlet sampling locations using EPA Method 4. Based on
this method, a measured volume of particulate-free gas was pulled through a
chilled impinger train. The" quantity of condensed water was determined
gravimetrically and then related to the volume of gas sampled to determine the
moisture content.
6.1.2.5 Flue Gas Molecular Weight Determination.
The integrated sampling technique described in EPA Method 3 was used at
the electrostatic precipitator inlet and outlet sampling locations to obtain a
composite flue gas sample for fixed gas (CL, COg, Ng) analysis. The fixed gas
analysis was used to determine the molecular weight of the gas stream. A
6-12
-------
small diaphram pump and a stainless steel probe were used to extract single
point flue gas samples. The samples were collected in a 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 composition of the gas sample was determined using a Shimadzu Model
3BT analyzer instead of the Fyrite or Orsat analyzer prescribed in EPA
Method 3. The Shimadzu instrument employs a gas chromatograph and a thermal
conductivity detector to determine the fixed gas composition of the sample.
6.1.2.6 Continuous Monitors.
Continuous monitoring was performed at the boiler outlet sampling
location for Op, C02, CO, NOX, SO^, and THC throughout the 4 to 6-hour period
that MM5 dioxin sampling was being conducted each test day. The primary
objectives of the continuous monitoring effort were to observe fluctuations in
flue gas parameters and to provide an indication of combustion conditions.
sample acquisition was accomplished using an in-stack filter probe and a 150
D
ft. length of heat-traced Teflon sample line connected to a mobile
laboratory. The heat-traced sample line was maintained at a temperature of at
least 120°C to prevent condensation in the sample line. The stack gas sample
was drawn through a sample gas conditioner, which consisted of an ice bath and
a knockout trap. The sample gas conditioner removes moisture and thus provide
a dry gas stream for analysis. A separate unconditioned gas stream was
supplied to the THC analyzer for analysis on a wet basis.
An Anarad Model 412 nondispersive infrared (NDIR) analyzer was used to
measure CO and CO-; a Beckman Model 755 paramagnetic analyzer was used to
measure 0?; a Teco Model 10 chemiluminescent analyzer was used to measure NO ;
™ S\
a Teco Model 40 pulsed fluorescence analyzer was used to measure S02; and a
Beckman Model 402 flame ionization analyzer was used to measure THC.
6.2 LIQUID SAMPLING
Five types of liquid samples were obtained during this test program:
strong black liquor, weak black liquor, white liquor, spent acid from the R2
C102 generator, and well-water. The corresponding sampling locations are
shown in Figure 4-1 as A, J, 6, I, and H, respectively.
6-13
-------
6.2.1 Strong Black Liquor Sampling
Strong black liquor samples were taken from a sample tap in a pressure
line to one of the black liquor firing guns in the furnace. The host site
performs strong black liquor sampling at this location.
Three identical composite strong black liquor samples were obtained
during each of the three tests: a 1 liter composite was shipped to Troika for
dioxin precursor analysis, and 125 ml composite was analyzed for dioxin
precursors by Radian/RTP. The composite strong black liquor samples for each
run were comprised of hourly 1-liter grab samples from a line loading to the
black liquor firing guns. The hourly grab samples were placed into a heated
jar to prevent the sample from solidifying prior to taking the final sample
aliquots. This was accomplished by wrapping the sample composite bottle with
rubber coated heat tape.
6.2.2 Auxiliary Black Liquor Circuit Sampling
Samples of the white liquor, weak black liquor, well water and spent acid
from the R2 C102 generator were obtained to indicate the relative amounts of
chlorine entering the black liquor circuit through various input sources. One
125 ml composite sample of each stream was obtained during each test.
Individual samples were taken twice during each test run, and the composite
samples were prepared accordingly. The samples were analyzed for total
chlorine content only. The chlorine content data was used in conjunction with
mass flow data to determine the relative amounts of chlorine associated with
each potential source of chlorine input to the black liquor circuit. The
chlorine analysis'was perfromed by the Radian Analytical Services laboratory
in Austin, Texas using ion chromatography.
The weak black liquor samples were collected from a sample tap in the
transfer line between the weak black liquor storage tank and the vacuum
evaporators. The white liquor was collected from a sample tap on the transfer
line from the storage tank to the digestors. The R2 C102 generator spent acid
was collected from a sample tap in the line from the C102 generation plant to
the weak black liquor storage tank. The process makeup water was sampled from
taps at the two wells (North and South) serving the plant.
6-14
-------
6.3 SOLID SAMPLING
Two types of sol-id samples were obtained at Site BLB-B: by-product
/
saltcake from the R3 ClOg generation process and soils from plant property.
The sampling locations and methods are discussed below.
6.3.1 Bv-Product Saltcake Sampling
Samples of by-product saltcake from the R3 generation system were
collected from the vacuum filter belt. A single grab sample was collected
once per test run. Access to the sampling area was limited because of
elevated ambient chlorine concentrations. A 125 gram aliquot of the grab
sample was sent to Radian's Austin Laboratory for total chlorine analysis.
6.3.2 Soil Sampling
A single composite soil sample comprised of 10 individual soil samples
was obtained at Site BLB-B. Soil sampling protocol for Tiers 3, 5, 6, and 7
of the National Dioxin Study are specified in the document, "Sampling Guidance
Manual for the National Dioxin Study." A similar protocol was used for soil
sampling at this test site. A total of 10 soil sampling locations were
selected on plant property surrounding the black liquor boiler complex. The 10
individual soil sampling locations are shown in Figure 6-7 and are listed in
Table 6-2. Soil samples were collected by forcing a bulb planter into the
soil to a depth of 3 inches. The soil samples were then composited in a clean
stainless steel bucket. Five hundred grams of the composite was placed in a
950 ml amber glass bottle and returned to Radian/RTP for archiving.
6-15
-------
TABLE 6-2. DESCRIPTION OF SOIL SAMPLING LOCATIONS AT SITE 05
Aliquot
Number
Location Description
1 River bank at North end of plant
2 Near Plant gate
3 Behind administration buildings
4 Dirt beside road at Biceps
5 Dirt beside road at maintenance area
6 Dirt near wastewater clarifier
7 Dirt beside road near clarifier
8 Dirt beside road south of #3 machine room
9 Dirt beside road to water wells
10 River bank at south end of plant
6-16
-------
;/| -~H ^-H *
^c^M^L—J g o o I lldJiN?
"
•43 • ^ ••
-------
-------
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. Analyses for
dioxins/furans were performed by EPA's Troika laboratories. The procedures
used for these analyses are described in detail in the Analytical Procedures
and QA Plan for the Analysis of Tetra through Octa CDD's and CDF's in Samples
from Tier 4 Combustion and Incineration Processes (addendum to
EPA/600/3-85-019, April 1985) and are summarized in Section 7.1.
Black.liquor boiler feed samples from Site BLB-B were analyzed to
determine concentrations of chlorinated phenols (CP), chlorobenzenes (CB),
polychlorinated biphenyls (PCBs), total organic halogen (TOX), and total
chlorine. Procedures used for these analyses are detailed in Section 7.2.
7.1 DIOXINS/FURANS
The analytical procedures described in this section were used for the
determination of PCDD and PCDF in stack effluent samples (MM5). 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 solutions consisted of impinger catch and solid samples
including filters and XAD resin. Isotopically-labeled surrogate compounds
were added to all samples prior to extraction to allow determination of method
efficiency.
Organic liquid samples (acetone and hexane or methylene chloride) were
concentrated using a nitrogen blowdown apparatus. The residue, which
contained particulates from the 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 sample
was then concentrated by nitrogen blowdown and subjected to chromatographic
cleanup procedures.
Aqueous solutions 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
-------
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/diol 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 Chromatooraph - Injector configured for capillary column, split!ess
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 1mA; mass resolution 8,000 to 10,000; ion source temperature 270°C.
7.2 DIOXIN/FURAN PRECURSORS
Feed samples for Site BLB-B were analyzed by Radian/RTP for chlorophenols
(CP), chlorobenzenes (CB) and polychlorinated biphenyls (PCBs) by GC/MS; total
organic halides (TOX) by GC/Hall detector; 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.
7.2.1.1 Sample Preparation
A flow chart for the sample preparation procedure used for Site BLB-B
feed samples is shown in Figure 7-1. The first step involved adding 200 ml of
7-2
-------
methanol to the sample. The next step in the procedure involved adding
labeled surrogate compounds to provide a measure of extraction method
efficiency and sonicating the sample for 30 minutes. The sonicated sample was
filtered and rinsed with 85 mL MeCl2 and distilled H20. The filtrate was
extracted three times with 50 mL MeCl2 in a separatory funnel and the
resulting aqueous and organic fractions saved for derivatization and/or
further cleanup. Cleanup procedures consist of 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 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 05 samples are provided in
the sections below.
The aqueous fraction (or acids portion) was acidified to pH #2 with HC1
and then extracted three times with MeCl2, then two times with NaHCO-. The
MeCl2 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. Add 2.0 mL isooctane, 2.0 mL acetonitrile, 50 uL pyridine, and 20
uL acetic anhydride to the extract. Put the test tube containing
the extract in a 60°C water bath for 15 minutes, shaking 30 seconds
every 2 minutes.
Add 6 mL of 0.01 N H3P04 to the test tube and agitate the sample for
2 minutes on a wrist action shaker.
Remove the organic layer and add the quantisation standard.
Concentrate the sample in a Reacti-VialR at room temperature (using
prepurified NZ) to 1 mL prior to GC/MS analysis.
Cleanup of the organic (or base/neutrals) layer from the initial MeCl2
extraction involved successively washing the extract with concentrated H2S04
and deionized water. The acid or water was added in a 30 mL portion and the
sample was shaken for two minutes. After the aqueous and organic layers were
completely separated, the aqueous or acid layer was discarded.
2.
3.
7-4
-------
The acid washing procedure was repeated until the acid layer was colorless.
The sample was then dried with anhydrous Na2S04, exchanged into hexanes 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, taper 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 M NaOH, and 2.0 g silica. The concentrate was quantitatively transferred to
the column and eluted with 90 ml hexanes. The entire eluate was collected and
concentrated to a volume of 1 mL in a centrifuge tube, as above.
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, which has 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 from above was quantitatively
transferred onto the liquid chromatography column, and the centrifuge tube was
rinsed consecutively with two 0.3-mL portions of a 3 percent MeCKrhexanes
solution, and the rinses were transferred to the chromatography column.
The column was eluted with 20 ml of a 50 percent (v/v) MeCK:hexanes, and
the elute was retained. The retained fraction was concentrated to a volume of
approximately 1 ml by heating the tubes in a water bath while passing a stream
of prepurified N2 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 for CP, CB and PCBs- present in the feed sample extracts were
performed using 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
Project Plan. An internal standard calibration procedure was used for sample
quantitation. Compounds of interest were calibrated against a fixed
7-5
-------
TABLE 7-1. INSTRUMENT CONDITIONS FOR GC/MS PRECURSOR ANALYSES
Parameter
Chlorobenzenes/
Polychlorinated biphenyls
Chlorophenols
Column
Injector 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
Separator Oven Temperature 290°C
9 psi
1 mL/min
40(4)-290°C,
10°/rnin & 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
-------
concentration of either d12-chrysene (CB, PCB) or tig-naphthalene (CP).
Compounds of the calibration solution are shown in Table 7-2. For multi-point
calibrations, this solution was injected at levels of 10, 50, 100, and 150
ng/mL.
Compound identification was confirmed by comparison of chromatographic
retention times and mass spectra of unknowns with retention times and mass
spectra for reference compounds. Since the selected ion monitoring technique
was necessary for the types of samples analyzed, care was taken to monitor a
sufficiently wide mass region to avoid the potential for reporting false
positives.
The instrument detection limit was estimated to be approximately 500
picograms 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 TOX ANALYSIS
Boiler feed samples were analyzed for total organic halide (TOX) by
short-column GC and a Hall detector (GC/Hall). Samples were extracted with
benzene for at least 16 hours in a Soxhlet apparatus. The extracts were
washed three times with 100 ml portions of reagent-grade water concentrated to
10 ml.
An attempt to use a fused silica capillary column to separate surrogates
from target compounds was unsuccessful due to the complexity of the sample
constituents. Determinations for TOX were therefore performed on samples
without surrogates and no measure of extraction efficiency is available.
Instrument conditions are shown in Table 7-3. Sample quantitation was
based on an average response factor developed from a mixture of chlorinated
benzenes and brominated biphenyls. Individual CP, CB and PCBs were also
injected at various concentrations to develop a calibration curve for
comparison to the mixture response factors.
7.4 TOTAL CHLORINE ANALYSIS
Total chlorine concentrations in feed samples were determined by Parr
Bomb combustion followed by ion chromatography (1C). A 0.5g sample was placed
7-7
-------
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-pentachlorobi phenyl
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
decachlorobiphenyl
p-dichlorobenzene
1,2,4-trichlorobenzene
1,2,3,5-tetrachlorobenzene
pentachlorobenzene
hexachlorobenzene
d4-l,4-dichlorobenzene (SS)1
3-bromobiphenyl (SS)
2,2',5,5'-tetrabromobiphenyl (SS)
2,2',4,4',6,6'-hexabromobiphenyl (SS)
octachloronaphthalene (QS)2
d10-phenanthrene (QS)
d12-chrysene (QS)
1
Surrogate standard.
•Quantitation standard.
Acids
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)
d10-phenanthrene (QS)
d12chrysene (QS)
7-8
-------
TABLE 7-3. ANALYTICAL CONDITIONS FOR TOX ANALYSIS
Hall Detector Conditions
Reactor temperature - 850°C
Solvent - n-propanol
Hydrogen flow rate - 35 mL/min
GC Conditions (Varian 3700)
Injection volume (1-5 uL)
Helium carrier gas flow rate - 60 mL/min
Column - 3-ft packed column with 1 in 10% 0V 101
Column temperature - 200°C isothermal
7-9
-------
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.
7-10
-------
-------
8.0 QUALITY ASSURANCE/QUALITY CONTROL (QA/QC)
This section summarizes the results of the quality assurance and quality
control (QA/QC) activities for Site BLB-B. The flue gas 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. Run 03 (ESP inlet sample) was the only
sample having surrogate recoveries outside the QC limits of 40 to 120 percent
for hepta- and octa-CDD's. The results of the analysis of the fortified
laboratory QC sample were all within 25 percent of the true value, which is
well within the Tier 4 objective of ±50 percent. These data indicate that the
dioxin/furan results are within accuracy criteria specified for Tier 4.
The dioxin/furan precursor analysis of the feed samples was not as
accurate as the dioxin/furan homologue analysis. Surrogate recoveries of the
base neutrals fraction were generally within the specified QC limits of
±50 percent; however, the surrogate acid fractions were generally below the
specified limits. In spite of the low recoveries of the acid fraction, 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 BLB-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. The laboratory analysis QA/QC activities are
summarized Jn Section 8.3.
»
8.1 MANUAL GAS SAMPLING
Manual gas sampling methods used at Site BLB-B included Modified Method 5
(MM5), the HC1 acid train 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, 3) procedural QC checks, and 4) sample custody
procedures. Key activities and QC results in each of these areas are
8-1
-------
discussed in this section. Also discussed are problems encountered that may
have affected data quality.
8.1.1 EquipmentCalibration and Glassware Preparation
Pretest calibrations or inspections were conducted on pi tot tubes,
sampling nozzles, temperature sensors and analytical balances. Both pre- and
post-test calibrations were also performed on dry gas meters. All of this
equipment met the calibration criteria specified in the QAPP. Differences in
pre- and post-test dry gas meter calibrations were less than 2.5 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 could potentially interfere with the
analysis for dioxins and furans. To minimize the potential for contamination
in the field, all sample train glassware was kept capped until use and a
controlled environment was maintained in the recovery trailer during sample
train assembly and recovery.
8.1.2 Procedural QC Activities/Manual Gas Sampling
Procedural QC activities during manual gas sampling focused on:
* inspecting equipment visually;
collecting sampling 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 rate calculations for the MM5 test runs are shown
in Table 8-2. As shown in Table 8-2, the average isokinetic sampling rate for
the MM5 sampling trains achieved the QA objective of ±10 percent for all test
runs.
8-2
-------
TABLE 8-1. GLASSWARE PRECLEANING PROCEDURE
NOTE: USE DISPOSABLE GLOVES AND ADEQUATE VENTILATION
1. Soak all glassware in hot soapy water (Alconox) 50°C or higher.
2. Distilled/deionized H20 rinse (X3)a.
3. Chromerge rinse, if glass, otherwise skip to 6.
4. High purity liquid ehromatography grade FLO rinse (X3).
5. Acetone rinse (X3), (pesticide grade).
6. Hexane rinse (X3), (pesticide grade).
7. Cap glassware with clean glass plugs or hexane rinsed aluminum foil
a (X3) - three times.
8-3
-------
TABLE 8-2. SUMMARY OF ISOKINETIC RATE RESULTS FOR MM5 SAMPLING, SITE 05
ESP Outlet
Isokinetic
Run Rate
01 98.0
02 . 104.8
03 103.7
Meets QC
Objective?
yes
yes
yes
ESP Inlet
Isokinetic
" Rate
103.9
102.8
102.6
Meets QC
Objective?
yes
yes
yes
NOTE: The quality control objective for MM5 sampling was an isokinetic rate
of 100 ± 10%.
8-4
-------
8.1.3 Sample Custody
Sample custody procedures used during this program emphasized careful
documentation of the samples collected and the use of chain-of-custody records
for samples to be transported. Steps taken to identify and document samples
collected included labeling each sample with a unique alphanumeric code and
logging the sample in a master sample 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
chain-of-custody seal so that the container could not be opened without
tearing the seal.
8.2 CONTINUOUS MONITORING/ MOLECULAR WEIGHT DETERMINATION
Flue gas parameters measured continuously at the Inlet Location during
the MM5 test runs include CO, C02, 02 total hydrocarbons (THC), S02, and NO .
The concentrations of 02, C02 and nitrogen (N2) were also determined for
integrated bag samples of the flue gas. Quality control results for these
analyses are discussed in this section.
Drift check results for the continuously monitored flue gas parameters
are summarized in Table 8-3. Data reduction was performed by assuming a
linear drift of the instrument response over the test day based on drift
checks at the beginning and end of the day. The largest calibration drifts
were observed for the S02 analyzer, but none exceeded QC target goals. The
smallest instrument drift was observed in the oxygen monitor.
The quality control standards for this program consisted of mid-range
concentration standards that were intended for QC purposes and not for
instrument calibration. The QC gases were analyzed immediately after
calibration each day to provide data on day-to-day instrument variability.
The acceptance criteria for the analysis of each QC standard was agreement
within ±10 percent of the running mean value. The CEM data quality was good
for all constituents except 02. The rest of the CEM data is accurate and
valid for Tier 4 parameter comparisons (accurate, reproducible measurements
were made of what existed after the sample conditioning system leak).
8-5
-------
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Molecular weight was determined by analyzing integrated bag samples of
flue gas for 02, C02 and Ng. 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 sample quantification.
These criteria were met for all molecular weight determination.
8.3 LABORATORY ANALYSIS
QA/QC activities were carried out for dioxin/furan, precursor, and total
chloride analyses performed on Site BLB-B samples. The dioxin/furan analyses
of MM5 train samples performed by Troika are considered in Section 8.3.1; the
precursor analyses of black liquor boiler feed samples performed by Radian/RTP
are considered in Section 8.3.2; and the total chloride analyses of HC1 train
samples and process samples performed by Radian/Austin are considered in
Section 8.3.3.
8.3.1 Dioxin/Furan Analyses
Two individual topics related to the dioxin/furan analyses at Site BLB-B
are discussed in this section. Analytical recoveries of labeled surrogate
compounds spiked onto MM5 train, samples are reported in Section 8.3.1.1.
Sample blank data are reported in Section 8.3.1.2.
8.3.1.1 Surrogate Recoveries of the Test Samples
Table 8-4 presents the analytical recovery data reported by Troika for
four isotopically labeled surrogate compounds spiked onto the MM5 train
samples. Samples were spiked with all four of the surrogates. Average
recovery for the MM5 train samples was 75 percent for the inlet and 78 percent
for the outlet.
8.3.1.2 Sample Blanks
Table 8-5 summarizes the analytical results reported by Troika for
internal laboratory blanks, laboratory fortified quality control (QC) samples,
proof blank MM5 train samples, and field recovery blank MM5 train samples. In
8-7
-------
Table 8-4. Percent Surrogate Recoveries for Site BLB-B
Dioxin/Furan Analyses
Sample
37C1
U4
TCDD
13C
4
TCDD
37C1
U4
Hepta-CDD
13C
L12
Octa-CDD
HM5 Train Samples
Inlet
Run 01
Run 02
Run 03
Outlet
Run 01
Run 02
Run 03
96
107
86
96
96
104
97
101
80
100
77
94
55
63
39
60
54
55
76
66
28
79
64
62
8-8
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-------
general, the data showed good surrogate recoveries, with values ranging from
46 to 100 percent which satisfied the QA objectives for the project (40 to 120
percent recovery). Comparison of the measured and spiked values for the
laboratory fortified QC samples showed agreement to within ±25 percent for all
target species except the penta-CDF isomer. The measured value for the
penta-CDF isomer was roughly 37 percent lower than the spiked value. Dioxin
and furan species were non-detectable in all proof blank MM5 train samples.
Small but detectable quantities of several dioxin and furan species were found
in the field blank HM5'train at the ESP inlet, but were not detected in the
field blank for the MM5 train at the ESP outlet. Table 8-6 gives a comparison
of the dioxin/furan analytical results for the field blank MM5 train and the
test run MM5 trains. For the inlet values, only the octa-CDD homologue had a
detectable field blank value, equal to 19 percent of the minimum test run
value. However, for the outlet data, both the "other TCDF" and "hexa-CDF" had
reported field blank values very close to the detection limit. Overall, the
field clean-up procedures were found to be adequate for this test site.
Emissions data reported in Section 5.4 are not blank-corrected.
8.3.2 Precursor Analyses
Table 8-7 presents analytical recovery efficiencies for seven
isotopically labeled compounds used as surrogates for the target precursor
analytes in the Site BLB-B feed samples. The surrogate recovery values in
Table 8-7 vary considerably by specific surrogate species but are fairly
uniform between runs for the same species. Several of the recoveries are
below the 50 percent objective stated in the Tier 4 QA Project Plan and are
below those generally considered achievable when analyzing for similar
compounds in water or from MM5 train components. In spite of the relatively
low surrogate recovery values for some of the feed samples, the resulting
analytical sensitivity for the target analytes was considered acceptable for
the purpose of this study.
8.3.3 Total Chloride Analysis
Total chloride analyses were performed by Radian/Austin on the HC1 train
samples. QA/QC activities include total chloride analysis of field recovery
8-10
-------
Table 8-6. Field Blank Dioxin/Furan Data for Site BLB-B MM5 Samples
Amount
Field Blank Value
Isomer/Homologue
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
Inlet
ND
ND
ND
ND
ND
0.3
ND
ND
ND
ND
ND
ND
Outlet
ND
ND
ND
ND
ND
ND
ND
0.2
ND
0.2
ND
ND
Detected,
Nanoarams ner Train
Minimum Test Run Value Pprrpntanoa
Inlet
ND
ND
ND
0.6
0.4
1.6
ND
ND
ND
ND
ND
ND
Outlet
ND
ND
ND
0.3
0.7
2.3
0.1
0.2
ND
0.2
0.1
0.1
Inlet
0
0
0
0
0
19
0
0
0
0
0
0
Outlet
0
o
n
n
n
0
n
100
o
100
n
0
Percentage shown is the ratio of the field blank value to the minimum test
run value, expressed as a percentage.
8-11
-------
TABLE 8-7. PERCENT SURROGATE RECOVERIES FOR SITE BLB-B FEED SAMPLES
Surrogate Compound
Percent Surrogate Recovery
Run 01
Black Liquor Feed
Run 02 Run 03 Average
d^-di chlorobenzene
bromobiphenyl
2',5,5* tetrabromobiphenyl
dg-phenol
d^-2-chlorophenol
13
C -pentachlorophenol
6
91
101
84
3
9
12
73
91
74
3
9
13
70
78
71
2
7
10
78
90
76
3
8
12
8-12
-------
blank HC1 train samples, total chloride analysis of an aliquot of the KOH
solution used in the sample train impingers, and duplicate total chloride
analyses of the impinger rinse from Run 02. Chlorides were not detected in
either the field recovery blank train samples or the aliquot of KOH solution
analyzed. Duplicate analyses of the impinger rinse of the HC1 train from Run
02 differed by a factor of 2. Total chloride analysis was also performed in
duplicate for the strong black liquor sample collected from Run 02. The
duplicates differed by only 2 percent, which indicates excellent analytical
precision.
8-13
-------
-------
APPENDIX A
FIELD SAMPLING DATA
-------
-------
APPENDIX A-l
MODIFIED METHOD 5 AND
EPA METHODS 1-4 FIELD RESULTS
A-l
-------
_
-------
METHOD 3 —
PLANT
PLANT SITE
SAMPLING LOCATION
TEST tt
DATE
TEST PERIOD
SITE- 05
NA , NA
REVISED DIAMETER
05-MM5-D-01
02/26/85
1452-2043
PARAMETER
VALUE
Sampling time (min.)
Barometric Pressure (in.Hg)
Sampling nozzle diameter (in.)
Meter .Volume (cu.-ft.)
Meter Pressure (in.H20)
Meter Temperature (F)
Stack dimension (sq.in.)
Stack Static Pressure
Average stack temperature (F)
Percent CO2
Percent O2
Percent N2
Delps Subroutine result
DBM Factor
Pi tot Constant
160
30.22
.242
32.693
1.045
93.53O31
6133
-4.5
S37.4
29.88912
318.09O9
16.3242
3.8701
73.6014
21.36631
1.0097
.84
A-3
-------
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
SITE 05
NA , NA
REVISED DIAMETER
O5-MM5-D-O1
O2/26/85
1452-2043
PARAMETER
RESULT
Vm(dsc-f)
Vm(dscm)
Vw gas(sc-f)
Vw gas
Flow(dscmm)
'/. I
•/. EA
SO.6472
2.2S3929
39.48341
1.11817
32.86707
.6713293
29.O2947
25.40441
334O.907
1O1S.569
14229O.1
4029.657
64753.83
1833.828
103.8512
24.87104
Program Revision:1/16/84
A-4
-------
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
METHOD 3—
SITE 05
NA , NA
ESP INLET
O5-MM5-D-Q;
2/27/85
1230-1925
PARAMETER-
VALUE
Sampling time
-------
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
SITE 05
NA , NA
ESP INLET
05-MM5-D-O2
2/27/85
1230-1925
PARAMETER
RESULT
Vm(dsc-F)
Vm(dscm)
Vw gas(sc-f)
Vw gas (SCOT)
'/. moisture
Md
MWd
MW
Vs(-Fpm)
Vs (mpm)
Flow (ac-f m)
Flow
-------
I i^r-4 SOURCE
MEITHOID S —
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
SITE O5
NA , NA
REVISED DIAMETER
05-MM5-D-03
O2/2S/S5
1055-1615
PARAMETER
VALUE
Sampling time (min.)
Barometric Pressure (in.Hg)
Sampling nozzle diameter (in.)
Meter Volume (cu.-ft.)
Meter Pressure (in.H2O)
Meter Temperature (F)
Stack dimension (sq.in.)
Stack Static Pressure (in.H20)
Stack Moisture Collected (gm)
Absolute stack pressure(in Hg)
Average stack temperature (F)
Percent C02
Percent 02
Percent N2
Delps Subroutine result
DGM Factor
Pi tot Constant
200
3O.2
.242
104.71
1.O68
95.6625
6133
-4.5
1037.9
29.S6912
335.35
15. 1
5.2
75
22.28008
1.0097
.84
A-7
-------
M
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
SOURCE
THODS S —S
RESULTS
SITE 05
NA , NA
REVISED DIAMETER
O5-MM5-D-O3
02/28/85
1O55-1615
PARAMETER
RESULT
Vm(dsc-f)
Vm(dmcm)
Vw gas(sc-f)
Vw gas
-------
RADIAN
EPA M
(RAW
PLANT
PLANT SITE
SAMPLING LOCATION
TEST t
DATE
TEST PERIOD
SOURCE TEST
ETHOD 2-5
DATA)
SITE05
ESP OUTLET
05-MM5-E-01
02/26/85
1415-2003
PARAMETER
VALUE
Sampling time (min.)
Barometric Pressure (in.Hg)
Sampling nozzle diameter (in.)
Meter Volume (cu.ft.)
Meter Pressure (in.H20)
Meter Temperature (F)
Stack dimension (sq.in.)
Stack Static Pressure (in.H20)
Stack Moisture Collected (gm)
Absolute stack pressure(in Hg)
Average stack temperature (F)
Percent C02
Percent 02
Percent N2
Delps Subroutine result
DGM Factor
Pitot Constant '
240
30.22
.25
94.98908
.6678125
85.74167
16286.05
— 6
936.4724
30.17588
317.1667
14.1
5.9
74.5
16.16233
1.0092
.84
A-9
-------
RADIAN SOURCE
EPA METHODS 2
TEST
- 5
FINAL
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
RESULTS
SITE05
ESP OUTLET
05-MM5-E-01
02/26/85
1415-2003
PARAMETER
RESULT
Vm(dscf)
Vm(dscm)
Vw gas(scf)
Vv gas (scm)
Z moisture
Md
MWd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flov(acmm)
Flow(dacfm)
Flow(dscmm)
Z I
Z EA r
93.82869
2.657229
44.15468
1.25046
32
.68
28.952
25.44736
2513.034
766.169
284218.1
8049.055
132427.7
3750.351
98.00472
42.853
Program Revision:I/16/84
A-10
-------
R C E
2-5
RADIAN SOU
EPA METHOD
(RAW DATA)
PLANT SITE 05
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
TEST
ESP OUTLET
05-MM5-E-02
02/27/85
1300-1742
PARAMETER
VALUE
Sampling time (min.)
Barometric Pressure (in.Hg)
Sampling nozzle diameter (in.)
Meter Volume (cu.ft.)
Meter Pressure (in.H20)
Meter Temperature (F)
Stack dimension (sq.in.)
Stack Static Pressure (in.H20)
Stack Moisture Collected (gm)
Absolute stack pressure(in Hg)
Average stack temperature (F)
Percent C02
Percent 02
Percent N2
Delps Subroutine result
D6M Factor
Pitot Constant
240
30.2
.308
153.5271
1.640208
92.375
16286.05
-.6
1550.7
30.15589
308.3542
14.6
5.4
75.4
15.96329
1.0092
.84
A-ll
-------
SITE 05
RADIAN SOURCE
EPA METHODS 2
FINAL RESULTS
PLANT
PLANT SITE
SAMPLING LOCATION
TEST *
DATE
TEST PERIOD
TEST
5
ESP OUTLET
05-MM5-E-02
02/27/85
1300-1742
PARAMETER
RESULT
Vm(dacf)
Vm(dacm)
Vv gas(scf)
Vv gas (scm)
Z moisture
Md
MWd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flow(acmm)
Flow(dscfm)
Flow(dscmm)
I I
Z EA
150.0854
4.250418
73.1155
2.070631
32.75771
.672423
29.264
25.57417
2476.746
755.1054
280113.9
7932.825
130454.8
3694.48
104.8448
37.227
Program Revision:1/16/84
A-12
-------
RADIAN
EPA. METHOD
(RAW DATA)
PLANT SITE 05
PLANT SITE
SAMPLING LOCATION
TEST *
DATE
TEST PERIOD
SOURCE TEST
2-5
ESP OUTLET
05-MM5-E-03
02/28/85
1059-1553
PARAMETER
VALUE
Sampling time (min.)
Barometric Pressure (in.Eg)
Sampling nozzle diameter (in.)
Meter Volume (cu.ft.)
Meter Pressure (in.H20)
Meter Temperature (F)
Stack dimension (sq.in.)
Stack Static Pressure (in.H20)
Stack Moisture Collected (gm)
Absolute stack pressure(in Hg)
Average stack temperature (F)
Percent C02
Percent 02
Percent N2
Delps Subroutine result
DGM Factor
Pitot Constant
240
30.22
.308
158.035
1.7675
87.42709
16286.05
-.6
1486.5
30.17588
318.5625
15.3
5.3
75.7
16.7148
1.0092
.84
A-13
-------
SITE 05
RADIAN SOURCE
EPA METHODS 2
FINAL RESULTS
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
T
5
E S T
ESP OUTLET
05-MM5-E-03
02/28/85
1059-1553
PARAMETER
RESULT
Vm(dscf)
Vm(dscm)
Vw gas(scf)
Vv gas (scm)
Z moisture
Md
MWd
MW
Va(fpm)
Vs (mpm)
Flow(acfm)
Flow(acmm)
Flow(dacfm)
Flow(dscmm)
Z I
Z EA
156.0396
4.41904
70.08848
1.984906
30.99504
.6900496
29.624
26.02114
2570.123
783.5742
290674.7
8231.908
137191.2
3885.255
103.6518
36.09175
Program Revision:1/16/84
A-14
-------
RADIAN
SOURCE TEST
EPA METHOD
(RAW DATA)
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
2-5
SITE 05
ESP INLET-SOUTH DUCT
PRELIMINARY VELOCITY
02/25/85
PM
PARAMETER VALUE
Sampling time (min.) 160
Barometric Pressure (in.Eg) 30.22
Sampling nozzle diameter (in.) .242
Meter Volume (cu.ft.) 82.693
Meter Pressure (in.H20) 1.045
Meter Temperature (F) 93.53031
Stack dimension (sq.in.) 6291.25
Stack Static Pressure (in.H20) -4.5
Stack Moisture Collected (gm) 837.4
Absolute stack pressure(in Hg) 29.88912
Average stack temperature (F) 326.4211
Percent C02 16.3242
Percent 02 3.8701
Percent N2 73.6014
Delps Subroutine result 22.04748
DGM Factor 1.0097
Pitot Constant .84
A-15-
-------
RADIAN SOURCE
EPA HETHODS 2
FINAL RESULTS
PLANT SITE 05
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST
- 5
TEST PERIOD
ESP INLET-SOUTH DUCT
PRELIMINARY VELOCITY
02/25/85
PM
PARAMETER
RESULT
VmCdscf)
Vm(dscm)
Vw gas(scf)
Vw gas (scm)
Z moisture
Md
MWd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flow(acmm)
Flow(dscfm)
Flow(dscmm)
Z I
Z EA
80.6472
2.283929
39.48341
1.11817
32.86707
.6713293
29.02947
25.40441
3447.417
1051.042
150615
4265.417
67816.28
1920.557
101.7201
24.87104
Program Revision:1/16/84
A-16
-------
SITE 05
RADIAN SOURCE
EPA METHOD 2 -
( R A W DATA)
PLANT
PLANT SITE
SAMPLING LOCATION
TEST t
DATE
TEST PERIOD
TEST
ESP INLET-NORTH DUCT
PRELIMINARY VELOCITY
02/25/85
PM
PARAMETER VALUE
Sampling time (min.) 160
Barometric Pressure (in.Hg) 30.22
Sampling nozzle diameter (in.) .242
Meter Volume (cu.ft.) 82.693
Meter Pressure (in.H20) 1.045
Meter Temperature (F) 93.53031
Stack dimension (sq.in.) 6291.25
Stack Static Pressure (in.H20) -4.1
Stack Moisture Collected (gm) 837.4
Absolute stack pressure(in Hg) 29.91853
Average stack temperature (F) 322.8182
Percent C02 16.3242
Percent.02 3.8701
Percent N2 73.6014
Delps Subroutine result 21.71486
DGM Factor 1.0097
Pitot Constant .84
A-17
-------
SITE 05
RADIAN SOURCE
EPA METHODS 2
FINAL RESULTS
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
TEST
5
ESP INLET-NORTH DUCT
PRELIMINARY VELOCITY
02/25/85
PM
PARAMETER
RESULT
Vm(dscf)
Vm(dscm)
Vw gas(scf)
7w gas (scm)
Z moisture
Md
MWd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flow(acmm)
Flov(dscfm)
Flov(dscmm)
Z I
Z EA
80.6472
2.283929
39.48341
1.11817
32.86707
.6713293
29.02947
25.40441
3393.738
1034.676
148269.8
4199.001
67133.6
1901.223
102.7546
24.87104
Program Revision:I/16/84
A-13
-------
RADIAN SOURCE
EPA METHOD 2 -
( R A W DATA)
TEST
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
SITE 05
ESP INLET-NORTH DUCT
VELOCITY-1
02/26/85
PM
PARAMETER VALUE
Sampling time (min.) 160
Barometric Pressure (in.Hg) 30.22
Sampling nozzle diameter (in.) .242
Meter Volume (cu.ft.) 82.693
Meter Pressure (in.H20) 1.045
Meter Temperature (F) 93.53031
Stack dimension (sq.in.) 6291.25
Stack Static Pressure (in.H20) -3.8
Stack Moisture Collected (gm) 837.4
Absolute stack pressure(in Hg) 29.94059
Average stack temperature (F) 320.5833
Percent C02 16.3242
Percent 02 3.8701
Percent N2 73.6014
Delps Subroutine result 21.03932
DGM Factor 1.0097
Pitot Constant .84
A-19
-------
>SITE 05
RADIAN SOURCE
EPA METHODS 2
FINAL RESULTS
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
BATE
TEST PERIOD
TEST
5
ESP INLET-NORTH DUCT
VELOCITY-1
02/26/85
PM
PARAMETER
RESULT
Vm(dscf)
Vm(dscm)
Vv gas(scf)
Vv gas (scm)
Z moisture
Md
MWd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flow(acmm)
Flow(dscfm)
Flov(dscnm)
Z I
Z EA
80.6472
2.283929
39.48341
1.11817
32.86707
.6713293
29.02947
25.40441
3286.949
1002.119
143604.3
4066.873
65255.38
1848.032
105.7121
24.87104
Program Revision:I/16/84
A-20
-------
RADIAN SOURCE
EPA METHOD 2 -
( R A W DATA)
PLANT SITE 05
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST
TEST PERIOD
ESP INLET-NORTH DUCT
VELOCITY-2
02/27/85
PM
PARAMETER VALUE
Sampling time (min.) 160
Barometric Pressure (in.Hg) 30.22
Sampling nozzle diameter (in.) .242
Meter Volume (cu.ft.) 82.693
Meter Pressure (in.H20) 1.045
Meter Temperature (F) 93.53031
Stack dimension (sq.in.) 6291.25
Stack Static Pressure (in.H20) -4.5
Stack Moisture Collected (gm) 837.4
Absolute stack pressure(in Hg) 29.88912
Average stack temperature (F) 334.087
Percent C02 16.3242
Percent 02 3.8701
Percent N2 73.6014
Delps Subroutine result 22.66928
DGM Factor 1.0097
Pitot Constant .84
A-21
-------
RAD
EPA
FINAL
PLANT
PLANT SITE
SAMPLING LOCATION
TEST f
DATE
TEST PERIOD
IAN SOURCE
METHODS 2
TEST
5
RESULTS
SITE 05
ESP INLET-NORTH DUCT
VELOCITY-2
02/27/85
PM
PARAMETER
RESULT
Vm(dacf)
Vm(dscm)
Vw gas(scf)
Vw gas (acm)
Z moisture
Md
MWd
MV
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flov(acmm)
Flow(dscfm)
Flov(dscmm)
Z I
Z EA
80.6472
2.283929
39.48341
1.11817
32.86707
.6713293
29.02947
25.40441
3544.643
1080.684
154862.8
4385.713
69055.76
1955.659
99.89439
24.87104
Program Revision:I/16/84
A-22
-------
I
i onos
PLANT
PLANT SITE
SAMPLING LOCATION
TEST 4)
DATE
TEST PERIOD
: SITE 05
: CONFIDENTIAL , XX
3 ESP INLET
: 05VELN3
: O2/23/85 NORTH DUCT VELOCITY ONLY
: .1.055-16] 5
PARAMETER
RESULT
Vm
Vs (ntpm)
Flow
-------
PLANT
•PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
c AIM OO»_SF*:O:IE=:
: T H O O S --'
SITE O5
CONFIDENTIAL
ESP INLET
O5VELN3
02/28/35 NORTH DUCT VELOCITY ONLY
1.055-1615 :
PARAMETER
VALUE
Sampling time (min.)
Barometri c Pressure (in. r-lg)
Sampling nozzle diameter (in.)
Meter Volume (cu.ft.)
Meter Pressure tin.H2O>
Meter Temperature
Averaqe st=*ck temper-rai-iire (F)
Percent CO2
Percent O2
Perc-nt M2
De 1 p s Sub r ou 11 n <= r -s &.i 11
DGM Factor
Pi t-ot Constan':
2OO
30. 2
. 242
1O4.71
J. „ 068
^5. -3625
6291.25
-4.5
1037.9
29.86912
31O.4O91
75
22.16424
I .O097
.£34
A-24
-------
APPENDIX A-2
CONTINUOUS EMISSION MONITORING RESULTS
A-25
-------
-------
GEMS DATA - SITE 03 - TEST 1
»»
»•»
»»
»»
»»
»»
•»•»
»»
**
»•»
**
»»
»»
»#
»»
»*
»*
*»
»*
»*
»»
»»
»»
»»
»•
»*
»»
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**
**
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**
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»*
»*
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»*
»»
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»»
»*
**
»»
»»
NO. PTS.
MEAN
STD. DEV.
FACTOR
FOR 37. 02
NORMALIZATION
OF
OTHER PROCESS
GASES
mmmammmmmm
4.9247
4.1679
4. 4539
4.2133
4. 1990
4.2470
4.1913
2.9025
2. 1066
1.9387
2.0105
2.0477
1 . 9465
2.3404
1.9620
2. 2367
1.9542
2.0313
2. 0729
2.0909
2. 2073
2.0787
2.2942
2. 1434
2. 2260
2.4041
2. 1238
2. 1669
2.3614
2. 1961
2. 1919
• 2.3282
2. 1352
2. 2460
2. 1322
2. 1847
2.3219
2. 2008
2. 2608 •
2.3060
2.3409
2.3453
2.3763
2.3871
2.6014
2.3860
2. 4404
2. 276O
2.4169
2. 1742
2.1915
2.3887
2.1436
2. 1745
2. 4720
2.2016
2.2185
2.3994
2.2429
2.3830
2.2329
2.2767
2. 4977
2. 2044
2. 1906
2. 1830
2.0378
1 . 9445
1.9526
1.9197
2. 034S
1.8119
1 . 8089
2.1316
1 . 3870
2.0326
1 . 9023
77
2.4001
a. A,
»» NORMALIZED / CORRECTED DATA
**
»»
»* TIME
*«
»* _
*» 1330
»» 1333
»» 1400
»» 1405
»* 1410
*» 1413
»» 1420
•» 1423
*» 1430
»* 1433
»» 1440
** 1443
»» 1430
»» 1455
*» 1305
»» 1310
»» 1515
** 1520
** 1530
»» 1535
»* 1540
•• 1545
*« ' 1550
»« 1535
»* 1600
*•» 1605
»» 1610
»» 1615
*« 1620
** 1625
•* 1630
»» 1635
** 1640
** 1645
•» 1630
»* 1633
»» 1700
»* 1703
*» 1710
»* 1715
•» 1720
»* 1725
»» 1730
»» 1733
»» 1740
»» 1745
»» 1750
•» 1755
•* " iaoe
*« 1805
»• 1810
»• 1813
»* '1820
»» - 1825
•• 1830
*» 1335
** 1840
»» 1845
** 1850
»* 1333
»» . 1900
»» 1903
•» 1910
»« 1913
»* 1920
»» 1925
»* 1930
»» 1935
»* 1940
»» 1945
»» 1950
*» 1933
»* 2000
»* 2003
»• 2010
•• 2013
»» 2020
NO. PTS.
MEAN
STO. DEW.
02
(XV)
17.3
16.6
16.9
16.7
16.6
16.7
16.6
14.7
12.4
11.7
12.0
12.2
11.7
13.3
11.8
12.9
11.7
12.1
12.3
12.3
12.8
12.3
13.1
12.5
12.9
13.5
12.5
12.6
13.3
12.7
1-2.7
13.2
12.5
12.9
12.6
12.7
13.2
12.8
13.0
13.8
13.3
13.3
14.0
13.4
14.0
13.4
13.6
13.0
13.5
12.7
12.7
13.4
12.6
12.7
13.7
12.3
12.3
13.4
12.9
14.0
12.9
13.0
13.7
12.3
12.7
12.7
12.1
11.7
11.7
11.6
12.1
11.0
11.0
12.6
11.4
12.1
11.5
77
13. 1
1.4
CO
(PPMV)
7984.2
8163.7
9609.3
11103.7
10392.3
11137.4
10481.7
11990.3
10130.2
12236.4
11690.3
13042.9
12310.7
12314.9
12333.7
12071.7
12499.3
9672. 9
10274.7
11857.6
12323.3
11673.7
10461.3
12713.7
12369.3
10647.6
11316.3
9451.3
7144.6
5342. 7
6974.0
3031.2
7338.6
7637.7
7691.3
6237.3
7008. 4
3983. 4
3392.9
6391.3
7274. 2
6962. 1
8946. 0
7723.6
8828. 1
10404.0
11934.2
8036. 7
10373.2
10638. 1
12484.3
10729.3
12080.0
13999.7
13430.8
10673.2
9528.3
10387. 1
10720. 1
9063.7
8913.2
13175.0
13333.5
14537.2
14063.3
14415. O
13464.3
12037.3
12902.3
12382.5
13O65.S
12011.2
11999.2
14108.7
12333.2
12134.7
12323.8
77
10607.8
2337.9
C02
C/.V)
20.3
17.6
13.4
18.0
17.8
17.8
17.9
18.2
16.0
16.5
15.6
17.3
16.1
15.0
16.0
15.1
16.4
16.7
17.0
15.7
17.8
16.3
14.9
16.9
16.9
15.1
16.8
16.8
16.1
16.9
15.9
13.3
16.9
14.3
17.0
16.9
13.3
16.9
16.9
16.8
17.1
16.3
19.0
17.4
13.4
16.3
18.8
17.4
13.4
17.4
17.3
13.4'
17.2
16.9
19.6
17.3
16.3
19.1
17.4
13.6
17.4
17.5
15.5
17.4
16.6
13.5
17.4
15.3
17.9
17.1
18.6
17.0
17.0
21.6
16.9
13.3
17.3
77
17.0
1.2
-WITH ACTUAL 02
S02
fPPMV)
374.8
636.5
773.7
337.0
338.6
971.6
362.2
1109.7
884.8
1235.3
1062.6
1328.9
1325. 1
1270.8
1348.3
1541.7
1338.6
876.7
942.7
1136.3
1293.3
1185.0
1020. 4
1321.8
1336.9
1043.2
1094.0
987.4
821.0
627.0
730.8
833.2
770.1
665.2
699.7
602.4
636.4
.380.5
371.4
366.7
654.7
577.5
673.3
387.4
631.8
814.6
913.0
353.2
737.1
742.7
973.4
724.3
907.2
1209.2
1109.3
946.1
723.9
824.8
388.4
733.0
729.8
1164.9
1290.2
1323. 7
1401.3
1414.0
1212.9
961.2
938.9
887.6
966.4
1003. 1
1033.4
1262.0
1003.0
387.9
638.2
77
948.6
272.3
NOX
(PPMV)
84.7
66.4
65.6
62.6
62.9
63.4
64.6
30. 5
41.5
35.6
36.9
36.7
32.3
28.1
26.8
38.8
31.3
38.5
41.8
32.0
38.8
36.3
30.6
31.4
30.3
29.3
33.7
33.1
43.7
30.1
44.0
33.0
46.3
38.0
46.7
30.2
44.4
30.7
31.5
32.3
33.2
30.5'
39.6
54.1
43.0
42.1
43.6
31.5
35. O
46.5
37.0
36.3
37. 1
27.8
33.3
34.9
43.7
48.6
40.0
38.2
46.2
28.9
16.0
11.7
9.3
18.4
23.2
23.0
32.2
33.4
36.7
32.3
33.2
119.3
30.3
30.4
41.9
77
41.6
15.7
A-27
-------
CEHS DATA - SITE 05 •• TEST I
" " ' THIS DATA HAS NOT BEEN RCDOCED TO 3X 02
TIME
13SB
1333
1499
1493
1419
1413
1429
1423
1439
14T3
1449
1443
1439
1433
13(13
1383
1319
1313
1329
1323
1339
1333
1349
1343
1339
1333
1499
1493
1619
1413
1429
1623
1639
1633
1449
1443
1439
1433
1799
1793
1719
1713
1729
1723
1739
1733
1749
1743
. 1739
1733
1199
1583
1019
1813
1929
laiS
1839
1931
1849
1843
1939
1833
1989
1983
1919
1913
1729
1923
1939
1933
1949
1743
1938
1933
2399
2893
2919
2913
2929
2323
2339
2933
2949
2943
2339
2833
2109
2193
NO. PTS.
MEAN
STO. OEV.
02
(r.v>
17.3
14.4
14.9
14.7
16.6
16.7
16.6
14.7
12.4
11.7
12.0
12.2
11.7
13.3
11.8
12.9
11.7
12.1
12.3
12.3
12.8
12.3
13.1
12.3
12.9
13.3
12.3
12.6
13.3
12.7
12.7
13.2
12.3
12.9
12.6
12.7
13.2
12.8
13.9
13.8
13.3
13.3
14.9
13.4
14.9
13.4
13.4
13.9
13.3
12.7
12.7
13.4
12.4
12.7
13.7
12.8
12.8
13.4
12.9
14.9
12.9
13.9
13.7
12.9
12.7
12.7
12.1
11.7
U.7
11.6
12.1
11.0
11.9
12.6
11.4
12.1
11.3
77
13.1
1.4
CO
(ppnvi
1621.3
1939.2
2136.6
26.33.3
2474.9
2622.4
2309.8
4131.2
4819.3
6311.3
3914.3
6769. 4
6324. 6
3241.9
4738.3
3397.0
6396.3
4761.9
4936.8
3671.0
3673. 7
3616.8
4339.9
3933.9
3646.6
4428.9
3328.6
4341.7
3323.6
2432.8
3181.7
3438. 1
3340.9
3489.6
3373.9
2833.9
3913.4
2718.8
2333.3
2639.2
3197.3
2969.6
3471.8
3236.3
3393.6
4369. 4
4898.3
3331.9
4272.8
4902.9
3696.9
4471.8
3622. 4
6438.2
3141.3
4848.9
4294.9
4412.3
4779.6
3399.8
3792.7
3786.8
3338.3
6394. 7
6429. 1
6693.2
6697.3
6 170. .3
6697. 7
6334.3
6421.9
4629.9
6633.3
6337.2
6641.9
3979.9
6383.6
77
4677.7
1474.6
C02
(XVI
4.1
4.2
4.1
4.3
4.2
4.2
4.3
6.3
7.6
8.3
7.8
8.6
a. 3
6.4
8.2
6.7
a. 4
9.2
9.2
7.3
9.1
a. i
6.3
7.9
7.6
6.3
7.9
7.3
6.9
7.7
7.2
7.9
7.9
6.6
7.9
7.7
6.6
7.7
7.3
6.7
7.3
6.9
7.4
7.3
3.9
6.8
7.7
7.6
6.4
9.8
7.9
6.3
9.8
7.9
7.9
7.9
7.6
•f.f
7.7
6.8
7.8
7.7
6.2
7.9
7.6
8.3
9.3
8.1
9.1
8.9
9.1
9.4
9.4
10.9
a. 9
7. a
9.2
77
7.4
1.3
S02
(PPMVI
81.7
187.9
122.2
148.1
141.9
161.4
143.2
272.1
393.6
472.9
386.3
449.3
497.2
"74.7
376.3
382.2
381.3
313.3
329.3
376.2
422.4
413.3
323.9
444.3
43.3. 9
313.3
373.2
329.9
231.4
286.4
249.8
236.4
261.1
216.9
233.2
199.4
199.1
199.6
192.3
162.6
281.3
178.9
186.6
176.9
173.3
246.6
267.7
173.8
224.9
244.3
329.3
219.9
383.1
402.1
319.2
319.9
233.9
243.3
283.3
283.4
233.3
369.3
373.4
388.2
463.2
464.3
438.8
341.7
347.7
336.1
341.7
484.8
416.8
413.9
398.1
313.8
231.2
77
784.9
114.3
NO*
(PPMVI
17.2
13.7
14.7
14.8
13.8
M.-J
13.4
17.4
19.7
18.3
18.4
17.9
16.6
12.8
13.6
17. .3
16.8
19.8
28.2
13.3
17.6
17.4
13.3
14.6
13.7
13^7
16.2
18.3
22.8
28.1
22.8
21.7
16.7
21.7
23.9
19.1
23.1
22.8
21.1
21 1 3
23.1
22.7
16.3
17.7
18.7
22.6
14.3
21.4
16.9.
13.3
17.3
12.9
14.3
13.9
19.7
28.3
17.9
14.8 •
29.7
12.7 '
6.4
4.3 '
8.4
tl.4
11. a
16.3
17.4
18.9
17.9
13.4
33.4
16. 1 •
14.9
22.8
77
17.3
3.7
THC
(PPHV)
44.4
33.2
29.7
32.9
37.7
34.7
42.1
24.2
31.7
31.6
37.1
37.9
66.6
42. 3
'2.3
109.3
94.6
131.1
77.7
33.3
37.0
71.6
39.3
93. 1
29.1
16.6
19.4
22.7
21.9
17.3
78.3
29.2
32.7
64.8
33.3
31.6
24.3
39.4
49.1
79.2
47.2
33.7
33. I
49.2
48.3
33.2
78.3
179. 7
163.9
142.0
143.3
174.1
91.3
113.3
117. 1
96. 7
126.3
137.3
176.9
123.3
139.9
49.9
46.3
63 •*
66.9
43.7
A-28
-------
Cat* DAT* - SITC 9 - TEST Z
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12.7
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12.4
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12.3
12.3
12.3
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12.3
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12.3
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12.4
12.3
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13.7
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13.2
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3*.l
31.*
33.1
32.9
33.3
42.1
97.*
4*. 7
33.2
32.3
47.*
4*. 9
34.2
34.3
3*.*
43.9
33.1
34.3
29.3
3*.*
4*. 3
4*. 7
44.*
*!.*
3*.*
43.3
11.2
A-29
-------
CEHS DATA - SITE 3 - TEST I
TtnE
1113
• 11=9
11=3
1139
1133
1149
1143
1139
1133
1=99
1=93
1=19
1=13
i=:a
12=3
1279
1=33
1=49
1243
1=39
1233
1399
1393
1319
1313
13=9
1323
1339
1333
1349
1343
1339
1333
1499
1493
1419
1413
14=9
1423
1439
1433
1449
1443
1439
1433
1399
1393
1319
1313
1329
13=3
1339
1373
1349
1343
1339
1333
1609
U93
1619
1613
16=9
16=3
1679 •
1633
1649
1643
1639
1633
1799
1793
1719
1713
1729
1723
1779
1733
1749
1743
1739
1733
1899
1893
1819
1813
1829
1023
1*39
1833
1848
1343
1839
1833
1999
1993
1919
1913-
19=9
1923
1938
1933
NO. rr».
3TD. DCV.
' THIS
02
(XV)
12.9
13.8
12.9
12.7
12.7
12.3
12.6
12.3
12.4
12.3
12.4
12.4
12.7
12.7
12.7
12.8
12.7
12.6
1=.6
12.3
i=.a
12.3
12.3
12.3
12.6
12.3
12.3
12.9
12.1
12.9
12.9
12.3
13.4
12.1
12.3
12.2
12.1
12.3
12.1
12.4
12.3
12.3
12.9
12.4
12.4
13.9
12.4
12.4
12.3
12.4
12.4
12.4
12.6
12.7
12.7
12.4
12.7
12.6
l=.7
12.6
12.8
1=.8
t:.6
12.7
13.9
13.2
13. 1
13.9
13.2
IT. 3
13.3
13.2
11.3
13.3
13.4
13.6
13. Z
13.3
13.4
13.3
13.9
13.3
12.9
13.3
13.3
13.1
13.1
1.3.9
13.3
13.3
13.3
91
12.7
9.4
DBTfl HflS NOT BEEN REDUCED TO
CO C02 302
(PPMV1
676=. 7
3776.7
6718.3
6762.7
6762.7
6762.7
6762.7
6762.3
6742.7
6741.4
6698.3
6611.2
3963.6
3914.7
6336. 4
6737.4
6313.3
6733.8
6436.3
6297.9
3418.7
4793.9
3189.3
4=92.3
7346.4
3641.1
3793.9
7391.6
4441.9
4441.6
4963.3
3=43.9
6624.6
6733.7
3681.9
6347. 1
3439. 1
6649.3
6733.9
6762.7
6391.6
6294.3
3719.7
6382.6
6336.4
4889.9
6497. 4
6727.3
6762. 7
6698.2
6734.3
6437.3
6339.3
6413.6
3869.9
6198.9
6623.7
6499. 1
6699.2
6343.8
6373.8
6939.9
6973.7
6=19.3
33=9.8
6423.2
6642.9
6699.3
6364. 4
6137.3
3222.9
3=93.9
4233.3
7618.1
3942. 9
6996.1
3B32. 7
3136.4
3492.9
3627.8
3779. 7
4161.3
4729.7
37.31., 3
3393.6
6987.1
3194.9
3393.7
3399.6
3639. 9
6927.3
91
3879.6
383.8
8.6
7.3
8.9
9.1
9.3
9.2
9.2
9.1
9.3
9.4
9.6
9.4
8.1
9.2
9.9
9.1
8.9
9.1
9.8
9.3
8.9
9.3
9.3
8.2
9.2
9.1
9.3
9.3
9.6
9.8
9.3
8.4
9.3
9.3
7.9
9.3
9.3
9.3
9.2
9.1
9.1
9.9
7.7
9.4
9.9
7.3
9.2
9.1
9.1
9.9
9.2
9.2
8.9
8.8
9.9
3.9
3.8
9.1
8.9
3.6
8.8
a. a
3.3
9.9
3.6
8.9
3.4
9.6
8.3
8.4
7.3
3.4
8.2
7.4
3.1
8.3
3.7
a. 2
8.2
8.4
3.7
7.9
3.6
8.4
6.9
3.4
9.3
3.4
8.2
7.7
8.1
91
a.a
9.6
433.8
713.1
377.2
437.4
428.1
463.6
473.8
4=8.4
336.6
4=6.3
348.9
336.9
348.9
=94.9
279.9
414.8
=68.9
312.4
3=1.6
719.3
=93.9
222.1
==?. 9
191.9
169.1
133.4
164.4
147.1
136.7
219.3
2-7.2
242.2
296.1
396.7
277.3
769.2
246.3
493.8
449.9
339.9
742.2
=33.3
=38.1
393.9
321.7
=94.7
337.9
376.8
439:4
449.1
398.9
794.9
797.8
372.3
731.9
741.2
493.3
492.3
471.9
733.4
379.6
3=7.8
722.6
3=6. 1
=34.8
374.1
413.4
379.3
341.7
317.9
=89.3
=39.1
173.9
138.7
3=3.7
744.3
=41.3
=62.9
=99.2
717.9
274.6
144.7
=96.2
=33.9
=63.7
313.3
=37.3
=36.9
268.4
272.4
734.3
91
718.9
as. 3
3X 02 '
NO*
(PPMV)
14.3
17.6
16.9
14.3
13.7
14.3
14.3
ti.r
13.9
14.6
13.3
17.6
14.3
:=.=
16.3
14.3
16.9
19.9
18.3
=9.9
18. 7
38.1
=6.1
26.9
34.3
34.3
76.6
37.1
77.3
74.3
79.9
=4.3
23.4
=8. a
=8.3
==.9 '
=8.4
=1.3
29.7
16. »
=9.8
21.8
18.9
22.4
=9.3
22.2
31.9
17.7
13.4
14.4
17.9
19.3 .
17.1
is. a
19.7
17.9
14.4
is.:
14.3
14.6
is.a
14.8
14.7
16.8
19.4
M.3 '
13.1
14.9
14.3
14.9
13.3
13.9
=3.6
=8.7
13.9
1.3.3
=9. 1
16.9
13. 1
13.3
17.2-
19.4
=3.7
13.7
12.6
17.4
=1.7
21.3
19.8-
17.4
16.3'
•«•••*«•«:
91
19.3
3.7
THC
(PPHV)
143.2
74.4
37.1
97.9
111.3
47.9
182.3
39.9
28.3
39.9
92.9
96.3
68.9 ;
48. a
77.2
=9.4
7=. 1
~7.8
76.1
73.7
31.4
46.9
73.4
43.9
41.2
44.8
=6.6
=4.1
=9.6
19. .7
= 4.3
3a.6
48.2
37.4
34.7
74.3
44.7
.33.7
37.6
73.7
62.7
93.1
78.8
77.9
111.8
72.8
38.3
,. =4.3
=3.=
67.6
93.7
176. 3
96.3
93.6
187.4
68.1
73.1
71. =
41.3
91.4
34.3
86.4
42.8
41.4
3=. 7
47.8
39. I
43.6
33. a
33.6
39.2
32.2
38. 1
73.9
43.2
49. t
37.3
67.8
42. a
71.7
31 .3
31.4
77.=
43.9
46.3
69.4
196.8
69.3
69. 9
49.7
199.3
1=6.9
93
39.2
=7.8
A-30
-------
CEMS DATA - SITE 05 - TEST 3
*»
»*
*•»
»»
»*
*!
»*
»*
»»
»•
»»
»»
»»
»»
»»
**
»»
»*
»»
»*
»*
»*
*•»
»*
»»
»*
*»
»*
**
»•
»»
»•
»»
»*
**
**
»»
»*
»»
»»
*»
**
**
**
**
»«•
»»
**
»*
**
»»
*•
*•»
»»
*»
*
*
»
»
*
»»
»*
»*
»»
*•»
*•»
•»*
»» ««
»»
**
NO. PTS.
MEAN
STD. DEV.
FACTOR
FOR 3X 02
NORMALIZATION
OF
OTHER PROCESS
QASES
..........
1.9302
1.9064
1.7693
1 . 9766
1.9603
1.3271
1.7729
1.3138
1 . 3495
1 . 3309
1.7616
1 . 7825
1.3407
1.7488
1.7594
1 . 8303
1.7404
1.9287
1.7511
2.0009
2.0043
1.7819
1 . 7849
1.7531
1.8191
1 . 7673
1.6925
1.6899
1.7998
1.6797
1 . 706S
1.7441
1.6942
1 . 674S
1.6939
1.7033
1.7763
1.8333
. 1.7749
2.5798
1.7323
1 . 8242
1.7537
1 . 7539
1.7514
1.7623
1 . 7557
1 . 7441
1 . 7783
1.8733
1 . 7437
1 . 7633
1.3773
1.3245
1 . 7606
1.7384
1.7896
1.7875
1 . 7896
1.7812
1.9648
1.7902
1.7961
1.3666
64
1.8031
0.1
»*
**
**
»*
" »*
»*
**
»*
»•»
»»
»*
**
•*
»*
»»
»»
**
»•
*•»
**
•»*
»*
»*
**
*»
»»
»»
»»
»*
••
**
»»
**
•»
**
»»
**
**
»*
*»
**
»»
**
»*
»•»
»*
»»
»»
**
»»
»»
»*
•»»
•»•»
»*
»»
••»
**
**
»*
**
**
**
»»
»»
»*
»»
»•
»»
NORMALIZED / CORRECTED DATA
TIME
....... ..•
1100
1103
1110
1113
1120
1125
1130
1135
1140
1145
1130
1155
1200
1205
1210
1215
1220
1225
1230
•1235
1240
1245
1250
1233
1300
1303
1310
1313
1320
1325
1330
1335
1340
134S
1330
1355
1400
1405 '
1410
1415
1425
1430
1435
1440
1445
1450
1433
1300
1303
1510
1313
1320
1323
1330
1335
1340
1345
1330
1555
1600
1605
1610
1615
1620
NO. PTS.
MEAN
STD. OEV.
02
(XV)
••Maim
11. 1
11.0
10.8
11.4
11.3
11.1
10.3
11.0
11.2
11.1
10.7
10.9
11.2
10.7
10.7
11.1
10.6
11.6
10.7
12.0
12.0
10.9
10.9
10.7
11.1
10.8
10.3
10.3
11.0
10.2
10.4
10.6
10.3
10.2
10.3
10.4
10.8
11.2
10.8
14.0
10.6
11. 1
10.7
10.7
10.7
10.7
10.7
10.6
10.8
11.4
10.6
10.8
11.4
11.1
10.7
10.9
10.9
10.9
10.9
10.9
11.3
10.9
10.9
11.3
64
10.9
0.5
CO
(PPMV)
....... a
10385.5
11335. 1
9441.5
7313.7
11352.9
11792.3
10970.6
9460. 2
11735.0
10351.0
• 9042.6
9324. 1
9493.2
10148.2
9232. 7
11733.0
7483.7
3037.7
5063. 4
5528.7
3588.6
2181.1
2028.2
2832.6
2371.1
2808. 7
9232.6
7931.2
7698. 2
10026.2
10693. 0
10893.8
11007.6
10733.3
11010.9
11014.3
3750.5
11912.9
11513.3
3318.6
11065.3
11181.0
• 11313.1
11329.6
11339.5
1 1407. 5
11333.3
11283.4
11302.6
10964.7
10323.3
11342.2
11132.0 -
9906.3
11132.1
11321.7
11314.2
11168.3
10636.2
7464.2
6946.6
7620. 1
9693.3
9310.1
64
9210.4
2793. 7
C02
(XV)
tmmmmmm
13.3
17.9
17.3
14.8
16.7
17.1
16.9
14.4
17.9
17.1
16.9
13.9
13.3
16.9
13.3
17.8
16.3
14.4
16.7
17.4
17.1
16.8
16.1
16.7
14.1
16.4
16.6
16.4
14.6
16.3
16.6
16.4
16.3
16.1
16.4
16.2
7.3
18.2
17.6
0.9
16.4
16.3
16.4
16.2
16.8
16.4
16.3
16.8
16.3
13.2
16V-6
16.6
16.3
16.3
16.6
17.1
16.6
16.6
16.9
16.5
16.3
16.6
16.8
16.7
64
16.1
2.4
-WITH ACTUAL 02
S02
(PPMV)
.......
491.2
646.6
337.6
349.7
693.6
662.4
321.3
453.7
533.1
395.0
540.3
524.4
561.2
571.6
317.5
718.5
523.6
333.0
329.3
366.3
392.7
335.0
293.5
369.8
307.0
363.2
644.4
532.2
477.7
622.7
613.4
679.3
772.3
790.2
603.0
655.1
401.1
680.8
344.5
206.9
358.9
608.4
646.0
720.0
637.6
741.2
782.6
733.2
333.1
671.4
393.4
684.8
756.2
521.4
335.0
572.0
665.5
648.2
617.5
303.7
439.2
409.5
594.5
476.3
64
363.3
143.9
NOX
(PPMV)
31.3
32.7
41.9
37.2
34.2
36.1
38.6
32.3
37.1
40.7
42.3
32.0
43.1
40.3
37.9
41.3
33.3
30.4
54.6
39.2
38.0
70.0
66.3
62.0
33.7
55.5
47.3
51.6
43.8
46.3
43.4
42.2
38.7
38.3
40.5
42.2
21.9
49. 1
49.2
44. 1
47.7
42.7
40.4
41.8
39.4
33.4
35.8
34.4
32.3
44.6
32.7
37.0
45.0
39.9
40.2
41.7
44.3
47.6
57.0
56.0
55. 1
46.2
49.3
63
44.0
9.1
A-31
-------
CEMS OATA - SITE 5 - TEST 3
......... THIS DATA HAS NOT BEEN REDUCED TO 37. 02
TIME
naa
11B3
ma
1113
n:a
1 113
11*9
tt33
mo
1143
lisa
1133
i2aa
1=83
t:ia
t=t3
12:9
12=3
1238
1213
1=49
1=43
1=38
1=33
i3»9
1333
i3ta
1313
1319
1323
1339
1313
1349
1343
1339
1333
1408
14*3
1418
1413
i4=a
1423
i43a
1433
144*
1443
1439
1433
ISM
1313
ista
1313
ts:a
13=3
1339
1533
1349
1343
issa
1333
16B8
1683
16 ia
1413
16=8
1623
1633
1633
1649
1643
1639
NO. PTS.
MEAN
STD. DCV.
02 CO
(XVI (PPT1V)
11.1 3674.
11. E
19. E
11.'
11. e
it.
ta.E
it. i
11.:
11.
ia.;
19.1
11.:
19.-
IB.;
11.
19. i
it. t
IB.'
12. i
12.1
19."
19.1
19.
11.
ta.E
ia.:
19.,
11. i
ia.:
19.'
19.4
if.'
18.:
19.-
18.
ia.t
it.:
la.E
14.1
18.4
11.
19.
19."
19.'
19.'
19.'
19.
19.
11.
18.
ta.
it.
11.
18.
ta.
18.
ia.
ia.
ia.
it.
ia.
ta.
n. •"
1 6331.
1 3333.
1 4884.
1 3791.
6434.
1 6108.
1 328*.
: 6343.
3762.
' 3133.
t 3343.
'. sisa.
' 3B83.
• 3247.
64ta.
> 4391.
> 2612.
r 2391.
1 2763.
1 2787.
f 12=4.
' 1136.
T i6is.
1393.
i 1389.
[ 3484.
S 4723.
1 4277.
2 3*6*.
> 6263.
i 6246.
! 6497.
! 6423.
; 64*2.
I 6466.
1 3237.
J 6427.
i 6486.
1 1296.
b 6397.
61=7.
' 6438.
' 6441.
r 6474.
' 6473.
r 6468.
646*.
6467.
3947.
6828.
64=3.
3928.
342*.
6323.
6442.
6.322.
6249.
3734.
4198.
3333.
4236.
3392.
! 4432.
6
7
7
a
4
2
a
9
1
7
3
2
4
1
6
4
1
a
6
t
6
a
3
a
4
i
6
a
3
2
9
2
3
1
6
9
3
»
a
4
6
3
9
2
7
m
1
3
a
a
3
2
3
9
1
3
3
3
6
3
3
7
3
a
64 64
18.1
' 3147.
a. 3 16=9.
a
7
C02
17.1
ta.
23.
19.
17.
19.
=1.
17.
=a.
22.
24.
18.
=4.
23.
=1.
=2.
31.
26.
31.
=9.
=a.
39.
37.
33.
=9.
31.
27.
39.
24.
27.
=6.
=4.
22.
22.
23.
24.
12.
=6.
27.
23.
26.
24.
23.
23.
22.
19.
29.
19.
17.
=3.
18.
19.
=4.
22.
22.
=3.
23.
26.
32.
=8.
3a.
23.
=6.
1
7
a
3
a
a
3
1.
T
3
a
3
1
3
7
a
i
2
6
9
3
3
4 '
3
4
9
3 •
3.
a
6 •
2
9
9
9
a
3
3
7
4
2
4
a
9
3
a
3
4
2
6
3.
7
7
7
3
3
1
6
a
3-
a
7
7
63
24.
3.
6
a
THC
(PPMV)
64.
39.
77.
37.
43.
36.
61.
46.
43.
43.
36.
33.
SB.
36.
34.
SI.
34.
46.
11.
6.
19.
28.
43.
7.
9.
7.
13.
11.
9.
39.
24.
62.
31.
33.
48.
41.
46.
a.
33.
42.
43.
31.
338.
231.
38.
49.
33.
42.
33.
34.
T6.
39.
63.
47.
68.
63.
59.
46.
34.
64.
37.
49.
61.
31.
19.
13.
23.
=*.
17.
3
7
2
9
a
i
8
7
3
7
7
6
7
3
4
3
1
a
3
3
6
2
7
2
3
a
2
9
9
3
1
3
2
2
6
9
6
1
a
4
4
4
3
3
a
a
i
a
a
7
4
3
6
4
a
3
4
9
6
3
3
7
3
a
9
1
I
7
69
46.
46.
9
a
A-32
-------
APPENDIX A-3
HC1 TRAIN RESULTS
A-33
-------
_
-------
RADIAN SOURCE
EPA METHOD 2 -
( R A W DATA)
SITE 05
TEST
PLANT
PLANT SITE
SAMPLING LOCATION
TEST f
DATE
TEST PERIOD
ESP OUTLET
05-HCL-E-01
02/26/85
1448-1648
PARAMETER VALUE
Sampling time (min.) 120
Barometric Pressure (in.Hg) 30.22
Sampling nozzle diameter (in.) .247
Meter Volume (cu.ft.) 47.60401
Meter Pressure (in.H20) .4908333
Meter Temperature (F) 95.25
Stack dimension (sq.in.) 16286.05
Stack Static Pressure (in.H20) -.6
Stack Moisture Collected (gm) 451.7
Absolute stack pressure(in Hg) 30.17588
Average stack temperature (F) 313.6667
Percent C02 14.1003
Percent 02 . 5.8937
Percent N2 74.5374
Delps Subroutine result 14.21983
DGM Factor .9924
Pitot Constant .84
A-35
-------
SITE 05
RADIAN SOURCE
EPA METHODS 2
FINAL RESULTS
PLANT
PLANT SITE
SAMPLING LOCATION
TEST *
DATE
TEST PERIOD
TEST
5
ESP OUTLET
05-HCL-E-01
02/26/85
1448-1648
PARAMETER
RESULT
Vm(dscf)
Vm(dscm)
Vv gas(scf)
Vw gas (scm)
Z moisture
Md
MWd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flow(acmm)
Flow(dscfm)
Flov(dscmm)
Z I
Z EA
45.42835
1.286531
21.29766
.6031496
31.91808
.6808193
28.96059
25.46218
2210.359
673.8898
249986.2
7079.609
117145.7
3317.565
109.9023
42.75701
Program Revision:1/16/84
A-36
-------
RADIAN SOURCE
EPA METHOD 5
PARTICULATE LOAD
PLANT SITE 05
PLANT SITE
SAMPLING LOCATION
TEST *
DATE
TEST PERIOD
TEST
ING
ESP OUTLET
05-HCL-E-01
02/26/85
1448-1648
PARAMETER
FRONT-HALF
TRAIN TOTAL
Total Grams
Grams/dscf
Grams/acf
Grains/dscf
Grains/acf
Grams/dscm
Grams/acm
Pounds/dscf
Pounds/acf
Pounds/Hr
Kilograms/Hr
0
0
0
0
0
0
0
0
0
1
0034700
0000764
0000358
0011786
0005523
0026971
0012639
0000002
0000001
1838280
0.5369808
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
o.ooooooo
* BACK-HALF IMPINGER ANALYSIS WAS NOT REQUIRED
Program Revision:I/16/84
A-37
-------
RADIAN SOURCE
EPA METHOD 2-
DATA)
SITE 05
TEST
(RAW
PLANT
PLANT SITE
SAMPLING LOCATION
TEST *
DATE
TEST PERIOD
OUTLET - HCL
05-HCL-E-02
02/27/85
1306-1506
PARAMETER VALUE
Sampling time (min.) 120
Barometric Pressure (in.Hg) 30.2
Sampling nozzle diameter (in.) .247
Meter Volume (cu.ft.) 53.034
Meter Pressure (in.H20) . . .6208333
Meter Temperature (F) 82.45835
Stack dimension (sq.in.) 16286.05
Stack Static Pressure (in.H20) -.6
Stack Moisture Collected (gm) 525.9
Absolute stack pressure(in Hg) 30.15589
Average stack temperature (F) 313.6667
Percent C02 14.6
Percent 02 5.4
Percent N2 75.4
Delps Subroutine result 15.93428
DGM Factor .9924
Pitot Constant .84
A-38
-------
B. A. D IAN
SOU
EPA
METHOD
R C
S
T
5
E S T
FINAL
PLANT
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
RESULTS
SITE 05
OUTLET - HCL
05-HCL-E-02
02/27/85
1306-1506
PARAMETER
RESULT
Vm(dscf)
Vm(dscm)
Vw gas(scf)
Vw gas (sen)
Z moisture
Md
MVd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flov(acmm)
Flow(dscfm)
Flow(dscinm)
Z I
Z EA
51.78572
1.466571
24.79619
.702228
32.37865
.6762135
29.264
25.61687
2470.184
753.105
279371.8
7911.81
129944.2
3680.02
112.943
37.227
Program Revision:I/16/84
A-39
-------
RADIAN SOURCE
EPA METHOD 5
PARTICDLATE LOAD
PLANT SITE 05
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
TEST
ING
OUTLET - HCL
05-HCL-E-02
02/27/85
1306-1506
PARAMETER
FRONT-HALF
TRAIN TOTAL
Total Grams
Grams/dscf
Grams/acf
Grains/dscf
Grains/acf
Grama/dscm
Grama/acm
Pounds/dacf
Pounds/acf
Pounds/Hr
Kilograms/Hr
0.0009200
0.0000178
0.0000083
0.0002741
0.0001275
0.0006273
0.0002918
0.0000000
0.0000000
0.3054180
0.1385367
0.0008500
0.0000164
0.0000076
0.0002533
0.0001178
0.0005796
0.0002696
0.0000000
0.0000000
0.2821797
0.1279959
Program Revision:1/16/84
A-40
-------
RADIAN SOURCE
EPA. METHOD 2 -
( R A W DATA)
PLANT
PLANT SITE
SAMPLING LOCATION
TEST *
DATE
TEST PERIOD
TEST
SITE 05
ESP OUTLET
05-HCL-E-03
02/28/85
953-1053
PARAMETER
VALUE
Sampling time (min.)
Barometric Pressure (in.Hg)
Sampling nozzle diameter (in.)
Meter Volume (cu.ft.)
Meter Pressure (in.H20)
Meter Temperature (F)
Stack dimension (sq.in.)
Stack Static Pressure (in.H20)
Stack Moisture Collected (gm)
Absolute stack pressure(in Hg)
Average stack temperature (F)
Percent C02
Percent 02
Percent N2
Delps Subroutine result
DGM Factor
Pitot Constant
120
30.22
.247
52.22296
.6008333
87
16286.05
-.6
509.7
30.17588
315.5833
15.3
5.3
75.7
15.5216
.9924
.84
A-4r
-------
RADIAN SOURCE TEST
EPA METHODS 2-5
FINAL RESULTS
PLANT SITE 05
PLANT SITE
SAMPLING LOCATION ESP OUTLET
TEST # 05-HCL-E-03
DATE 02/28/85
TEST PERIOD 953-1053
PARAMETER
RESULT
Vm(dscf)
Vm(dscm)
Vw gas(scf)
Vv gas (scm)
Z moisture
Hd
MWd
MW
Vs(fpm)
Vs (mpm)
Flow(acfm)
Flqw(acmm)
Flow(dacfm)
Flow(dscmm)
I I
Z EA
50.60136
1.43303
24.03236
.6805963
32.2004
.677996
29.624
25.88102
2393.105
729.6052
270654.4
7664.932
125992.9
3568.118
113.821
36.09175
Program Revision:I/16/84
A-42
-------
RADIAN SOURCE
EPA METHOD 5
PARTICULATE LOAD
PLANT SITE 05
PLANT SITE
SAMPLING LOCATION
TEST #
DATE
TEST PERIOD
TEST
ING
ESP OUTLET
05-HCL-E-03
02/28/85
953-1053
PARAMETER
FRONT-HALF
TRAIN TOTAL
Total Grams
Grama/dacf
Grams/acf
Grains/dscf
Graina/acf
Grams/dscm
Grams/acm
Ppunds/dscf
Pounds/acf
Pounds/Hr
Kilograms/Hr
0.0034400
0.0000680
0.0000316
0.0010490
0.0004883
0.0024005
0.0011174
0.0000001
0.0000001
1.1331880
0.5140109
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
0.0000000
* BACK-HALF IMPINGER ANALYSIS WAS NOT REQUIRED
Program Revision:1/16/84
A-43
-------
-------
APPENDIX A-4
MODIFIED METHOD 5 SAMPLE CALCULATIONS
A-45
-------
-------
RADIAN SOURCE TEST
SPA METHOD 2-5
SAMPLE CALCULATION
PLANT
PLANT SITE
SAMPLING LOCATION
TEST *
DATE
TEST PERIOD
SITE-07
BAGHOUSE INLET
07-MH5-BI-01
04/16/85
1444-1604 1642-1657 1740-2005
Vm(std)
Vm(std)
1) Volume of dry gas sampled at standard conditions (68 deg-F ,29.92 in. flg)
Y x 7m x [T(std) + 460] x [Pb +(Pm/13 .6)]
P(std) x (Tm + 460)
1.001 x 130.845 x 528 x [ 29.98 + ( 1.066875 /13.6)1
29.92 x ( 77.3021 + 460)
Vm(std) - 129.304dscf
2) Volume of water vapor at standard conditions:
Vw(gas) - 0.04715 cf/gm x W(l) gm
Vv(gas) - 0.04715 x 375.2 » 17.691 scf
3) Percent Moisture in stack gas :
100 x Vv(gas)
•Vm(std) + Vw(gas)
100 x 17.691
_ 12.03 Z
129.304 + 17.691
4) Mole fraction of dry stack gas :
100 - ZM 100 - 12.03
———————————— m ____________ m
100 100
ZM
ZM
Md -
8796508
A-47
-------
SAMPLE CALCULATION
PAGE TWO
5)Averag@ Molecular Weight of DRY stack gas :
MWd - (.44 x ZC02) + ( .32 x Z02) + (.28 x ZN2)
MWd - (.44 x 7.6 ) + (.32 x 13.3 ) + (.28 x 79.1 ) - 29.748
6)Average Molecular Weight of vet stack gas :
MW - MWd x Md + 18(1 - Md)
MW - 29.748 x .8796508 + 18(1.- .8796508 ) - -...28.33414
7) Stack gas velocity in feet-per-ainute (fpm) at stack conditions :
Vs - KpxCp x [SQRT (dP)]Savet x SQRT [Ts Savgt] x SQRT [l/(PsxMW)] x 60se<
Vs - 85.49 x .84 x 60 x 19.90611 x SQRT[l/( 29.61971 X 28.33414 )]
Vs - 2960.649 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)
2960.649 x 4320 x .8796508 x528x 29.61971
144 x 931.4792 x 29.92
Qsd « 43842.81 dscfm
Qsd
Qsd
A-48
-------
SAMPLE CALCULATION
PAGE THREE
9)Isokinetic sampling rate (Z) :
Dimensional Constant C - K4 x 60 x 144 x [1 / (Pi /4)]
K4 - .0945 FOR ENGLISH UNITS
IZ
IZ
C x Vm(std) x (Ts + 460)
Vs x Tt x Ps x Md x (Dn)»2
1039.574 x 129.3039 x 931.4792
2960.649 x 240 x 29.61971 x .8796508 x( .254 )°2
IZ - 104.8296
10) Excess air (Z) :
100 x Z02 100 x 13.3
EA - — »
(.264 x ZN2) - Z02 (.264 x 79.1 ) - 13.3
EA - 175.41
11) Particulate Concentration :
Cs - ( grams part.) / 7m(std) - 0 / 129.3039
Cs »
Ca -
Ca -
Ca -
LBS/HR
LBS/HR
LBS/HR
0.0000000 Grams/DSCF
T(std) x Md x Ps x Cs
P(std) x Ts
528 x .8796508 x 29.61971 x 0.0000000
29.92 x 931.4792
0.0000000 Grams/ACF
Cs x 0.002205 x Qsd x 60
O.OOOOOOOx 0.002205 x 43842.8 x 60
Program Revision:I/16
A-49
-------
CALCULATIONS - DEFINITIONS
OF TERMS AND SAMPLE CALCULATION
A-51
-------
PARAMETER
RADIAN SOURCE
EPA METHODS 2
DEFINITIOH OF
DEFINITION
TEST
5
TERMS
Tt(min.)
Dn(in.)
Ps(in.H20)
VmCcu.ft .)
Vw(gm.)
Pm(in.H20)
Tm(F)
Pbdn.Hg.)
Z C02
Z 02
Z M2
SQR(DELPS)
As(sq . in.)
Ts(F)
Vm(dscf)
Vm(dscm)
Vv gas(scf)
Z moisture
Md
MWd
MW
Vs(fpm)
Flow(acfm)
Flow(acmm)
Flov(dscfm)
Flov(dscmm)
Z I
Z EA
DGM
Y
*g
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. PRODUC
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. C
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 LB/LB-MOLE
MOLECULAR WEIGHT OF STACK GAS,WET BASIC LB/LB-MOLE
AVERAGE STACK GAS VELOCITY
AVERAGE STACK GAS FLOW RATE(ACTUAL STACK COND.)
AVERAGE STACK GAS FLOW RATE(ACTUAL STACK COND.)
AVERAGE STACK GAS VOLUMETRIC FLOW RATE(DRY BASIS)
AVERAGE STACK GAS VOLUMETRIC FLOW RATE(DRY BASIS)
PERCENT ISOKINETIC
PERCENT EXCESS AIR IN STACK GAS
DRY GAS METER
DRY GAS METER CORRECTION FACTOR
STACK STATIC GAS PRESSURE
PITOT COEFFICIENT
ORIFICE PLATE DIFF. PRESS. VALUE
PITOT DIFF. PRESS. VALUE
Temperature - 68 deg-F (528 deg-R)
Pressure - 29.92 in. Hg.
A-53
-------
-------
APPENDIX B
SAMPLE SHIPMENT LETTERS
-------
-------
March 1,1985
U. S. EPA ECC Toxicant Analysis Center
Building 1105
Bay St. Louis, MS 39529
Attention: Danny McDaniel
Subject: Tier 4 - Analysis Instructions
Dear Sir:
The objective of this letter is to clarify instructions and
priorities for individual samples from specific Tier 4 combustion
sites. This instruction letter is Mo. 5 and pertains to EPA Site
No. 05 at Brunswick GA.
Episode No. is 2612, and SCC numbers assigned to this
numbers DQ001400 through DQ001499.
SCC numbers DQ001401 through DQ001406 have
been assigned to Troika for internal QA/QC purposes.
DQ001407 through DQ001422 have been assigned to
samples included in this shipment and number DQ001418
have been assigned to samples being archived at Radian
remaining SCC numbers are unused.
SCC numbers
All
The sample shipment for EPA Site No. 05 consists of 6
boxes containing 57 samples in 65 containers.(Note-The Modified
Method 5 samples are comprised of 6 components as listed
below.Some MM5 sample runs have more than one container per
component as indicated by asterisk.) The sample shipment was
shipped air freight on March 1st,1985 by Federal Express under
Airb-ill(s) No.770332511 and No.544545466
Instructions for extraction and analysis follow.
1. The following samples require immediate extraction
and analysis (Priority #1 samples).
Radian Run J05-MM5-E-01
(Total of 6 train components)
SCC
DQ001408
DQ001408
DQ001408
DQ001408
DQ001408
DQ001408
Component
1
2*(2
3
4
5
6
containers)
Fract ion
Filter
Probe Rinse
Back Half/Coil Rinse
Condensate
Impinger Solution
XAD Module
B-l
-------
Radian Run # 05-MM5-D-01
(Total of 6 train components)
SCO *
DQ001409
DQ001409
DQ001409
DQ001409
DQ001409
DQ001409
Component s
1
2
3
4
5
6
Frac t ion
Filter
Probe Rinse
Back Half/Coil Rinse
Condens ate
Impinger Solution
XAD Module
Radian Run # 0.5-MM5-D-02
(Total of 6 train components)
SCC #
Components
DQ001411
DQ001411
DQ001411
DQ001411
DQ001411
DQ001A11
1
2
3
4*(2
5*(2
6
container)
container)
Radian Run *05-MM5-E-BL
(Total of 6 train components)
SCC #
DQ001412
DQ001412
DQ001412
DQ001412
DQ001412
DQ001412
Components
1
2
3
4
5
6
Fract ion
Filter
Probe Rinse
Back Half/Coil Rinse
Condensat e
Impinger Solution
XAD Module
Fract ion
Filter
Probe Rinse
Back Half/Coil Rinse
Condensate
Impinger Solution
XAD Module
Radian Run # Q5-MM5-D-BL
(Total of 6 train components)
SCC
DQ001413
DQ001413
DQ001413
DQ001413
DQ001413
DQ001413
Component s
1
2
3
4
5
6
Fraction
Filter
Probe Rinse
Back Half/Coil Rinse
Condensat e
Impinger Solution
XAD Module
Radian Run # 05-MM5-E-02
(Total of 6 train components.)
B-2
-------
sec #
Component a
Tract ion
DQ001414
DQ001414
DQ001414
DQ001414
DQ001414
DQ001414
1
2*(2
3
4*(2
5
6
containers)
containers)
Radian Run # 05-MM5-D-03
(Total of 6 train components)
SCC #
DQ001415
DQ001415
DQ001415
DQ001415
DQ001415
DQ001415
Component a
I
2
3
4*(2
5*(2
6
containers)
containers)
Radian Run # 05-MM5-E-03
(Total of 6 train components)
SCC #
DQ001416
DQ001416
DQ001416
DQ001416
DQ001416
DQ001416
Component s
1
2
3
4*(2
5
6
containers)
Filter
Probe Rinse
Back Half/Coil Rinse
Condensat e
Impinger Solution
XAD Module
Fraction
Filter
Probe Rinse
Back Half/Coil Rinse
Condens ate
Impinger Solution
XAD Module
Fract ion
Filter
Probe Rinse
Back Half/Coil Rinse
Condens ate
Impinger Solution
XAD Module
Radian train proof (cleaned unused field sampling glassware train
components.) The proof train consists of the following fractions:
SCC #
COMPOMENT
FRACTION
DQ001419
DQ001419
DQ001419
The following
1 analys is.
DQ001421
DQ001422
DQ001420
2-5
1
6
Methylene Chloride Rinse
Hexane Extracted Filters (2)
Sorbent Module
field solvent blanks are also included for priority
05-ACETONE-FBL-A
05-H20-FBL-A
05-MeCL-FBL-A
Acetone
HPLC Water
Methylene Chloride
B-3
-------
2.
The strong black liquor samples are the only Priority
samples* They should be held for analysis by Troika
•pending the results of Priority #1 sample analysis.
sec *
DQ001407
DQ001410
DQ001417
05-SBL-01-A
05-SBL-02-A
05-SBL-03-A
Sample
Strong black liquor
Strong black liquor
Strong black liquor
The soil sample is the only Priority #3 sample. It will
be held by Radian for analysis by Troika pending the results
of Priority fl and Priority #2 sample analyses.
. SCO #
DQ001418
Sample
05-S-A Soils
If there are any questions concerning this sample shipment
please contact either Bob Jongleux or Vinton Kelly at Radian
Corporation (919) 481-0212 or (919)-541-9100.
S incerely,
DiR
cc.E. Hanks-EPA/AKTB
A. Miles-Radian
B-4
-------
APPENDIX C
DIOXIN/FURAN ANALYTICAL DATA FOR MODIFIED METHOD 5 TRAINS
-------
-------
-TABLE C-l. DIOXIN/FURAN ANALYTICAL DATA FOR MM5 TRAINS (INLET)
Isomer/Homolgue
Amount Detected, Picograms Per Sample Train'
Run 01 Run 02 Run 03
Dioxins
2378 TCDD
Other TCDD
Penta COD
Hexa CDD
Hepta CDD
Octa CDD
Total PCDD
Furans
2378 TCDF
Other TCDF
Penta CDF
Hexa CDF
Hepta CDF
Octa CDF
Total PCDF
0
0
0
0
400
1600
2000
100
100
0
200
100
100
600
0
0
0
0
2100
6700
8800
0
0
0
300
1000
700
2000
0
0
0
600
19600
98600
118800
200
1300
0
700
1800
1300
5300
Value - amount detected in MM5 sample train.
C-l
-------
TABLE C-2. DIOXIN/FURAN ANALYTICAL DATA FOR MM5 TRAINS (OUTLET)
Isomer/Homolgue
Amount Detected, Picograms Per Sample Traina
Run 01 Run 02 Run 03
Dioxlns
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
0
0
0
500
900
2800
4200
0
700
0
1900
700
200
3500
0
0
0
0
700
2300
3000
0
0
0
0
300
200
500
0
0
0
300
700
2400
3400
100
300
0
600
400
200
1600
Value - amount detected in MM5 sample train.
C-2
-------
APPENDIX D
RUN-SPECIFIC DIOXIN/FURAN EMISSIONS DATA
-------
-------
APPENDIX D-l
AS-MEASURED CONCENTRATIONS
D-l
-------
-------
TABLE D-l. DIOXIN/FURAN EMISSIONS DATA FOR RUN 1, SITE BLB-B INLET
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 ( 3.95E-02)
ND ( 3.9SE-02)
NO ( 3.95E-02)
ND ( 3.95E-02)
1.75E-01( N/A )
7.02E-01( N/A )
8.77E-01
9.93E-03(
3.67E-02(
ND ( 2.95E-03)
ND ( 2.95E-03)
ND ( 2.67E-03)
ND ( 2.43E-03)
N/A )
N/A )
4.66E-02
ND ( 8.69E+00)
ND ( 8.69E+00)
ND ( 8.69E+00)
ND ( 8.69E+00)
3.86E+01
1.54E+02
1.93E+02
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
4.39E-02(
4.39E-02(
ND (
8.77E-02(
4.39E-02(
4.39E-02(
2.63E-01
N/A )
N/A )
1.05E-01)
N/A
N/A
N/A
3.45E-03( N/A ) 9.65E+00
3.45E-03( N/A ) 9.65E+00
ND ( 7.45E-03) ND ( 2.32E+01)
5.63E-03( N/A ) 1.93E+01
2.58E-03( N/A ) 9.65E+00
2.38E-03( N/A ) 9.65E+00
1.75E-02 5.79E+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 when values are positive.
ng = 1.0E-09g
ug = 1.0E-06g
ppt = parts per trillion, dry volume basis
8760 operating hours per year
D-3
-------
TABLE D-2. DIOXIN/FURAN EMISSIONS DATA FOR RUN 2, SITE BLB-B INLET
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 ( 6.25E-02)
ND ( 6.25E-02)
ND ( 6.94E-03)
ND ( 8.68E-02) ND (
7.29E-01( N/A ) 4.13E-02(
2.33E+00( N/A ) 1.22E-01(
3.06E+00 1.63E-01
ND ( 4.67E-03)
ND ( 4.67E-03)
ND ( 4.69E-04)
5.34E-03)
N/A )
N/A )
ND ( 1.40E+01)
ND ( 1.40E+01)
ND ( 1.56E+00)
ND ( 1.95E+01)
1.64E+02
5.23E+02
6.87E+02
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
ND ( 6.25E-02)
ND ( 6.25E-02)
ND ( 3.47E-02)
1.04E-01(
3.47E-01(
2.43E-01(
6.94E-01
N/A
N/A
N/A
ND (
6.68E-03(
2.04E-02(
1.32E-02(
4.03E-02
ND ( 4.91E-03)
ND ( 4.91E-03)
2.46E-03)
N/A
N/A
N/A
ND ( 1.40E+01)
ND ( 1.40E+01)
ND ( 7.80E+00)
2.34E+01
7.80E+01
5.46E+01
1.56E+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 when values are positive.
1.0E-09g
1.0E-06g
parts per trillion, dry volume basis
8760 operating hours per year
D-4
-------
TABLE D-3. DIOXIN/FURAN EMISSIONS DATA FOR RUN 3, SITE BLB-B INLET
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
2.08E-01
6.81E+00
3.42E+01
2.43E-02)
2.43E-02)
8.68E-02)
N/A )
: N/A )
( N/A )
4.13E+01
1.28E-02
3.85E-01
1.79E+00
ND ( 1.82E-03)
ND ( 1.82E-03)
ND ( 5.87E-03)
( N/A )
N/A )
N/A )
2.19E+00
ND ( 5.46E+00)
ND ( 5.46E+00)
ND ( 1.95E+01)
4.68E+01
1.53E+03
7.69E+03
9.27E+03
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
6.94E-02(
4.51E-01(
ND (
2.43E-01(
6.25E-01(
4.51E-01(
1.84E+00
N/A
N/A
8.68E-02)
5.46E-03( N/A ) 1.56E+01
3.55E-02( N/A ) 1.01E+02
ND ( 6.14E-03) ND ( 1.95E+01)
N/A ) 1.56E-02( N/A ) 5.46E+01
N/A ) 3.68E-Q2( N/A ) 1.40E+02
N/A ) 2.45E-02( N/A ) 1.01E+02
1.18E-01 4.13E+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 when values are positive.
ng = 1.0E-09g
ug = 1.0E-06g
ppt = parts per trillion, dry volume basis
8760 operating hours per year
D-5
-------
-------
APPENDIX D-2
CONCENTRATIONS CORRECTED TO 3 PERCENT OXYGEN
0-7
-------
-------
TABLE D-4. DIOXIN/FURAN EMISSIONS DATA FOR RUN 1, SITE BLB-B INLET
(Concentrations Corrected to 3% Oxygen) .
Dioxin/Furan
Isomer
Isomer Concentration
In Flue Gas
(ng/dscni @ 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
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
ND ( 4.15E-02)
ND ( 4.15E-02)
ND ( 4.15E-02)
ND ( 4.15E-02)
1.84E-01( N/A )
7.37E-01( N/A )
9.22E-01
4.61E-02( N/A )
4.61E-02( N/A )
ND ( 1.11E-01)
9.22E-02( N/A )
4.61E-02( N/A )
4.61E-02( N/A )
2.77E-01
ND ( 3.10E-03)
ND ( 3.10E-03)
ND ( 2.80E-03)
ND ( 2.55E-03)
1.04E-02( N/A )
3.86E-02( N/A ) .
4.90E-02
3.62E-03( N/A )
3.62E-03( N/A )
ND ( 7.83E-03)
5.91E-03( N/A )
2.71E-03( N/A )
2.50E-03( N/A )
1.84E-02
ND ( 8.69E+00)
ND ( 8.69E+00)
ND ( 8.69E+00)
ND ( 8.69E+00)
3.86E+01
1.54E+02
1.93E+02
9.65E+00
9.65E+00
ND ( 2.32E+01)
1.93E+01
9.65E+00
9.65E+00
5.79E+01
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 when values are positive.
ng = 1.0E-09g
ug = 1.0E-06g
ppt = parts per trillion, dry volume basis
8760 operating hours per year
D-9
-------
TABLE D-5. DIOXIN/FURAN EMISSIONS DATA FOR RUN 2, SITE BLB-B INLET
(Concentrations Corrected to 3% Oxygen)
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 ( 6.90E-02)
ND ( 6.90E-02)
ND ( 7.67E-03)
ND ( 9.59E-02)
8.05E-01( N/A ) 4.56E-02(
2.57E+00( N/A ) 1.34E-01(
3.37E+00 1.80E-01
ND ( 5.16E-03)
ND ( 5.16E-03)
ND ( 5.18E-04)
ND ( 5.90E-03)
N/A )
N/A )
ND ( 1.40E+01)
ND ( 1.40E+01)
ND ( 1.56E+00)
ND ( 1.95E+01)
1.64E+02
5.23E+02
6.87E+02
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
ND ( 6.90E-02)
ND ( 6.90E-02)
ND ( 3.83E-02)
3.83E-01(
2.68E-01(
7.67E-01
N/A
N/A
N/A
ND ( 5.43E-03)
ND ( 5.43E-03)
ND ( 2.71E-03)
7.38E-03(
2.26E-02(
1.45E-02(
4.45E-02
N/A
N/A
N/A
ND ( 1.40E+01)
ND ( 1.40E+01)
ND ( 7.80E+00)
2.34E+01
7.80E+01
5.46E+01
1.56E+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 when values are positive.
ng - l«OE-09g
ug - 1.0E-06g
ppt » parts p'er trillion, dry volume basis
8760 operating hours per year
D-10
-------
TABLE D-6. DIOXIN/FURAN EMISSIONS DATA fOR RUN 3, SITE BLB-B INLET
(Concentrations Corrected to 3% Oxygen)
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 ( 2.77E-02
ND ( 2.77E-02
ND ( 9.89E-02
N/A
N/A
N/A
,37E-01(
,75E+00(
.90E+01(
4.70E+01
1.46E-02(
4.39E-01(
2.04E+00(
2.49E+00
ND ( 2.07E-03
ND ( 2.07E-03
ND ( 6.68E-03)
N/A )
N/A )
N/A )
ND ( 5.46E+00)
ND ( 5.46E+00)
ND ( 1.95E+01)
4.68E+01
1.53E+03
7.69E+03
9.27E+03
2378 TCDF
Other TCDF
Penta-CDF
Hexa-CDF
Hepta-CDF
Octa-CDF
Total PCDF
7.91E-02
5.14E-01
ND
2.77E-01
7.12E-01
5.14E-01I
N/A )
N/A )
9.89E-02)
N/A )
N/A )
[ N/A )
2.10E+00
6.22E-03(
4.04E-02(
ND (
1.78E-02(
4.19E-02(
2.79E-02(
1.34E-01
N/A )
N/A )
7.00E-03)
N/A )
N/A )
N/A )
1.56E+01
1.01E+02
ND ( 1.95E+01)
5.46E+01
1.40E+02
1.01E+02
4.13E+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 when values are positive.
ng = 1.0E-09g
ug = 1.0E-06g
ppt = parts per trillion, dry volume basis
8760 operating hours per year
D-ll
-------
-------
APPENDIX E
RUN-SPECIFIC RISK MODELING INPUT DATA
-------
-------
APPENDIX E-l
ESP INLET
E-l
-------
-------
TABLE E-l. RISK MODELING PARAMETERS FOR RUN 1, SITE BLB-B INLET
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
Concentratio
In Flue Gas
(ng/dscm)
ND ( 3.95E-02
ND ( 3.95E-02
4.39E-02
4.39E-02
ND ( 3.95E-02
ND ( 1.05E-01
ND ( 3.95E-02
8.77E-02
1.75E-01
4.39E-02
7.02E-01
4.39E-02
Isomer Hourly
n Emissions
Rate
(ug/hr)
) ND ( 8.69E+00)
) ND ( 8.69E+00)
9.65E+00
9.65E+00
ND ( 8.69E+00)
ND ( 2.32E+01)
ND ( 8.69E+00)
1.93E+01
3.86E+01
9.65E+00
1.54E+02
9.65E+00
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 ( 7.61E+01)
ND ( 7.61E-01)
8.46E+00
8.46E-02
ND ( 3.80E+01)
ND ( 2.03E+01)
ND ( 3.04E+00)
1.69E+00
3.38E-01
8.46E-02
.OOE+00
.OOE+00
Net 2378 TCDD Equivalent Atmospheric Loading
1.07E+01
ND =
N/A =
ng =
ug =
mg =
not detected (detection limit in parentheses)
detection limit not available
1.0E-09g
1.0E-06g
1.0E-03g
E-3
-------
TABLE E-2. RISK MODELING PARAMETERS FOR RUN 2, SITE BLB-B INLET
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 ( 6.25E-02)
ND ( 6.25E-02)
ND ( 6.25E-02)
ND ( 6.25E-02)
ND ( 6.94E-03)
ND ( 3.47E-02)
ND ( 8.68E-02)
1.04E-01
7.29E-01
3.47E-01
2.33E+00
2.43E-01
Isomer Hourly
Emissions
Rate
(ug/hr)
ND ( 1.40E+01)
ND ( 1.40E+01)
ND ( 1.40E+01)
ND ( 1.40E+01)
ND ( 1.56E+00)
ND ( 7.80E+00)
ND ( 1.95E+01)
2.34E+01
1.64E+02
7.80E+01
5.23E+02
5.46E+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 ( 1.23E+02)
ND ( 1.23E+00)
ND ( 1.23E+01)
ND ( 1.23E-01)
ND ( 6.83E+00)
ND ( 6.83E+00)
ND ( 6.83E+00)
2.05E+00
1.44E+00
6.83E-01
.OOE+00
.OOE+00
Net 2378 TCDD Equivalent Atmospheric Loading
4.17E+00
ND
N/A
ng
"9
mg
not detected (detection limit in parentheses).
detection limit not available
1.0E-09g
1.0E-06g
1.0E-03g
Standard conditions: 293 K (20 C) temperature and 1 atmosphere pressure.
8760 operating hours per year
E-4
-------
TABLE E-3. RISK MODELING PARAMETERS FOR RUN 3, SITE BLB-B INLET
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 ( 2.43E-02)
ND ( 2.43E-02)
6.94E-02
4.51E-01
ND ( 8.68E-02)
ND ( 8.68E-02)
2.08E-01
2.43E-01
6.81E+00
.6.25E-01
3.42E+01
4.51E-01
Isomer Hourly
Emissions
Rate
(ug/hr)
ND ( 5.46E+00)
ND ( 5.46E+00)
1.56E+01
1.01E+02
ND ( 1.95E+01)
ND ( 1.95E+01)
4.68E+01
5.46E+01
1.53E+03
1.40E+02
7.69E+03
1.01E+02
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 ( 4.78E+01)
ND ( 4.78E-01)
1.37E+01
8.88E-01
ND ( 8.54E+01)
ND ( 1.71E+01)
1.64E+01
4.78E+00 .
1.34E+01
1.23E+00
.OOE+00
.OOE+00
Net 2378 TCDD Equivalent Atmospheric Loading
5.04E+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
E-5
-------
-------
APPENDIX E-2
ESP OUTLET
E-7
-------
-------
TABLE E-4. RISK MODELING PARAMETERS FOR RUN 1, SITE BLB-B OUTLET
Latitude - 31 10 23
Longitude = 81 31 13
Stack Height (From Grade Level) = 84.7
Stack Diameter (ID) = 3.66
Flue Gas Flow Rate (Dry Standard) = 3750.4
Flue Gas Exit Temperature = 431.6
Flue Gas Exit Velocity (Actual) = 766.17
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 ( 3.01E-02)
ND ( 3.01E-02)
ND ( 3.76E-02)
2.63E-01
ND ( 4.51E-02)
ND ( 2.74E-01)
1.88E-01
7.14E-01
3.38E-01
2.63E-01
1.05E+00
7.52E-02
Isomer Hourly
Emissions
Rate
(ug/hr)
ND ( 6.77E+00)
ND ( 6.77E+00)
ND ( 8.46E+00)
5.92E+01
ND ( 1.02E+01)
ND ( 6.18E+01)
4.23E+01
1.61E+02
7.61E+01
5.92E+01
2.37E+02
1.69E+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 ( 5.93E+01)
ND ( 5.93E-01)
ND ( 7.41E+00)
5.19E-01
ND ( 4.45E+01)
ND ( 5.41E+01)
1.48E+01
1.41E+01
6.67E-01
5.19E-01
.OOE+00
.OOE+00
Net 2378 TCDD Equivalent Atmospheric Loading
3.06E+01
ND =
N/A =
ng =
ug =
mg =
not detected (detection limit in parentheses).
detection limit not available
1.0E-09g
1.0E-06g
1.0E-03g
C)
'^sphere pressure.
E-9
-------
TABLE E-5. RISK MODELING PARAMETERS FOR RUN 2, SITE BLB-B OUTLET
Latitude - 31 10 23
Longitude = 81 31 13
Stack Height (From Grade Level) = 84.7
Stack Diameter (ID) - 3.66
Flue Gas Flow Rate (Dry Standard) - 3694.5
Flue Gas Exit Temperature = 426.7
Flue Gas Exit Velocity (Actual) = 755.1
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 ( 1.18E-02)
ND 1.18E-02)
ND 4.00E-02)
ND 4.00E-02)
ND 3.29E-02)
ND ( 3.29E-02)
ND ( 8.47E-02)
ND ( 1.36E-01)
1.65E-01
7.06E-02
5.41E-01
4.71E-02
Isomer Hourly
Emissions
Rate
(ug/hr)
ND ( 2.61E+00
ND ( 2.61E+00
ND ( 8.87E+00
ND ( 8.87E+00
ND ( 7.30E+00
?ND ( 7.30E+00
ND ( 1.88E+01]
ND ( 3.03E+01]
3.65E+01
1.56E+01
1.20E+02
1.04E+01
Relative
Potency
Factor
1.000
.010
.100
.001
.500
.100
) .040
1 .010
.001
.001
.000
.000
2,3,7,8 - TCDD
Equivalent
Emissions
(mg/yr)
ND ( 2.28E+01)
ND ( 2.28E-01)
ND ( 7.77E+00)
ND 7.77E-02)
ND ( 3.20E+01)
ND ( 6.40E+00)
ND ( 6.58E+00)
ND ( 2.65E+00)
3.20E-01
1.37E-01
.OOE+00
.OOE+00 •
Net 2378 TCDD Equivalent Atmospheric Loading
4.57E-01
ND
N/A
ng
ug
mg
not detected (detection limit in parentheses).
detection limit not available
1.0E-09g
1.0E-06g
1.0E-03g
Standard conditions: 293 K (20 C) temperature and 1 atmosphere pressure.
8760 operating hours per year
E-10
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TABLE E-6. RISK MODELING PARAMETERS FOR RUN 3, SITE BLB-B OUTLET
Latitude = 31 10 23
Longitude = 81 31 13
Stack Height (From Grade Level) =84.7
Stack Diameter (ID) » 3.66
Flue Gas Flow Rate (Dry Standard) = 3885.3
Flue Gas Exit Temperature = 432.4
Flue Gas Exit Velocity (Actual) - 783.6
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 ( 2.49E-02)
ND ( 2.49E-02)
2.26E-02
6.79E-02
ND ( 1.36E-01)
ND ( 1.36E-01)
6.79E-02
1.36E-01
1.58E-01
9.05E-02
5.43E-01
4.52E-02
Isomer Hourly
Emissions
Rate
(ug/hr)
ND ( 5.80E+00)
ND ( 5.80E+00)
5.27E+00
1.58E+01
ND ( 3.16E+01)
ND ( 3.16E+01)
1.58E+01
3.16E+01
3.69E+01
2.11E+01
1.27E+02
1.05E+01
Relative
Potency
Factor
1.000
.010
.100
.001
.500
.100
.040
.010
.001
.001
.000
.000
2,3,7,8 - TCDD
Equivalent
Emi ssions
(mg/yr)
ND ( 5.08E+01)
ND ( 5.08E-01)
4 62E+00
1.39E-01
ND ( 1.39E+02)
ND ( 2.77E+01)
5.54E+00
2.77E+00
3.23E-01
1.85E-01
.OOE+00
.OOE+00
Net 2378 TCDD Equivalent Atmospheric Loading 1.36E+01
ND =
N/A =
ng =
ug =
mg
not detected (detection limit in parentheses).
detection limit not available
1.0E-09g
1.0E-06g
1.0E-03g
«7fin nnd C°l?diti°ns: 293 K (20 C) temperature and 1 atmosphere pressure.
8760 operating hours per year
E-ll
-------
-------
APPENDIX F
COMPOUND-SPECIFIC PRECURSOR RESULTS
-------
-------
TABLE F-l. COMPOUND-SPECIFIC DIOXIN PRECURSOR
DATA FOR SITE 05 FEED SAMPLES
•Precursor Precursor
Compounds
Run
0
HI
1
Concentration, ua/a fnnm^
ack
M<
Run
liior
0?
Feed
Run
03
Base Neutrals Fraction
Chlorinated Benzenes;
Pichlorobenzenes
>ichlorobenzenes
NO
ND
NO
fetrachlorobenzenes
ND
ND
Pentachlorobenzenes
ND
ND
ND
Hexachlorobenzenes
Total Chlorinated Benzenes
ND
ND
ND
ND
ND
Chlorinated Biphenvls:
Chlorobiohenvls
Dichlorobiohenvls
ND
ND
Trichlorobiphenvls
Tetrachlorobi ohenvl s
ND
ND
ND
Jffi.
ND
ND
Pentachlorobi ohenvls
ND
ND
ND
Hexachlorobiohenvl s
Heotachlorobi ohenvls
ND
ND
ND
Octachlorobi ohenvls
ND
ND
Nonachlorobiohenvls
Decachlorobi ohenvls
ND
ND
ND
ND
JD_
ND
ND
Total Chlorinated Biohenvls
ND
ND
ND
ND
Acids Fraction
Chlorinated Phenols;
Dichloroohenols
ND
ND
ND
THchlorophenols
Tetrachlorophenols
ND
JD_
ND
ND
ND
Pentachloroohenols
Total Chlorinated Phenols
ND
trace
ND
trace
0
ND = not detected
See Section 8.3 for a discussion of quality assurance/quality control
results for these analyses.
F-l
-------
-------
APPENDIX G
RESEARCH TRIANGLE INSTITUTE (RTI) AUDIT REPORT
G-l
-------
-------
QUALITY ASSURANCE AUDIT FOR TIER 4 OF THE NATIONAL OIOXIN STUDY:
BLACK LIQUOR RECOVERY BOILER, SITE BLB-B
by
Donna J. Holder
Richard V. Crume
EPA Contract No. 68-02-3149
Work Assignment 10-1
RTI Project No. 472U-2500-48
EPA Technical Project Monitor
D. Oberacker
Prepared for
William B. Kuykendal, Air Management Technology Branch
Monitoring and Data Analysis Division
Office of Air Quality Planning and Standards
Environmental Protection Agency
Research Triangle Park, NC 27711
April 1985
G-3
-------
-------
TABLE OF CONTENTS
Chapter
1.0 Summary „ 1
2.0 Introduction 4
2.1 Process Description 4
2.2 Test Program Design 4
2.3 Audit Objectives ... 5
3.0 Audit Observations 11
3.1 Introduction 11
3.2 Process Operation 11
3.3 Modified Method 5 Sampling Train 11
3.4 Blank MM5 and HC1 Sampling Trains 12
3.5 Ambient MM5 Sampling Train 12
3.6 HC1 Sampling Train 12
3.7 Continuous Emission Monitors 12
3.8 Process Samples 13
3.9 Sample Handling, Transportation, and
Storage 13
3.10 Soil Sampling. , . 13
4.0 Conclusions 15
5.0 References 16
6.0 Appendix 18
6.1 Checklist for RTI Recommendations
From ISW-A Audit 19
6.2 Checklist for RTI Comments on Site BLB-B. . . 20
G-5
-------
TABLES
Number
1
2
3
List of Persons Present During RTI Audit.
Critical Quality Assurance Elements . . .
Reference Materials Used to Evaluate the Radian
Test Program
2
6
10
6-6
-------
1.0 SUMMARY
On February 27, 1985, Research Triangle Institute (RTI) performed a
quality assurance (QA) audit of an emission test program underway at a black
liquor recovery boiler (Site BLB-B). The emission test program was one of a
series of-tests performed by Radian Corporation for the U.S. Environmental
Protection Agency (EPA). The data collected during these tests will be added
to the data base supporting Tier 4 of EPA's National Dioxin Study. The primary
objective of Tier 4 is to determine if various combustion sources are sources
of dioxin emissions. If any of the combustion sources are found to emit
dioxin, the secondary objectives of Tier 4 are to quantify these dioxin emis-
sions and, if possible, to relate these emissions to combustion device operat-
ing conditions. The audit was performed by Richard V. Crume and Donna J. Holder,
both environmental engineers with RTI. The EPA project officer is William B.
Kuykendal of the Office of Air Quality Planning and Standards, Research Triangle
Park, North Carolina. A list of persons during the audit is presented in
Table 1.
The goals of the audit were to: (1) evaluate Radian Corporation's adher-
ence to the test program's Test Plan and QA Plan and (2) determine whether
the recommendations made by RTI as a result of an earlier audit had been fully
implemented. (The earlier audit took place on November 8, 1984, and involved
an evaluation of Radian Corporation's testing at industrial incinerator site
ISW-A.)1 As with the earlier audit, the RTI auditors were impressed with the
Radian test team and the quality of their work. It appeared that the test
team faithfully adhered to their Test Plan and QA Plan and that the required
sampling procedures were carefully followed. Furthermore, with two minor
exceptions (the position of the condenser on the Modified Method 5 sampling
train and the marking of liquid levels on bottles), all of RTI's earlier
recommendations had been implemented. RTI is satisfied that the Radian test
team continues to generate quality data.
This audit report does not include an evaluation of Radian's analytical
facilities, which is expected to take place within the next 3 months. Con-
G-7
-------
Name
TABLE 1. LIST OF PERSONS PRESENT DURING THE RTI AUDIT
Affiliation
Mike Palazzolo
Dave Dayton
Lee Garcia
Gary Henry
Carol Jamgochian
Bob Jongleux
Winton Kelly
Jim McReynolds
Dave Savia
Bob Mournigham
Richard Grume
Donna Holder
Radian (Test team leader)
Radian Corporation
Radian Corporation
Radian Corporation
Radian Corporation
Radian Corporation
Radian Corporation
Radian Corporation
Radian Corporation
EPA (Cincinnati)
Research Triangle Institute
Research Triangle Insitute
G-8
-------
elusions regarding the entire Radian test program cannot be made until the
analytical laboratory audit has been completed.
G-9
-------
2.0 INTRODUCTION
2.1 PROCESS DESCRIPTION
The process unit under study during the Site BLB-B test program was a
Combustion Engineering recovery boiler with a rated capacity of 900 tons per
day (TPD) of unbleached pulp. The boiler typically operates at full load, 24
hours per day. The black liquor fed to the boiler has a solids content of
approximately 67 percent, by weight, and a heating value of approximately
6,000 Btu/lb. Various materials make up the strong black liquor, including:
Wood chips,
, • Makeup salt cake,
Slaked lime [Ca(OH)2],
C102 spent acid,
C102 byproduct salt cake, and
Well water (process makeup).
The concentrated black liquor is at an approximate temperature of 250 °F as it
enters the combustion zone of the boiler.
Forced draft fans supply primary and secondary combustion air to the
boiler. The oxygen concentration in the outlet flue gas is manually main-
tained at between 3.0 and 4.0 percent. Prior to being vented to the stack,
the exhaust gases from the black liquor boiler pass through a two-chamber
Flakt electrostatic precipitator (ESP) for particulate removal by drag- and
screw-type conveyors. The ESP outlet has a design particulate removal effi-
ciency of 99.6 percent. More details concerning the black liquor recovery
boiler can be found in Radian Corporation's Test Plan.2
2.2 TEST PROGRAM DESIGN
The test program can be divided into the following categories:
6-10
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Process monitoring, .
Modified Method 5 (MM5) sampling train,
Blank MM5 sampling train,
HC1 sampling train,
Continuous emission monitors,
Process samples,
Sample handling, transportation, and storage, and
Soil sampling.
Details concerning these operations can be found in Radian Corporation's Test
Plan,2 Quality Assurance Project Plan,3 and Sampling Procedures Document.4
The most important aspect of the test program concerns the sampling of
organic compounds (including any 2,3,7,8-TCOD present in the gas stream) using
an MM5 sampling train. The MM5 train is similar to the EPA Method 5 train,
except that a sorbent trap for the collection of vapor phase organics is
included. The trap consists of separate sections for cooling the gas stream
and for absorbing the organic compounds onto Amber!ite XAD-2 resin. The setup
and operation of the MM5 train are described in detail in the "ASME MM5 Sampling
Methodology for Chlorinated Organics," contained in Radian Corporation's Test
Plan.2 Three test runs, each of approximately 4 hours' duration, were to be
conducted at the test site.
2.3 AUDIT OBJECTIVES
The goals of the audit were to evaluate Radian Corporation's adherence to
the test program's Test Plan and QA Plan and to determine whether the recom-
mendations made by RTI as a result of an earlier audit had been fully imple-
mented. These goals were achieved by performing two types of audit activities:
systems audits and performance audits.
A systems audit consists of an onsite inspection and review of the test
procedures (including any QA activities) associated with test program measure-
ments. RTI's systems audit of the Radian test began with an evaluation of
Radian's QA project plan. This plan was evaluated according to the criteria
presented in EPA's QAMS-005/80 guideline document and summarized in Table 2.s
6-11
-------
TABLE 2. CRITICAL QUALITY ASSURANCE ELEMENTS
Project Description
Project description
Experimental design
Intended use of acquired data
Start and completion dates
Appropriate diagrams, tables, and figures
Project Organization and Responsibility
Organization of project
Line of authority
Key individuals (including quality assurance official)
Quality Assurance Objectives for Measurement Data
Precision
Accuracy
Completeness
Representati veness
Comparability
Sampling Procedures
Sampling site selection
Sampling procedures
Description of containers for sample collection, preservation,
transport, and storage
Procedures to avoid sample contamination
Sample preservation methods and holding times
Procedures for recording sample history, sampling conditions, and
analyses to be performed
Sample Custody Records
Preparation of reagents or supplies associated with sample
Location and conditions where sample was taken
Sample preservation methods
Labeling
Field tracking forms
Field and laboratory sample custodians
Laboratory custody log
Laboratory handling, storage, and dispersement procedures
(continued)
6-12
-------
TABLE 2. (continued)
Cali bration Procedures
Description of, or reference to, calibration procedure
Frequency of calibration
Calibration standards, including sources and traceability
procedures
Analytical Procedures
Analytical procedure
Appropriateness of method
Data Reduction, Validation and Reporting
Data reduction scheme
Equations to be used
Validation procedures
Identification and treatment of outliers
Internal Quality Control Checks
Replicates
Spiked samples
Split samples
Control charts
Blanks
Zero and span gases
Quality control samples
Surrogate samples
Reagent checks
Calibration standards and devices
Performance and Systems Audits
Schedule for conducting audits
Systems to be audited
Sources of audit materials
Procedures to Assess Data Precision, Accuracy and Completeness
Central tendency and dispersion •
Measures of variability
Significance test
Confidence limits
Testing for outliers
Preventive Maintenance
Schedule of maintenance tasks
List of critical spare parts on hand
(continued)
G-13
-------
TABLE 2. (continued)
Corrective Action
Predetermined limits for data acceptability
Procedures for corrective action
Responsible individuals
Quality Assurance Reports to Management
Frequency of reporting
Responsible individuals
Significant problems and recommended solutions
6-14
-------
Radian's test plan was similarly evaluated, although adherence to the QAMS-0€5/80
criteria was not required. RTI's comments on the Radian QA and Test Plans
were previously submitted.6 7 8 The systems audit continued with an onsite
inspection of the Radian test program and the preparation of this report. The
systems audit also included the determination of whether RTI's earlier recom-
mendations were implemented and whether RTI's comments on the Test Plan were
addressed. (An onsite systems audit of Radian's analytical laboratory will be
performed in 1985. The results of the laboratory audit will be presented in a
separate report.)
The objectives of a performance audit are similar to those of a systems
audit (i.e., to evaluate the quality of data likely to be generated by the
test or experimental program). The performance audit differs from the systems
audit in that it involves the actual measurement of critical test program
parameters using standardized reference materials. RTI's performance audit of
the Radian test program utilized the materials listed in Table 3. Radian
Corporation and EPA's Troika Laboratories will analyze these materials and
return the results to RTI for evaluation. Once these results are received and
evaluated, RTI will discuss the results in a separate report.
G-15
-------
TABLE 3. REFERENCE MATERIALS USED TO EVALUATE
THE RADIAN TEST PROGRAM
Material
Description
1. Fuel oil sample la
2. Fuel oil sample 2
3. Fuel oil sample 3
4. Fuel oil sample 4
5. HC1 impinger solution
6. HC1 impinger solution
7. Dioxi'n sample
8. Calibrated orifice
Fuel oil spiked with a known
chloride concentration
Similar to material No. 1
Similar to material No. 1
Similar to material No. 1
HC1 train impinger solution
having verified chloride
concentration
Similar to material No. 5
2,3,7,8-TCDD in isooctane
Used to evaluate the sampling
trains' dry gas meter
calibrations
Fuel oil samples were not collected during the test program.
(Auxiliary fuel oil was not burned at the plant.) However, during
earlier tests where fuel oil samples were collected, audit data
indicated that the fuel oil/chlorine analytical method used by a
Radian subcontractor may have been inappropriate at chlorine concen-
trations below 1,000 ppm.9 At Radian's request, the fuel oil samples
listed in the above table were provided to examine the performance of
the method selected to replace the original method.
G-16
-------
3.0 AUDIT OBSERVATIONS
3.1 INTRODUCTION
RTI's observations for the Site BL8-B audit are discussed below. Since
the sampling procedures used by Radian at this site were nearly identical to
the procedures used during the previous audit, it is not necessary to repeat
in this report the sampling checklists presented in the previous audit report.
However, two new check lists are presented here which compare: (1) RTI's
recommendations from the earlier audit with the procedures actually followed
at Site BLB-B; and (2) RTI's comments on the Site BLB-B Test Plan with the
procedures actually followed. These two checklists are presented in the
Appendix.
3.2 PROCESS OPERATION
. In contrast to the difficulties encountered with the Site ISW-A incin-
erator (i.e., variable loads and process disruptions), the Site BLB-B boiler
operated smoothly during the audit. The plant's Director of Environmental
Engineering reported that the boiler*was at 100 percent capacity and that the
feed composition was indicative of normal operation. The boiler's new electro-
static precipitator (ESP) was observed to discharge from the stack large dust
flakes. However, this did.not appear to interfere with post-ESP sampling.
The selection of an ESP-inlet sampling location was complicated by a
split in the ductwork leading to two ESP chambers. Although Radian sampled
only one of the two ductwork splits, it appeared that the gas composition in
both splits would be identical.
3.3 MODIFIED METHOD 5 SAMPLING TRAIN
The MM5 sampling train appeared to be set up and operated according to
the ASME MM5 sampling methodology specified in Radian's Test Plan, with two
exceptions. First, the solvent used for recovery was changed from hexane to
methylene chloride. This change in solvent was recommended by EPA as a result
of the high blank values which occurred during earlier tests when hexane was
G-17
-------
used as the solvent.10 The second exception to the ASME MM5 methodology
involved the mounting of the XAO trap condenser in a horizontal position, as
opposed to the vertical orientation specified in the ASME method. The horizontal
mounting of the condenser was approved by EPA as a modification to the ASME
MM5 methodology presented in Radian's Test Plan. (This approval was based on
evidence that, for this test program, all condensed liquids are carried forward
into the XAD resin regardless of whether the condenser is horizontally or
vertically mounted.)
One sampling probe was broken during testing as a result of a torn cable
during the vertical traversing at the inlet sampling location. Otherwise, all
MM5 procedures specified in the test plan appeared to be implemented correctly.
3.4 BLANK MM5 AND HC1 SAMPLING TRAINS
The blank MM5 sampling train was to be located on the roof of the building
where the standard MM5 train was set up. (The blank train was not in use
during the day of the audit.) It consisted of the essential elements of a
standard MM5 train, except for the probe and meter box. The probe condenser
inlet and the final impinger outlet were to be capped with hexane-rinsed
aluminum foil, as required. The blank MM5 train was to remain assembled for
the duration of one complete test run.
The blank HC1 sampling train was also to be located on the roof of the
building on which the standard MM5 train was set up. As with the blank MM5
train, the probe inlet and the final impinger outlet of the blank HC1 train
were capped with hexane-rinsed aluminum foil. The blank HC1 train was to
remain assembled for the duration of one complete test run.
3,5 AMBIENT MM5 SAMPLING TRAIN
An ambient MM5 sampling train was not used in this test program.
3.6 HC1 SAMPLING TRAIN
No problems were reported or observed in the operation of the HC1 train.
(During the earlier audit, a broken probe occurred.)
3.7 CONTINUOUS EMISSION MONITORS
The continuous emission monitoring system consisted of a coarse filter,
sampling probe, heated sampling line, moisture removal system, monitoring
6-18
-------
units, strip charts, and an excellent automated data acquisition system.
Strip charts were carefully marked and all calibration data were recorded.
Three-point calibrations were performed at the beginning of the test program,
and two-point calibrations were performed at the beginning and end of each
test run. Calibration and quality control gases were introduced at the begin-
ning of the sample line near the stack for all gases except THC, which was
introduced at the end of the sample line near the THC monitor. (Since THC is
monitored on a wet basis, it is not necessary to pass either the stack gases
or the calibration/QC gases through the gas conditioning system and sampling
manifold.)
Strip charts were offset 10 percent to compensate for possible negative
drifts. Monitor drift, in general, was negligible. Temperature variations
within the continuous monitor trailer were minimized as a result of the air
conditioning system.
3.8 PROCESS SAMPLES
The process sample collection activities, involved the collection of
representative samples of strong black liquor, white liquor, weak liquor,
spent adds, byproduct salt cake, and well water. The test team collected two
grab samples per test run of all samples, except for the strong black liquor
which was collected hourly during each run. Process operating parameters were
recorded hourly by hand. Additionally, the plant's printout of the operating
parameters was retained in case any backup information was required.
3.9 SAMPLE HANDLING, TRANSPORTATION, AND STORAGE
Radian carefully packed samples to avoid possible breakage. The clean-
liness of the analytical trailer and orderliness of equipment and supplies had
been significantly improved since the first audit. Radian continued to mark'
sample weights rather than liquid levels on their sample bottles.
3.10 SOIL SAMPLING
The soil sampling activities were planned to be conducted as specified in
the Test Plan. (The soil sampling was not performed on the day of the audit.)
Site selection, proximity of samples, and sample compositing were recognized
by Radian as being important aspects of the soil sampling program and were
being studied at the time of the audit. The test team leader was considering
G-19
-------
sampling around the following locations: (1) area surrounding the C102 systems;
,(2) area surrounding the evaporators; and (3) the perimeter of the plant.
These samples would cover a wide area of grounds within, and surrounding, the
plant, where potential dioxin contamination is most likely.
G-20
-------
4.0 CONCLUSIONS
Overall, RTI was impressed with the Radian test team and the quality of
their work. It appeared that the test team faithfully adhered to their Test
Plan and QA Plan and that the required sampling procedures were carefully
followed. Furthermore, most of RTI's earlier recommendation had been imple-
mented. RTI is satisfied that the data generated by the test program will be
of sufficient quality to achieve the objectives of the study, provided that:
(1) the analytical procedures are performed correctly and (2) the sampling
procedures continue to be performed with the same level of care exhibited
during the Sites ISW-A and BLB-B tests.
G-21
-------
5.0 REFERENCES
1. Richard V. Grume, Research Triangle Institute. "Quality Assurance Audit
for TIER 4 of the National Dioxin Study: Industrial Incinerator Site
ISW-A." Research Triangle Park, North Carolina. February 1985.
2. M. A.-Palazzolo, Radian Corporation. "Site Specific Test Plan, Black
Liquor Recovery Boiler, Test Number Four, Site BLB-B, National Dioxin
Study, Tier 4: Combustion Sources." DCN No. 85-213-056-12-12. Research
Triangle Park, North Carolina. February 1, 1985.
3. M. A. Palazzolo, R. F. Jongleux, L. E. Keller, and J. Bursey, Radian
Corporation. "National Dioxin Study, Tier 4, Combustion Sources, Quality
Assurance Project Plan." DCN No. 231-056-12-17. Research Triangle Park,
North Carolina. March 5, 1985.
4. Radian Corporation. "Draft Report, National Oioxin Study, Tier 4, Combus-
tion Sources, Sampling Procedures." OCN No. 84-240-016-51-09. Research
Triangle Park, North Carolina. October 17, 1984.
5. U.S. Environmental Protection Agency. "Interim Guidelines and Specifica-
tions for Preparing Quality Assurance Project Plans." QAMS-005/80.
Washington, D.C. December 29, 1980.
6. Richard V. Grume, Research Triangle Institute. Review of Radian Corpora-
tion's Draft Report entitled "National Dioxin Study Tier 4: Combustion
Sources Quality Assurance Project Plan." Research Triangle Park, North
Carolina. October 23, 1984.
7. Richard V. Grume, Research Triangle Institute. Review of Radian Corpora-
tion's Revised Report entitled "National Dioxin Study Tier 4: Combustion
Sources Quality Assurance Project Plan." Research Triangle Park, North
Carolina. January 4, 1985.
8. Richard V. Crume, Research Triangle Institute. Letter to Mr. Bill Kuykendal,
Office of Air Quality Planning and Standards, U.S. Environmental Protection
Agency. Subject: Review of Radian Test Plan BLB-B. Research Triangle
Park, North Carolina. February 20, 1985.
9. Richard V. Crume, Research Triangle Institute. Letter to Mr. Willam 8.
Kuykendal. Subject: Report of Analytical Results for the Audit Material
of No. 2 Fuel Oil spiked with Chlorine. Research Triangle Park, North
Carolina. February 4, 1985.
G-22
-------
10. William 8. Kuykendal, U.S. Environmental Protection Agency. Letter to
Addressees. Subject: Change in Sample Recovery Reagents for Modified
Method 5 Sampling on Tier 4 Sites. Research Triangle Park, North Carolina.
February 27, 1985.
G-23
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6.0 APPENDIX
6.1 AUDIT CHECKLISTS
Additional information concerning the Site BLB-B audit is presented in
the following audit checklists.
6-24
-------
6.1. CHECKLIST FOR RTI RECOMMENDATIONS FROM ISW-A AUDIT
Recommendation
from ISW-A audit
Implemented
at BLB-B site
Comments
1. Vertical XAD-condenser
setup
2. Blank MM5 train sealed
throughout each test run
3. Calibration gases for the
continuous monitors intro-
duced through the entire
sampling interface
4. Temperature variations
minimized in the con-
tinuous monitor trailer
5. Stripcharts offset 10% to
avoid negative drifts
6. Soil sampling:
Representative sampling
Sampling area properly
cleaned prior to
sampling
7. General items:
Process shutdown
Stack exhaust fan
interference
Ambient air intake
damper
Operator cooperativeness
No
Yes
Yes
Yes
Yes
N/A
N/A
N/A
N/A
N/A
Yes
Radian believes that the
impinger box would be diffi-
cult to balance if a vertical
condenser is used.
Capped with hexane-rinsed
aluminum foil.
All calibration gases were
introduced through the entire
sample line, except for the
THC sample.
Air conditioning system was
working properly.
Soil sampling had not been
conducted at the time of the
audit. However, Radian reported
that RTI's recommendations would
be considered in designing
the sampling scheme.
The boiler operated con-
tinuously without signifi-
cant load variations.
All plant personnel were
extremely cooperative.
N/A = Not Applicable
G-25
-------
6.2. CHECKLIST FOR RTI COMMENTS ON SITE BLB-B
TEST PLAN
Comment on
test plan
Implemented
during test
Explanation
1.
2.
3.
4.
The collection of wood
chip samples may be
worthwhile, in case the
chlorine content of the
wood chips is ever ques-
tioned
Collection of ambient air
samples
Determination of black
liquor heating value
N/A
N/A
No
Strong Black Liquor
Sampling
5. Vertical XAD condenser
Yes
No
6. Quality Control:
HC1 duplicates
QC samples
Well water blanks
Flow rate audits
Computer system evalu-
ation
QC gases
7. Special safety precau-
tions for handling the
"hot" black liquor
N/A
•Yes
The sampling of wood chips
was not required by EPA during
the Site BLB-B tests.
The collection of ambient air
samples was not required by EPA
during the Site BLB-B tests.
This was not done. However,
according to the plant's
Environmental Manager, the feed
composition during testing was
representative of normal
operation.
The frequency of strong black
liquor sampling (hourly)
appeared to accommodate normal
process variations.
The condenser was mounted in a
horizontal position. Radian
believes that the impinger box
would be difficult to balance
if a vertical condenser is used.
Some duplicates and blanks were
to be used, including XAD blanks.
However, flow rates were not to
be checked. The computer system
was assumed by Radian to produce
valid data. QC gases were
used, separate from calibration
gases.
Respirators were available for
use during the collection of
process samples. Care was
taken to avoid contact with
hot liquids.
N/A * Not Applicable
6-26
-------
APPENDIX H
PROCESS MONITORING DATA
-------
-------
APPENDIX H-l
HOURLY AVERAGE VALUES
OF BOILER OPERATING PARAMETERS
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APPENDIX H-3
ELECTROSTATIC PRECIPITATOR ELECTRICAL DATA
H-37
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APPENDIX I
FIELD DATA SHEETS
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Of
EPA METHOD 1
TRAVERSE POINT LOCATION FOR CIRCULAR OUCTS
PLANT.
DATE _
l-S
INSOEOFFARfALLTO
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Figure B-3. Traverse point location for circular ducts.
1-1
-------
PRELIMINARY VELOCITY TRAVERSE
PLANT.
MTE_L
LOCATION
STACK ID 1 ''S'1
BAROMETRIC PRESSURE, w. H|
STACK GAUGE PRESSURE, m. H.Q —
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334,
333
Figure B-l. Preliminary velocity traverse.
1-2
-------
CORPORATION
EPA METHODS 1-4, §
NOMOGRAPH DATA
PLIMT SL5-g
SAMPLING LOCATION
CALIBRATED PRESSURE DIFFERENTIAL ACROSS
ORIFICE, in. HjO
AVERAGE METER TEMPERATURE (AMBIENT + 20*F). "F
PERCENT MOISTURE IN GAS STREAM BY VOLUME
BAROMETRIC PRESSURE AT METER, in. H|
STATIC PRESSURE IN STACK, in. Hf - V,5 " /f ^
(P.±0.073 i STACK GAUGE PRESSURE m in. H20)
RATIO OF STATIC PRESSURE TO METER PRESSURE
AVERAGE STACK TEMPERATURE. "F
AVERAGE VELOCITY HEAD. in. HjO
MAXIMUM VELOCITY HEAD. in. HjO
C FACTOR
CALCULATED NOZZLE DIAMETER, in.
ACTUAL NOZZLE DIAMETER, in.
REFERENCE Ap. in. H20
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SCHEMATIC OF TRAVERSE POINT LAYOUT
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EPAiDw. 233
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Figure B-l. Preliminary velocity traverse.
1-4
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PRELIMINARY VELOCITY TRAVERSE
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SCHEMATIC OF TRAVERSE POINT LAYOUT
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EPA METHOD 1
TRAVERSE POINT LOCATION FOR CIRCULAR DUCTS
PLANT.
DATE _
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PRELIMINARY VELOCITY TRAVERSE
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RADIAN
COHPOHATIOM
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NOMOGRAPH DATA
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STA-CJC OUTLET -
CALIBRATED PRESSURE DIFFERENTIAL ACROSS
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PERCENT MOISTURE IN GAS STREAM BY VOLUME
BAROMETRIC PRESSURE AT METER, in. H|
STATIC PRESSURE IN STACK, in. Hf
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AVERAGE VELOCITY HEAD, in. HjO
MAXIMUM VELOCITY HEAD, in. HjO
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o. oe x a.
i— g 03 a.
s
"^ U.
*
a.
LU
z
T -,,-
1-36
03
<
= 5 1- S
ec ui S<^ ec
ui» t—ui ui
^3 z5 z
z v» —35 —
S-**
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APPENDIX J
PROJECT PARTICIPANTS
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APPENDIX J
PROJECT PARTICIPANTS
Organization
Radian Corporation
Name
Mike Palazzolo
Bob Jongleux
Dave Dayton
Dave Savia
Jim McReynolds
Winton Kelly
Carol Jamgochian
Gary Henry
Lee Garcia
Robert Mournighan EPA-HWERL-Cincinnati
n
n
n
n
n
Responsibility
Field Engineer
Field Crew Lead
CEM Operator
Sample Recovery
ESP Inlet Location
ESP Inlet Location
ESP Inlet Location
ESP Outlet Location
ESP Outlet Location
Observer
Richard Crume
Donna Holder
Research Triangle Institute, Field Audit
Research Triangle Institute, Field Audit
J-l
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APPENDIX K
VOLUMETRIC FLOWRATE:
BLOCKED DUCT CORRECTIONS
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CALCULATION SHEET
CORPORATION
SIGNATURE.
PROJECT
DATE.
CHECKED.
JOB NO
CALC. NO.
, DATE
SUBJECT.
_ SHEET.
OF.
.SHEETS
..
ThjLckhbLetzL
O/. at @3
'
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APPENDIX L
ERROR ANALYSIS OF CONTROL DEVICE EFFICIENCY CALCULATIONS
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APPENDIX L
ERROR ANALYSIS: CONTROL DEVICE EFFICIENCY CALCULATIONS
Objective: Given the analytical uncertainty of the dloxin/furan analyses
(± 50% accuracy), estimate the uncertainty of the control device
efficiency calculations.
Let: C
the measured concentration of a given dioxin/furan
homologue at the outlet location.
the measured concentration of a given dioxin/furan
homologue at the inlet location.
the maximum possible concentration of the dioxin/
furan homologue given the measured value C .
out,meas'
the niin'iraum possible concentration of the dioxin/
furan homologue given the measured value C .
out, me as
the maximum possible concentration of the dioxin/
furan homologue, given the measured value C.
in,meas
'in min " the m1nim"n» possible concentration of the dioxin/
• •• 9 in i ii !?«•«*»«• Uj»_,.1 __..,_ _• ____ j.i __ i « _ '
out,meas
C.
in,meas
'out max
*
'out min
'in max
furan homologue, given the measured value C.
E - the removal efficiency of the control device
in,meas'
Assuming + 50 percent analytical accuracy:
Cmin " Cmeas ' °-5 Cmeas " °'5 Cmeas
Cmax - cmeas
'5 Cmeas m l-* Cmeas
Note that: E,
P
max
"max
in. max " out. min
C
in, max
'5 C
in,meas
/"*
out.min
in,max
" /3 (1 " Emeas)
C-i
-------
and:
•min
c - c
in.min out.max
in,min
1 - out.meas
1 - C
0.5 C
in,meas
'out, max
«
'in,min
- 3 U - Emeas>
min * meas
Now,
m1n
positive control (i.e., emissions
reduction across the control device)
- 2>
•meas
Therefore, if Emeas is larger than 66.7 percent, the true removal efficiency
can safely be assumed to be greater than zero.
And,
max
negative control (i.e., emissions
increase across the control device)
3 meas
< 0
meas
Therefore, if Emeas is less than -200 percent, the true efficiency can safely
be assumed to be less than zero.
To summarize:
Emeas > 66-7 Percent
positive control
-200 < E_Q,e < 66.7 percent
C-2
Emeas < 20°
no definitive conclusions
can be drawn
no negative control
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TABLE L.I VALUES OF Emax and Em1n FOR VARIOUS MEASURED CONTROL EFFICIENCIES
Control
meas
100
95
90
85
80
75
50
.25
0
-25
-50
-100
-200
Device Efficiency f?
max
100
98.3
96.7
95.0
93.4
91.7
83.4
75.0
66.7
58.4
50.0
33.4
0
&)
Emin
100
85
70
55
40
25
-50
-125
-200
-275
-350
-500
-800
Emax - <200 •+ Effleas)/3
Emin - 3Emeas ' 20°
t-3
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TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1. REPORT NO.
EPA-450/4-84-014n
2.
4. TITLE AND SUBTITLE
National Dioxin Study Tier 4 - Combustion Sources
Final Test Report - Site 5
Black Liquor Boiler BLB - B
7. AUTHOR(S)
Michael A. Palazzolo, Winton E. Kelly
Donna Holder
9. PERFORMING ORGANIZATION NAME AN
Radian Corporation
Post Office Box 13000
Research Triangle Park, NC 2
12. SPONSORING AGENCY NAME AND ADC
U.S. Environmental Protectic
Research Triangle Park, NC
Office of Research and Deve]
Washington, DC 20460
ID ADDRESS
.7709
RESS
m Agency, OAQPS
27711
.opment
3. RECIPIENT'S ACCESSION NO.
5. REPORT DATE
April 1987
6. PERFORMING ORGANIZATION CODE
8. PERFORMING ORGANIZATION REPORT NO.
87-222-109-02-21
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
68-03-3148
13. TYPE OF REPORT AND PERIOD COVERED
Final
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
EPA Project Officers: Donald Oberacker, ORD
William B. Kuykendal, OAQPS
16. ABSTRACT
This report summarizes the results of a dioxin/furan emissions test of a black liquor
recovery boiler equipped with a dry-bottom electrostatic precipitator for particulate
emissions control. Black liquor recovery boilers are used at Kraft pulp mills to pro-
duce process steam and to reclaim inorganic chemicals from spent wood pulping liquors.
This test is the fifth in a series of several dioxin/furan emissions tests being con-
ducted under Tier 4 of the National Dioxin Study. The primary objective of Tier 4 is
to determine if various combustion sources are found to emit dioxin or furan, the
secondary objective of Tier 4 is to quantify these emissions.
Black liquor recovery boilers are one of 8 combustion source categories that have been
tested in the Tier 4 program. After an initial information screening and one-day pre-
survey visit, this site (BLB-B) was selected partially because of the higher chloride
content of the black liquor (3.5 wt.% dry) compared to other black liquor recovery
boiler sites surveyed in the Tier 4 study (approx. 0.2 to 1.0 wt%, dry).
Data presented in the report include dioxin (tetra through octa homologue + 2378 TCDD)
and furan (tetra through octa homologue + 2378 TCDF) results for stack samples. In
addition, process data collected during sampling are also presented.
17.
a. DESCRIPTORS
KEY WORDS AND DOCUMENT ANALYSIS
b.lDENTIFIERS/OPEN ENDED TERMS
Air Emissions Air Pollution Emissions
Combustion Sources Data
Dioxin
Furans
2,3,7,8 Tetrachlorodibenzo-p-dioxin
Black Liquor Boiler
Pulp and Paper
18. DISTRIBUTION STATEMENT
Release Unlimited
19. SECURITY CLASS (This Report)
Unclassified
20. SECURITY CLASS (This page)
Unclassified
c. COSATI Field/Group
21. NO. OF PAGES
343
22. PRICE
EPA Form 2220-1 (R«v. .4-77) PREVIOUS EDITION is OBSOLETE
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