June 1995
PILOT-SCALE INCINERATION TESTING OF
FLUFF WASTE AND CONTAMINATED SOIL
FROM THE M. W. MANUFACTURING
SUPERFUND SITE
Volume I Technical Results
by
J. W. Lee, W. W. Vestal, S. Venkatesh, C. G. Goldman,
and L. R. Waterland
Acurex Environmental Corporation
Incineration Research Facility
Jefferson, Arkansas 72079
EPA Contract 68-C9-0038
Work Assignments 3-3 and 4-3
Project Officer: R. C. Thurnau
Technical Project Manager: M. K. Richards
Sustainable Technology Division
National Risk Management Research Laboratory
Cincinnati, Ohio 45268
NATIONAL RISK MANAGEMENT RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
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DISCLAIMER
The information in this document has been funded wholly by the U.S. Environmental Protection
Agency under Contract No. 68-C9-0038 to Acurex Environmental Corporation. It has been subjected to the
Agency's peer and administrative review, and it has been approved for publication as an EPA document. Mention
of trade names or commercial products does not constitute endorsement or recommendation for use.
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FOREWORD
The U.S. Environmental Protection Agency is charged by Congress with protecting the Nation's land,
air, and water resources. Under a mandate of national environmental laws, the Agency strives to formulate and
implement actions leading to a compatible balance between human activities and the ability of natural systems
to support and nurture life. To meet this mandate, EPA's research program is providing data and technical
support for solving environmental problems today and building a science knowledge base necessary to manage
our ecological resources wisely, understand how pollutants affect our health, and prevent or reduce environmental
risks in the future.
The National Risk Management Research Laboratory is the Agency's center for investigation of
technological arid management approaches for reducing risks from threats to human health and the environment.
The focus of the Laboratory's research program is on methods for the prevention and control of pollution to air,
land, water and subsurface resources; protection of water quality in public water systems ; remediation of
contaminated sites and ground water; and prevention and control of indoor air pollution. The goal of this research
effort is to catalyze development and implementation of innovative, cost-effective environmental technologies;
develop scientific and engineering information needed by EPA to support regulatory and policy decisions!; and
provide technical support and information transfer to ensure effective implementation of environmental
regulations and strategies.
This publication has been produced as part of the Laboratory's strategic long-term research plan. It is
published and made available by EPA's Office of Research and Development to assist the user community and
to link researchers with their clients.
E. Timothy Oppelt, Director
National Risk Management Research Laboratory
ill
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ABSTRACT
At the request of EPA Region III and U.S. Army Corps of Engineers, a series of six tests was
conducted at the U.S. EPA Incineration Research Facility (IRF) to evaluate the incinerability of the fluff waste
and contaminated soil from the M. W. Manufacturing Corporation Superfund site in Danville, Pennsylvania.
Both materials are contaminated with volatile organic compounds (VOCs), semivolatile organic compounds
(SVOCs), chlorinated dioxins and furans, and several trace metals, including antimony, arsenic, barium,
cadmium, chromium, copper, lead, nickel, silver, and zinc. Copper and lead, in particular, are at very high
concentrations in both the fluff and waste and contaminated soil. The fluff was incinerated at two kiln exit gas
temperatures: nominally 871 ° and 760°C (1,600° and 1,400°F). The soil was incinerated only at the higher kiln
exit gas temperature of 871 °C (1,600°F). Each test was run in duplicate (i.e., two tests were performed for each
incinerator feed/kiln temperature combination). The afterburner exit gas temperature for all tests was nominally
at 1,090°C (2,000°F). The primary air pollution control system consisted of a venturi/packed column scrubber
system followed by a flue gas reheater and baghouse.
Test results showed that greater than 99.99 percent DRE of the VOC and SVOC contaminants was
uniformly achieved. HC1 emissions were well below 1.8 kg/hr and system HC1 control efficiencies well above
99 percent. Particulate emissions at the baghouse exit were well below 34 mg/dscm (0.015 gr/dscf) corrected
to 7 percent Oj, a guideline level announced in the draft waste combustion strategy in May 1993. Baghouise exit
flue gas total chlorinated dioxin/furan levels were well below 30 ng/dscm corrected to 7 percent O2, another draft
combustion strategy guideline. Incineration effectively decontaminated both the fluff waste and soil of their VOC
and SVOC contaminants. However, the kiln ash discharge from the incineration of contaminated site soil at a
kiln gas temperature of 871°C (1,600°F) contained total chlorinated dioxin/furan concentrations of 2.4 to
3.6 ug/kg. Levels in the kiln ash from fluff incineration at the same temperature were 65 to 89 ug/kg, and
significantly increased, at 830 to 2,700 ug/kg, for incineration at a kiln gas temperature of 760°C (1,400°F).
In addition, the flue gas particulate collected as baghouse ash for all tests was a cadmium- and lead-contaminated
toxicity characteristic (TC) hazardous waste.
This report was submitted in fulfillment of Contract No. 68-C9-0038 by Acurex Environmental
Corporation under the sponsorship of the U. S. Environmental Protection Agency. This report covers a period
from October to December 1993, and the work was completed as of December 7, 1993.
IV
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CONTENTS _
Section Page
DISCLAIMER . ................... ..... . . . . ......... ii
FOREWORD ............... . . ............................. .............. jii
ABSTRACT ............. . .................................... ............ iv
FIGURES [[[ ............ vii
TABLES ' ''"'""'
1 INTRODUCTION
2 FACILITY DESCRIPTION, WASTE CHARACTERISTICS, AND TEST
CONDITIONS ...... [[[ 2-1
2.1 ROTARY KILN INCINERATION SYSTEM DESCRIPTION ................. 2-1
2.1.1 Incinerator Characteristics .............................................. 2-4
2. 1.2 Air Pollution Control System ............................................ 2-5
2.2 TEST WASTE CHARACTERISTICS ............... 2-6
2.3 TEST CONDITIONS ................................... '...'.'.'.'.'.'.'.'.'.'.'.' 2-11
3 SAMPLING AND ANALYSIS PROCEDURES ..... .......................... 3.!
3.1 SAMPLING PROCEDURES ....... ' ................ 3_1
3.2 ANALYSIS METHODS ......................................... ]\\\[ '3_15
4 TEST RESULTS ........................... . ......... . ......... ............ 4-1
4.1 PROXIMATE AND ULTIMATE ANALYSIS RESULTS ........ 4-1
4.2 SVOC ANALYSIS RESULTS ........ . ......................... "" 4.4
4.3 VOC ANALYSIS RESULTS ................................... [". ...... 4.12
4.4 PCDD/PCDF ANALYSIS RESULTS ............................ '.'.'.'.':'.'.' 4-18
4.5 TRACE METAL AND TCLP ANALYSIS RESULTS ............... 4-31
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CONTENTS (continued)
Section
QUALITY ASSURANCE
6.1 VOC ANALYSES ........................ 62
6.2 SVOC ANALYSES ............. ; . . . . ........ '.'.'.'.'.'.'. ............... 6-13
6.3 TRACE METAL ANALYSES ............ ........................... 6~26
6.4 CHLORIDE ANALYSES .............. .... ........................... 6~42
6.5 PCDD/PCDF ANALYSES ............................ "!"!!!.'" ...... 6-42
REFERENCES ................................................. R.j
APPENDICES
(Volumes 2 and 3 can be obtained from Marta Richards.)
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FIGURES
Number D
Page
2-1 Schematic of the rotary kiln incineration system 2-2
3-1 Test sampling locations 3_2
3-2 Generalized CEM gas flow schematic 3.7
4-1 Afterburner exit particle size distributions 4.39
Vll
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TABLES
Number Page
2-1 Design characteristics of the IRF rotary kiln incineration system ... 2-3
2-2 M. W. Manufacturing site waste contaminants from the ROD 2-7
2-3 M. W. Manufacturing site characterization sample analysis results 2-8
2-4 M. W. Manufacturing site characterization sample hazardous waste characteristics
analysis results 2-9
2-5 Test matrix ; 2-12
2-6 APCS operating conditions 2-13
2-7 Kiln operating conditions 2-14
2-8 Afterburner operating conditions 2-15
2-9 Air pollution control system operating conditions 2-16
2-10 Continuous emission monitor data 2-17
3-1 Continuous emission monitors used and locations monitored 3-6
3-2 Analysis procedures 3_g
3-3 Test program sample analysis summary 3_10
3-4 Sample analysis aliquot schedule for each test 3_12
3-5 Sample containers, preservation methods, and hold times 3-14
3-6 Semivolatile organic TCL constituents 3_17
3-7 Volatile organic TCL constituents 3_lg
4-1 Proximate and elemental analysis results for composite fluff and soil feed samples 4-2
vm
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TABLES (continued)
Page
4-2 Weights of test material fed and kiln ash collected ........................... 4.3
4-3 Semivolatile organic contaminant analysis results ........................ 4.5
4-4 SVOCPOHCDREs .................................. 4.8
4-5 BEHP concentrations in replicate fluff waste samples ____ ....................... 4_10
4-6 SVOC contaminant concentrations in replicate soil samples ____ .......... 4-1 1
4-7 Volatile organic contaminant analysis results ................ 4. J3
4-8 Tetrachloroethene DREs .......... . ...................... 4_16
4-9 Flue gas VOC concentrations ........... . .............................. 4_17
4-10 PCDDs and PCDFs in test feed samples ................. . . 4_2Q
4-11 PCDDs and PCDFs in kiln ash samples . ...................................... 4_2i
4-12 PCDDs and PCDFs in scrubber liquor samples . ............................... 4_22
4-13 PCDDs and PCDFs in baghouse ash samples ................................... 4.23
4-14 PCDDs and PCDFs in baghouse exit flue gas ................ ................... 4_24
4-15 2,3,7,8-TCDD toxicity equivalent factors ....................................... 4.25
4-16 Total dioxins and TEQs in test program samples ..... . . ....................... 4-26
4-17 Ratio of discharged dioxins and furans to fed amounts .......................... 4-28
4-18 Trace metal analysis results ......................................... 4.32
4-19 TCLP leachate analysis results ........................................ 4.35
4-20 Particulate and HC1 emissions ......................................... 4.33
IX
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TABLES (continued)
Number page
6-1 Sample hold times for the VOC analyses of solid and liquid samples by GC/FID 6-3
6-2 Sample hold times for the VOC analyses of Method 0030 samples by GC/MS 6-5
6-3 VOC measurement QAOs ..." 6-6
6-4 VOC measurement MDLs: objectives and achieved levels 6-7
6-5 VOC recoveries from MS samples analyzed by GC/FID 6-8
6-6 VOC recoveries from MS samples analyzed by GC/MS 6-9
6-7 Duplicate sample VOC analysis results 6-10
6-8 VOC surrogate recoveries in the GC/FID analysis of test samples 6-11
6-9 VOC surrogate recoveries in the GC/MS analysis of Method 0030 samples 6-12
6-10 Sample hold times for the SVOC analyses by GC/MS 6-14
6-1T SVOC measurement QAOs 6-18
6-12 SVOC measurement MDLs: objectives and achieved levels 6-19
6-13 SVOC recoveries from solid and liquid MS samples analyzed by GC/MS 6-20
6-14 SVOC recoveries from the Method 0010 MS samples analyzed by GC/MS 6-21
6-15 SVOC surrogate recoveries in the GC/MS analysis of solid and liquid samples ... 6-23
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TABLES (continued)
Number Page
6-16 SVOC surrogate recoveries in the GC/MS analysis of Method 0010 flue gas samples ... 6-25
6-17 Sample hold times for trace metal analyses by ICAP 6-28
6-18 Trace metal measurement QAOs 6-32
6-19 Trace metal measurement MDLS: objectives and achieved levels 6-32
6-20 Trace metal analyses of method blank samples 6-33
6-21 Replicate trace metal sample analysis results 6-34
6-22 Trace metal recoveries from MS samples analyzed by ICAP 6-39
6-23 Sample hold times for chloride analyses by ion chromatography 6-43
6-24 Flue gas chloride measurements QAOs 6-43
6-25 Chloride recoveries from MS samples analyzed by ion chromatography 6-44
6-26 Duplicate sample chloride analysis results 6-44
6-27 Sample hold times for the PCDD/PCDF analyses by GC/MS 6-45
6-28 PCDD/PCDF measurement QAOs ; 6-47
6-29 Duplicate sample PCDD/PCDF analysis results 6-48
6-30 Internal standards recoveries in the PCDD/PCDF analyses 6-49
6-31 Surrogate recoveries in the PCDD/PCDF analyses 6-51
6-32 PCDD/PCDF measurement MDLs: objectives and achieved levels 6-53
XI
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SECTION 1
INTRODUCTION
One of the primary missions of the Environmental Protection Agency's (EPA's)
Incineration Research Facility (IRF) is to support Regional Offices in evaluations of the
potential of incineration as a treatment option for wastes and other contaminated materials at
Superfund sites. One priority site is the M. W. Manufacturing site in Danville, Pennsylvania.
EPA Region m and the U.S. Army Corps of Engineers (USAGE) requested that a pilot-scale
test program be conducted at the IRF to support evaluations of the suitability of incineration as
a treatment technology for wastes and contaminated soil at the site.
The M. W. Manufacturing site began operation in 1966. M. W. Manufacturing
Corporation reclaimed copper from scrap wire using both mechanical and chemical processes.
Reclamation activities began in 1969 and continued until 1972 when M. W. Manufacturing filed
for bankruptcy. The chemical recovery processes used by M. W. Manufacturing led to site
contamination with volatile organic solvents. Warehouse 81, Inc., acquired the site in 1976 and
began mechanical recovery operations from the existing waste piles onsite. The mechanical
recovery operations generated large volumes of waste material, termed fluff.
The fluff waste produced by the mechanical stripping process consists of fibrous
insulation material mixed with plastic. Phthalate esters, copper, and lead are the major
contaminants in this material. The chemical recovery process used by M. W. Manufacturing was
a two-step process. The first step involved the use of a hot oil bath to melt the plastic insulation
1-1
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away from the metal in the scrap wire. Residual oils were removed from the separated copper
in the second step through the use of chlorinated solvents, including trichloroethene and
tetrachloroethene. Thus, these solvents are waste and soil contaminants at the site.
The June 1990 record of decision (ROD) document for the site identified five wastes
and contaminated materials for remedial treatment:
Fluff waste piles
Organic- and trace-metals-contaminated surface soils
Organic- and trace-metals-contaminated subsurface soils
Lagoon water
Contents of drums and tanks
Onsite incineration was identified as the selected treatment for the fluff and the soil, with
possible stabilization of the incineration ash prior to landfill disposal. Other, non-incineration
remedies were selected for treating the lagoon water and the drum/tank contents.
Region HI requested the pilot-scale test program at the IRF to support the further
progress of the remediation of the site, and specifically to supply data on optimum incineration
conditions for both fluff waste and contaminated soil to the remediation design effort. The
specific objectives of the IRF test program were defined as follows:
Verify that the fluff waste and the contaminated soil at the site can be incinerated
in compliance with the hazardous waste incinerator performance standards and
permit requirements of:
99.99 percent principal organic hazardous constituent (POHC) destruction
and removal efficiency (DRE)
HC1 emissions less than 1 percent of the air pollution control system (APCS)
inlet flowrate or 1.8 kg/hr (4 Ib/hr), whichever is greater
1-2
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CO emissions of less than 100 ppm at 7 percent O2, 1-hour rolling average
and the performance guidance announced in 1993 of:
Particulate emissions of less than 34 mg/dscm (0.015 gr/dscf) corrected to
7 percent O2
Total tetra- through octa- polychlorinated dibenzo-p-dioxin and poly-
chlorinated dibenzofuran (PCDD/PCDF) emissions of less than 30 ng/dscm
corrected to 7 percent O2
Measure the effectiveness of incineration treatment in decontaminating fluff and
soil of their organic contaminants and evaluate whether incineration temperature
affects the effectiveness of fluff decontamination
Measure the distribution of the contaminant metals in the fluff and the
contaminated soil among the incineration system discharge streams
Determine whether the bottom ash residue and the APCS discharges from the
incineration of fluff and contaminated soil will be toxicity characteristic (TC)
hazardous wastes
Determine whether the bottom ash residue from the incineration of contaminated
soil meets the cleanup levels for soil given in the ROD
To address these objectives, a series of seven tests was performed in the rotary kiln
incineration system (RKS) at the IRF. Results of this test program are discussed in this report.
Section 2 of the report describes the IRF's RKS in which the tests were performed. Section 2
also discusses the composition of the fluff waste and contaminated soil incinerated in the tests,
and the test incinerator system operating conditions. The sampling and analysis procedures
employed during the tests are discussed in Section 3. Section 4 presents the test results.
Section 5 summarizes the test program conclusions. Section 6 discusses the quality assurance
1-3
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(QA) aspects of the test program. The Appendices provide a complete data set from which
information of interest can be extracted for further study.
1-4
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SECTION 2
FACILITY DESCRIPTION,
WASTE CHARACTERISTICS, AND TEST CONDITIONS
A description of the RKS is presented in Section 2.1. Section 2.2 describes the
composition and characteristics of the fluff waste and contaminated soil as reported in earlier
site remedial investigation reports. The test matrix and incinerator operating conditions are
discussed in Section 2.3.
2.1 ROTARY KILN INCINERATION SYSTEM DESCRIPTION
A process schematic of the RKS is shown in Figure 2-1 and the system design
characteristics are listed in Table 2-1. The RKS consists of a rotary kiln primary combustion
chamber, a transition section, a fired afterburner chamber, and an afterburner extension for flue
gas flow conditioning to allow isokinetic sampling of afterburner exit flue gas. After exiting the
afterburner extension, flue gas flows through a quench section followed by a primary air pollution
control system (APCS). The initial element of the primary APCS for these tests consisted of a
venturi/packed column scrubber system which removes most of the coarse particulate and acid
gas such as HC1 in the flue gas. Downstream of the scrubber system, a 100-kW electric
resistance heater reheats the flue gas to about 120°C (250°F) which is about 22°C (40°F) above
the saturation temperature. A fabric-filter baghouse downstream of the reheater removes most
of the remaining flue gas particulate. Reheating the flue gas prevents moisture condensation, in
the baghouse, which if allowed to occur, would adversely affect baghouse operation. The flue
2-1
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to
N)
NATURAL
GAS,
LIQUID
FEED
TRANSFER
DUCT
PACKED
COLUMN
SCRUBBER
SECONDARY
BURNER
VENTURI
SCRUBBER
AFTERBURNER
EXTENSION
SCRUBBER
LIQUOR
RECIRCULATION
AFTERBURNER
SOLIDS
FEEDER
FLUE GAS
REHEATER
NATURAL
GAS,
LIQUID FEED
PRIMARY AIR POLLUTION
CONTROL SYSTEM
CARBON BED HEPA
ADSORBER FILTER
BA HOUSE
ROTARY KILN
INCINERATOR
REDUNDANT AIR
POLLUTION CONTROL
SYSTEM
o
ATMOSPHERE
STACK
ps»r
ID FAN
Figure 2-1. Schematic of the rotary kiln incineration system.
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TABLE 2-1. DESIGN CHARACTERISTICS OF THE IRF ROTARY KILN INCINERATION
SYSTEM
Characteristics of the Kiln Main Chamber
Length 2.26 m (7 ft-5 in)
Diameter, outside 137 m (4 ft-6 in)
Diameter, inside Nominal 1.04 m (3 ft-4.75 in)
Chamber volume 1.90 m3 (613. ft3)
Construction 0.95 cm (0375 in) thick cold-rolled steel
Refractory 18.7 cm (7375 in) thick high, alumina castable refractory, variable depth to produce a
frustroconical effect for moving solids
Rotation Clockwise or counterclockwise, 0.2 to 1.5 rpm
Solids retention time 1 hr (at 0.2 rpm)
Burner North American burner rated at 590 kW (2.0 MMBtu/hr) with liquid feed capability
Primary fuel Natural gas
Feed system:
Liquids Positive displacement pump via water-cooled lance
Sludges Moyno pump via front face, water-cooled lance
Solids Metered screw feeders or fiberpack ram feeder
Temperature (max) I.OIO'C (1,850°F)
Characteristics of the Afterburner Chamber
Length 3.05 m (10 ft)
Diameter, outside 1.22 m (4 ft)
Diameter, inside 0.91 m (3 ft)
Chamber volume 1.80 m3 (63.6 ft3)
Construction 0.63 cm (0.25 in) thick cold-rolled steel
Refractory 15.2 cm (6 in) thick high alumina castable refractory
Gas residence time 0.8 to 1.5 s depending on temperature and excess air
Burner North American Burner rated at 590 kW (2.0 MMBtu/hr) with liquid feed capability
Primary fuel Natural gas
Temperature (max) 1,200°C (2,200''F)
Characteristics of the Afterburner Extension
Length, with transition 4.43 m (14 ft-6.5 in)
sections
Diameter, outside 0.915 m (3 ft)
Diameter, inside 0.61 m (2 ft)
Chamber volume . 1.19 m3 (41.9 ft3)
Construction 0.63 cm (0.25 in) thick cold-rolled steel
Refractory 15.2 cm (6 in) thick high alumina castable refractory
Temperature (max) 1,200°C (2,200°F)
Characteristics of the Venturi/Packed-column Scrubber APCS
System capacity, inlet gas 107 m3/min (3,773 acfm) at l,200eC (2,2000F) and 101 kPa (14.7 psia)
flow
Pressure Drop
Venturi scrubber 75 kPa (30 in WC)
Packed column 1.0 kPa (4 in WC)
Liquid flow
Venturi scrubber 77.2 L/min (20.4 gpm) at 60 kPa (10 psig)
Packed column 116 L/min (30.6 gpm) at 69 kPa (10 psig)
pH control Feedback control by NaOH solution addition
' (continued)
2-3
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TABLE 2-1. (continued)
Characteristics of the Baghouse Collector
System capacity, inlet gas 70 m3/min (2,500 acfm) at 120eC (250'F)
flow
Operating temperature 200°C (400eF)
Operating pressure ±12.4 kPa (±50 in WC)
Diameter 1.8 m (6 ft)
Overall height 42 m (13 ft, 8375 in)
Filter elements (bags)
Material 16 oz. Nomex
Length 1.8m (6 ft)
Number 69
Total filter area 45 m2 (488 ft2)
Material of construction
Collector internals 304 SS
Airlock 316 SS
Venturi nozzles Aluminum
Insulation Heat loss less than 8.8 kW
(30,000 Btu/hr) at 200°C (400°F)
gas reheat/baghouse system was installed just prior to the initiation of these tests, in large part
to satisfy a Region III request.
Downstream of the baghouse, a backup secondary APCS, comprised of an activated-
carbon adsorber and a high-efficiency particulate air (HEPA) filter, is in place for further control
of organic compound and particulate emissions. The main components of the RKS and its APCS
are discussed in more detail in the following subsections.
2.1.1 Incinerator Characteristics
The rotary kiln combustion chamber has an inside diameter of 1.04-m (40.75-in) and is
2.26-m (7-ft 5-in) long. The chamber is lined with refractory formed into a frustroconical shape
to an average thickness of 18.7 cm (7.375 in). The refractory is encased in a 0.95-cm (0.375-in)
thick steel shell. Total volume of the kiln chamber; including the transition section, is 1.90 m3
(67.2 ft3). Four steel rollers support the kiln barrel. A variable-speed DC-motor coupled to a
reducing gear transmission turns the kiln. Rotation speeds can be varied from 0.2 to 1.5 rpm.
For these tests the kiln rotational speed was 0.2 rpm.
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The afterburner chamber has a 0.91-m (3-ft) inside diameter, and is 3.05 m (10 ft) long.
The afterburner wall is constructed of a 15.2-cm (6-in) thick layer of refractory encased in a
0.63 cm (0.25 in) thick carbon steel shell. The volume of the afterburner chamber is 1.80 m3
(63.6ft3).
2.1.2 Air Pollution Control System
For this test program, the RKS primary APCS consisted of the venturi scrubber/packed-
column scrubber combination, followed by a flue gas reheater and a baghouse. The flue gas
exiting the afterburner passes through the refractory-lined transfer section and enters the quench
section, where the flue gas temperature is reduced to approximately 82°C (180°F) by direct
injection of aqueous caustic scrubber liquor. The cooled flue gas then enters the venturi
scrubber, which is fitted with an automatically adjustable-area throat. The scrubber is designed
to operate at 6.2 kPa (25 in WC) differential pressure, with a maximum liquor flowrate of
77.2 L/min (20.4 gpm). The scrubber liquor, again an aqueous caustic solution, enters at the top
of the scrubber and contacts the flue gas to remove entrained particles and, to some degree, acid
gases.
Downstream of the venturi scrubber, the flue gas enters the packed-column scrubber,
where additional acid gas and particulate cleanup occurs. The scrubber column is packed with
5.1 cm (2 in) diameter polypropylene ballast saddles to a depth of 2.1 m (82 in). It is designed
to operate at 1.0 kPa (4 in WC) differential pressure, with a maximum liquor flowrate of
116 L/min (30.6 gpm).
The quench, venturi scrubber, and packed-column scrubbers receive their scrubber liquor
from the same recirculation system. This liquor is a dilute aqueous NaOH solution, the pH of
which is monitored continuously by a pH sensor. An integral pH controller automatically meters
the amount of NaOH needed to maintain the setpoint pH for proper acid gas removal.
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Following the quench, venturi scrubber, and packed-column scrubber systems, the flue
gas is reheated to about 120 °C (250 °F) by a 100-kW electric duct heater, and then passed
through the baghouse. The baghouse removes most of the remaining flue gas participate.
Reheating the flue gas ensures that no moisture condenses in the baghouse, which can adversely
affect its operation.
In a typical commercial incinerator system, the flue gas would be vented to the
atmosphere downstream of the baghouse. However, at the IRF, a backup APCS is in place to
further clean up the flue gas. The flue gas exiting the baghouse is passed through a bed of
activated carbon to allow the vapor-phase organic compounds to be adsorbed. A set of HEPA
filters designed to remove any remaining suspended paniculate from the flue gas is located
downstream of the carbon bed. An induced-draft (ID) fan draws and vents the treated flue gas
to the atmosphere.
22 TEST WASTE CHARACTERISTICS
Data on the contaminant concentrations in the fluff waste and the surface and
subsurface soil at the site, taken from the site record of decision (ROD) document, are
summarized in Table 2-2. Only contaminants present at an average concentration of 1 mg/kg
or greater in one or more contaminated site matrix are listed in the table. The data in Table 2-2
show that the major site contaminants are the two phthalate esters, bis(2-ethylhexyl)phthalate
(BEHP) and di-n-octylphthalate (DNOP). Thus, these compounds would be considered the
POHCs in the site wastes. In addition, Region ffl was interested in establishing that
tetrachloroethene is effectively destroyed by incineration, so tetrachloroethene was also defined
to be a POHC. Site wastes are also highly contaminated with copper and lead, with lesser,
though still significant, amounts of antimony, barium, chromium, nickel, and zinc.
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TABLE 2-2. M. W. MANUFACTURING SITE WASTE CONTAMINANTS FROM THE ROD
Concentration, mg/kg
Fluff
Contaminant
Volatile Organic Constituents
2-Butanone
Tetrachloroethene
Trichloroethene
1,1,2-Trichloroethane
1,2-Dichloroethene
Methylene chloride
Semivolatile Organic Constituents
Bis(2-ethylhexyl)phthalate
Di-n-octyl phthalate
Di-n-butyl phthalate
PCB-1254
Trace Metals
Antimony
Barium
Cadmium
Chromium
Copper
Lead
Nickel
Silver
Zinc
Range over
17 samples
2.8-6.4
0.72-18.0
up to 7.7
72,000-230,000
1.800-13,000
0.90-18.1
80-143
20-232
0.65-4.4
24-59
5,910-130,000
1,600-3,600
4.1-15
1.6-5.7
135-2,580
Average
1.6
4.4
0.45
149,000
4,400
9.4
65
93
2.4
40
50,000
2,400
4.6
1.8
620
Surface soil
Range over
21 samples
_«
0.023-67
0.002-21
0.003-2.8
0.002-10
up to 0.83
3.9-3,000
0.2-140
0.48
0.061-3.7
62-118
22-107
1.2-12
7.1-59
742-171,000
32-9,770
8.5-40
8.6
55-787
Average
10
1.0
0.28
0.49
0.04
836
37
0.02
0.21
16
74
2.0
27
21,600
1,450
22
0.4
240
Maximum average
subsurface soil
Range
up to 3.9
0.001-l,600b
0.002-2.6
up to 5.4
0.004-0.58
-
OJO-30,OOOb
0.038-150
0.036-130
0.077-1.0
, ,
47-218
1-13
14-70
24-38,900
7-741
42-50
.
56-319
Average
0.78
56
2.7
1.1
0.04
1,480 '
7,850
3.9
0.043
1 T
107
1
20
1,850
160
46
__
144
Depth
16-18
4-6
12-14
16-18
8-10
12-14
0-2
0-2
0-2
v
0-2
0-2
0-14
12-14
16-18
6-8
_
6-8
* = Not reported.
bMaximum value in range represents an estimated value above minimum detection limit but below lowest calibration standard ("J" flag).
-------
Samples of the fluff waste and surface and subsurface soil were sent to the IRF for
characterization analyses. Results of the analyses are summarized in Table 2-3. As shown, the
soil characterization samples had contaminant concentrations in the range reported in the ROD.
Contaminant concentrations in the fluff waste characterization samples were also in the range
reported in the ROD for most contaminants. However, the fluff characterization sample
TABLE 2-3. M. W. MANUFACTURING SITE CHARACTERIZATION SAMPLE ANALYSIS
RESULTS
Sample
Parameter
Characterization
Moisture, %
Ash, %
at 550°C
at 900°C
Heating value, MJ/kg
(Btu/lb)
Volatile Organic Constituents, mg/kg
Tetrachloroethene
1, 1,2-Trichloroethane
Semivolatile Organic Constituents, mg/kg
BEHP
DNOP
Trace Metals, mg/kg
Antimony
Barium
Cadmium
Chromium
Copper
Lead
Nickel
Silver
Zinc
Fluff
7.7
41
14
6.50
(2,800)
146
4.8
124,000
17,800
230
64
3.5
57
31,000
2,700
6.1
4.0
890
Surface soil
18
77
76
0.07
(30)
69
1.5
47.6
1.95
51
60
<0.2
30
8,300
1,800
15
<0.4
76
Subsurface soil
9.8
89
90
Will not burn
18
NDa
4.62
ND
<5
78
0.93
21
160
180
31
<0.4
62
aND = Not detected.
2-8
-------
contained substantially more tetrachloroethene, 1,1,2-trichloroethane, DNOP, and antimony that
did fluff samples reported in the ROD.
Characterization samples received were also analyzed for hazardous waste
characteristics, including the preparation and analysis of toxicity characteristic leaching procedure
(TCLP) leachates of the samples. Results are summarized in Table 2-4.
The two semivolatile POHCs in site materials, BEHP and DNOP, are poor candidates
for testing the incineration process with regard to destroying other site, waste organic
contaminants because they are ranked as relatively easy to thermally destroy compounds in the
TABLE 2-4. M. W. MANUFACTURING SITE CHARACTERIZATION SAMPLE
HAZARDOUS WASTE CHARACTERISTICS ANALYSIS RESULTS
Characteristic
Reactivity -S, mg/kg
Reactivity -CN, mg/kg
Corrosivity, pH
Ignitability, °F
TCLP leachate,. mg/L
Arsenic
Barium
Cadmium
Chromium
Copper
Lead
Mercury
Nickel
Selenium
Silver
Zinc
Pesticides and other organics
Fluff
waste
<0.01
<0.01
6.85
>200
<0.10
0.10
0.11
0.11
199
3.1
< 0.002
<0.01
<0.10
<0.01
5.1
NDb
Surface
soU
<0.01
<0.01
8.15
>200
<0.10
0.37
0.07
0.09
158
3.2
< 0.002
<0.01
<0.10
<0.01
0.49
ND
Subsurface
soil
<0.01
<0.01
6.37
>200
<0.10
0.21
0.07
0.09
1.88
0.20
< 0.002
<0.01
<0.10
<0.01
0.12
ND
Regulatory
level
Contains
and reacts
<2, >12
<140
5.0
100
1.0
5.0
__a
5.0
0.2
1.0
5.0
a = No regulatory level.
bND = Not detected at detection limits ranging from 0.004 to 0.01 mg/L.
2-9
-------
thermal stability based incinerability ranking (Reference 1). This ranking groups the 333
compounds ranked into seven stability classes from most stable, or most difficult to destroy
(Class 1), to least stable or easiest to destroy (Class 7). Both BEHP and DNOP are ranked in
Class 6, or relatively easy to destroy. To present a challenge to the incineration process and
develop data that suggest incineration is capable of achieving sufficient DREs for other site
organic contaminants, the test waste materials were spiked with naphthalene, a Class 1 (most
difficult to destroy) POHC, at 2 percent by weight. This spiking level allows DREs of over
99.999 percent to be quantitated at easily achieved flue gas sampling and analysis method
quantitation limits. In addition, it was decided to spike the volatile POHC, tetrachloroethene,
into test materials at a level of 3,100 mg/kg by weight. Tetrachloroethene is a Class 2 POHC.
Spiking was needed because site material concentrations of tetrachloroethene were too low to
allow establishing 99.99 percent DRE at achievable flue gas concentration quantitation limits.
Prior to initiating the test program, all test feed material was packaged into 1.5-gal
(5.7-L) polyethylene (PE)-bag-lined cubical cardboard containers for feeding to the RKS. For
fluff packaging, the contents of three 55-gal (208-L) shipment drums (of the 14 fluff-containing
drums received at the IRF for testing) were emptied into a 250-gal (946-L) mixing trough. The
trough contents were manually mixed with hoes until visually homogeneous. Trough contents
were then used to fill feed containers. Each container was filled with about 1.8 kg (4 Ib) of
mixed fluff. A mixed trough would fill 150 containers, with a small quantity left over. This small
quantity would be combined with the next three drums added to the trough for mixing.
This mixing process resulted in four full-trough fluff batches, with each batch used to
package 150 feed containers. All containers from a given batch were placed on a pallet for
short-term storage, resulting in four 150-container pallets. A fifth partial-trough batch was used
to package a final 120 feed containers, which were placed on a fifth pallet. The containers on
2-10
-------
the fifth pallet were used during scoping tests to verify the ability to feed the test material and
maintain target RKS operating conditions. For each of the actual four fluff incineration tests
performed, essentially equal numbers of Containers were randomly selected from each of the first
four pallets to constitute the feed materials for the test.
Naphthalene was added to each fluff-filled box as a preweighed count of solid
naphthalene crystals (36.4 g) contained in a 60-mL high-density polyethylene (HDPE) bottle with
a polypropylene screw cap closure, weighing about 14.4 g. The tetrachloroethene (5.6 g) was
added in a 4-mL HDPE bottle, with a polypropylene screw cap closure, weighing 2.6 g. Feed
boxes were spiked the day before a given test by imbedding the HDPE bottles in the feed box
contents. The box polyethylene liner was then closed with a plastic tie, and the box itself dosed
and sealed with paper packaging tape.
Contaminated soil for testing was similarly mixed, except that all five of the drums of
soil received at the IRF for testing (whether surface, subsurface, or mixed not specified) were
mixed in one trough mixing exercise. Mixed soil was packaged into the 120 feed containers, each
containing about 4.5-kg (10-lb) of soil. The naphthalene spike added the day before a soil test
was 90.9 g in a 125-mL HDPE bottle, and the tetrachloroethene spike was 14.5 g in an 8-rnL
bottle.
23 TEST CONDITIONS
The test program completed consisted of seven tests. Of these seven, two sets of
duplicate tests feeding fluff waste alone and one set of duplicate tests feeding contaminated soil
alone were performed. The two sets of fluff feed tests were conducted at different kfln
combustion gas temperatures. Soil and fluff were separately tested because the eventual site
remediation may treat each material separately for logistical reasons. In addition, Region in
2-11
-------
requested data to determine whether the ash from incinerated soil alone would meet the cleanup
levels given in the ROD. The target test operating conditions were as given in Table 2-5.
A seventh test, denoted Test 0 in Table 2-5, was performed as a blank burn. Only feed
packaging materials - the cardboard box, PE bag liner, HDPE spike bottles (no POHC spike)
with closures, plastic tie, and paper tape were fed to the RKS for the blank burn.
For all tests, the target afterburner exit gas temperature was 1,090 °C (2,000 °F). The
venturi/packed-column scrubber and baghouse APCS units were operated at their normal design
settings. Kiln rotation rate was set to give a 30-minute kiln solids residence time.
The target average test material feedrate was 54.5 kg/hr (120 Ib/hr) for all tests except
the blank burn. Test materials were fed to the RKS via the fiberboard container ram feed
system. A total of 30 containers per hour (one container every 2 minutes) was fed to achieve
the target feedrate for the fluff tests; 12 containers per hour (one container every 5 minutes)
were fed to achieve the target feedrate for the soil tests. The blank burn was conducted feeding
30 containers (no waste or soil) per hour.
For all tests, the scrubber system was operated at its design settings, listed in Table 2-6,
and at as close to total recirculation (zero to minimum blowdown) as possible. Given the
TABLE 2-5. TEST MATRIX
Test
0
1
2
3
4
5
6
Feed
Packaging container material
Fluff
Duplicate of Test 1
Soil
Duplicate of Test 3
Fluff
Duplicate of Test 5
Target kiln exit gas temperature,
O^t /O'K*\
** V. '/
870 (1,600)
870 (1,600)
870(1,600)
760 (1,400)
2-12
-------
TABLE 2-6. APCS OPERATING CONDITIONS
Venturi liquor flowrate 76 L/min (20 gpm)
Venturi pressure drop 6.2 kPa (25 in WC)
Packed tower liquor flowrate, 115 L/min (30 gpm)
Scrubber liquor temperature 49 °C (120 °F)
Scrubber blowdown rate 0 L/min (0 gpm) or minimum operable
relatively short (nominally 4 to 5 hours) duration of a test, no operational problems due to solids
buildup in the scrubber liquor occurred even at total recirculation. For the fluff waste and blank
burn tests, kiln ash was continuously deposited in initially clean 20-gal (76-L) drums placed in
the RKS ash pit. For the soil tests, kiln ash was continuously removed from the kiln ash hopper
via an ash auger transfer system and deposited into 55-gal (208-L) drums.
The actual kiln and afterburner operating conditions achieved for each test are
summarized in Tables 2-7 and 2-8, respectively. Table 2-9 provides a similar summary of the
APCS operating conditions for each test. Continuous emission monitor (CEM) data are
summarized in Table 2-10. The ranges and averages of the temperature, CEM, and scrubber pH
data presented in Tables 2-7 through 2-10 were developed for the periods of the flue gas
sampling, using the data automatically recorded by a personal computer-based data acquisition
system. The values given for the remaining parameters were derived from the control room
logbook data.
Transcribed data from the control room logs of the operating parameters, recorded at
15-minute intervals, are given in Appendix A. Appendix B contains graphic presentations of the
flue gas temperature and continuous emission monitor data for the kiln and afterburner.
Appendix B also contains graphic presentations of the scrubber exit and stack flue gas continuous
emissions monitor data. These data plots were based on incinerator system conditions recorded
2-13
-------
TABLE 2=7. KILN OPERATING CONDITIONS
to
Parameter
Average natural gas
feedrate,
Average combustion air
flowrate,
Average total air flowrate
(includes inleakage),
Average draft,
Exit gas temperature,
Exit gas O2
Average waste feedrate,
Average waste heat input,
Total heat input,
=====
scm/hr
(scfh)
kW
(kBtu/hr)
scm/hr
(scfh)
scm/hr
(scfh)
Pa
(inWC)
Range, "C
(F)
Average, "C
(°F)
Range, %
Average, %
kg/hr
(Ib/hr)
kW
(kBtu/hr)'
kW
(kBtu/hr)
TestO
(10/27/93)
33
(1,156)
339
(1,156)
226
(7,970)
679
(23,980)
7
0.03
842-898
(1,548-1,648)
871
(1,599)
8.4-13.4
11.6
5
(12) .
10
(34)
349
(1,190)
Testl
(11/9/93)
22
(778)
228
(778)
214
(7,560)
1,054
(37,200)
7
0.03
827-921
(1,520-1,689)
883
(1,622)
7.7-14.0
10.9
60
(132)
224
(765)
452
(1,543)
Test 2
(11/16/93)
23
(820)
240
(820)
205
(7,250)
1,067
(37,670)
7
0.03
814-918
(1,498-1,685)
876
(1,608)
8.2-14.6
11.0
59
(130)
218
(743)
458
(1,563)
======
TestS
(11/18/93)
13
(475)
139
(475)
191
(6,760)
1,000
(35^00)
5
0.02
716-804
(1321-1,479)
762
(1,403)
8.7-14.2
11.8
61
(134)
227
(774)
366
(1,249)
Test 6
(11/23/93)
14
(507)
149
(507)
174
(6,140)
1,008
(35,610)
7
0.03
724-807
(1336-1,484)
767
(1,412)
9.0-14.0
11.8
61
(134)
224
(765)
373
(1,272)
Test 3
(12/1/93)
JQ
J\t
(1,065)
312
(1,065)
200
(7,070)
675
(23,840)
5
0.02
853-912
(1,568-1,674)
876
(1,609)
8.0-13.5
11.1
59
(130)
30
(104)
342
(1,169)
.
Test 4
(12/2/93)
31
(1,085)
318
(1,085)
19ft
ixO
(6,990)
673
(23,750)
0.02
862-894
(1,583-1,642)
874
(1,606)
7.7-13.1
10.9
59
(130)
31 "
(104)
348
«J*tO
(1,189)
Calculated combustion gas
residence time,
seconds
-------
TABLE 2-8. AFTERBURNER OPERATING CONDITIONS
Parameter
Average natural gas
feedrate,
Average combustion air
flowrate,
Exit gas temperature,
Exit gas O2
scm/hr
(scfh)
kW
(kBtu/hr)
scm/hr
(scfh)
Range, "C
(F)
Average, °C
(F)
Range, %
Average, %
TestO
(10/27/93)
29
(1,025)
300
(1,025)
194
(6,840)
1,090-1,107
(1,994-2,025)
1,098
(2,008)
8.8-12.0
10.7
Testl
(11/9/93)
27
(948)
278
(948)
165
(5,830)
1,089-1,152
(1,992-2,106)
1,103
(2,017)
4.2-11.7
7.6
Test 2
(11/16/93)
26
(903)
265
(903)
156
(5,520)
1,087-1,105
(1,989-2,021)
1,097
(2,007)
5.7-10.8
8.2.
Test 5
(11/18/93)
24
(861)
252
(861)
129
(4,550)
1,091-1,105
(1,996-2,021)
1,097
(2,007)
5.1-10.8
8.0
Test 6
(11/23/93)
25
(876)
257
(876)
118
(4,180)
1,091-1,102
(1,995-2,016)
1,097
(2,007)
5.1-9.1
7.9
Test 3
(12/1/93)
27
(943)
276
(943)
157
(5,540)
1,091-1,115
(1,196-2,039)
1,098
(2,008)
8.7-14.2
11.8
Test 4
(12/2/93)
33
(1,166)
342
(1,166)
161
(5,700)
1,090-1,106
(1,994-2,023)
1,097
(2,007)
9.0-14.0
11.8
-------
TABLE 2-9. AIR POLLUTION CONTROL SYSTEM OPERATING CONDITIONS
ii =^^^s^aa
Parameter
Average quench chamber
liquid flowrate,
Average venturi scrubber
liquid flowrate
Average packed-column
scrubber liquid flowrate,
Scrubber liquor, pH
Average scrubber- makeup
flowrate,
Average scrubber liquor
temperature,
Average scrubber inlet gas
temperature,
Average scrubber exit gas
temperature,
===========.
L/min
(gpm)
L/min
(gpm)
L/min
(gpm)
Range
Average
L/min
(gpm)
«c
(°F)
«c
(.F)
«c
(°F)
TestO
(10/27/93)
76
(20)
76
(20)
114
(30)
6.9-7.1
7.0
1,098
(290)
67
(152)
76
(169)
59
(138)
i3SS355BS2KHH
=====
Test 1
(H/9/93)
76
(20)
79
(21)
110
(29)
5.9-8.2
6.9
57
(15)
69
(156)
78
(173)
64.
(147)
=====
========
Test 2
(11/16/93)
75
(20)
76
(20)
114
(30)
6.0-83
7.1
0
(0)
69
(156)'
78
(173)
64
(147)
=====
==
Test 5
(11/18/93)
76
(20)
79
(21)
114
(30)
6.8-8.2
7.3
193
(51)
67
(152)
77
(171)
60
(140)
Test 6
(11/23/93)
If.
/U
(20)
79
(21)
114
(30)
6.4-8.2
7.2
o
(0)
68
(155)
77
(171)
62
UA>
(143)
^^ -^ .
Test 3
(12/1/93)
72
(19)
QO
OJ
(22)
110
(29)
6.7-75
7.2
(3)
f.Q
oy
(156)
7/»
/O
(169)
£1
Ol
(141)
Test 4
(12/2/93)
1C.
76
(20)
*TiT
76
(20)
114
(30)
6.6-7.5
7.2
(0)
sn
by
(156)
*7£
76
(169)
£*
61
.("I)
-------
TABLE 240. CONTINUOUS EMISSION MONITOR DATA
Parameter
Kiln Exit
02
Afterburner Exit
02
C02
NOX
Baghouse Exit
02
CO
C02
TUHC
NOX
Stack
02
CO
Range, %
Average, %
Target, %
Range, %
Average, %
Target, %
Range, %
Average, %
Range, ppm
Average, ppm
Range, %
Average, %
Range, ppm
Average, ppm
Range, %
Average, %
Range, ppm
Average, ppm
Range, ppm
Average, ppm
Range, %
Average, %
Range, ppm
Average, ppm
TestO
(10/27/93)
8.4-13.4
11.6
10.0
8.8-12.0
10.7
8.0
53-8.1
6.2
45-82
66
12.0-15.1
12.9
<1-10
2
2.5-5.2
4.3
-------
at about 35-second intervals on the RKS data acquisition system. In addition, durations of flue
gas sampling periods, major events, cumulative amounts of waste fed into the incinerator, and
cumulative amounts of ash removed from the incinerator are included in some plots. These data
provide the basis for assembling a complete picture of the actual incinerator operating
conditions.
2-18
-------
SECTION 3
SAMPLING AND ANALYSIS PROCEDURES
The scope of the sampling efforts performed in the test program is illustrated in
Figure 3-1. The sampling effort performed is discussed in Section 3.1, followed by a discussion
of the sample analysis procedures in Section 3.2.
3.1 SAMPLING PROCEDURES
For all tests, the sampling matrix included:
Obtaining a composite sample of the test feed material
Obtaining a composite sample of the kiln ash discharge
Obtaining a composite sample of the pre-test and post-test scrubber system liquor
Obtaining a composite sample of the baghouse ash
Continuously measuring O2 concentrations in the kiln exit flue gas; O2, CO2, and
NOX in the afterburner exit flue gas; O2, CO, CO2, NOX, and total unhurried
hydrocarbon (TUHC) concentrations in the baghouse exit flue gas; and O2 and
CO concentrations in the stack gas
Sampling the flue gas at the baghouse exit for trace metals using the EPA multiple
metals train (Reference 2)
Sampling the flue gas at the baghouse exit for the waste and spiked semivolatile
POHCs and other semivolatile target compound list (TCL) constituents using an
EPA Method 0010 train (Reference 3)
3-1
-------
KILN
1
AFTER-
BURNER
FLUE GAS
QUENCH
2 3
VENTURI
SCRUBBER
1
PACKED
COLUMN
SCRUBBER
1
5
FLUE GAS
REHEAT
RAftMni IQP
1
6
7
CARBON
BED
HEPA
FILTER
u>
Continuous monitors
Test feed Kiln Scrubber Baghouse Healed
Sampling point material ash liquor ash O2 CO CO2 NO, TUHC
Flue gas
EPA multiple
metals train, Method 5,
test trace Method 0010, Method 0030, Method 23, participate
metals SVOCs VOCs PCDD/PCDF and HCI
1. Feed X
2. Kiln ash discharge X
3. Kiln exit flue gas
4. Afterburner exit
flue gas
X
XXX
5. Scrubber liquor
6. Baghouse hopper
7. Baghouse exit flue
X X X X
X
8. Stack gas
X X
Figure 3-1. Test sampling locations.
-------
Sampling the flue gas at the baghouse exit for the waste and spiked volatile
organic contaminants and other volatile fCL constituents using EPA Method 0030
(Reference 3), the volatile organic sampling train (VOST)
Sampling the flue gas at the baghouse exit for PCDDs/PCDFs using EPA
Method 23 (Reference 2)
Sampling the baghouse exit and the stack for particulate and HC1 using EPA
MethodS; the stack sample was needed to comply with the IRF's permit
requirements
Composite feed material samples were collected from each mixing trough after feed
material was mixed in the trough, as discussed in Section 2.2, but before packaging into the
cardboard containers. Samples were collected from six different locations in the trough and
combined to form the composite sample representing the trough's contents. Four fluff feed
samples resulted, each representing one full trough mixture. Two soil feed samples resulted, the
first taken before the packaging of the first soil feed container, the second after-the filling of 60
soil feed containers.
The feed sample for Test 0, the blank burn test, consisted of proportionate samples of
the cardboard box material, the polyethylene liner bag, the bag plastic tie, the HDPE bottle with
screw cap, and the paper packaging tape used to prepare feed boxes.
On a given test day, the incinerator was brought to nominally steady operation at test
conditions while firing auxiliary fuel (natural gas) alone. Test material feed was then initiated.
Flue gas sampling was started about 1 hour after test material feed initiation. At the conclusion
of each test day, the incinerator was operated on natural gas for 2 hours after waste feed
cessation while ash material in the kiln continued to discharge until the kiln was empty.
3-3
-------
During the fluff waste tests, kiln ash was continuously deposited in an initially dean
20-gal (76-L) drum placed in the RKS ash pit. The amount of collected ash was insufficient to
allow representative thief sampling, therefore grab samples consisting of a large fraction of the
collected ash were taken.
During the soil feed tests, kiln ash was continuously removed from the kiln ash pit via
a transfer auger and deposited into a 55-gal (208-L) drum. After all test ash was deposited in
this drum, representative kiln ash samples were taken by thief sampling in at least three locations
across the collection drum cross section. The three ash samples were combined to form one
composite sample.
No kiln ash resulted from the blank burn test.
Each test was run with the scrubber liquor loop operating at as close to total recycle (no
blowdown) as possible. At the end of each test day, a scrubber liquor sample was collected from
a tap in the recirculation loop. The scrubber liquor was then drained to a collection tank. In
addition, a sample was taken from the scrubber liquor loop from the same tap just before
initiating test material feed on a test day. The baghouse ash sample consisted of the entire
amount of baghouse ash collected in the baghouse ash hopper for each test.
The Method 5 trains for participate and HC1 collection had dilute caustic-filled
impingers (0.1 N NaOH). Admittedly, both HC1 and C12 in the flue gas are collected caustic
impingers. However, this conservative estimate of HC1 concentrations (HC1 plus C12) satisfied
test program objectives. A nominal 1.4 m3 (50 ft3) sample was collected at the two locations
sampled over about a 1-hour time period. The Method 0010, Method 23, and multiple metals
trains sampled nominally 2.8 m3 (100 ft3) of flue gas over a 3-hour period. Because mercury was
not a trace metal of interest in this program, the permanganate impingers for mercury collection
were not used in the multiple metals train, and sample recovery steps specified for eventual
3-4
-------
mercury analysis were not performed. Four Method 0030 trap pairs each sampled 20 L of flue
gas. Four trap pairs were taken as insurance against trap breakage.
The CEMs available at the IRF and the locations that they monitored during all tests
are summarized in Table 3-1. This monitoring arrangement was employed in all tests.
Figure 3-2 illustrates the generalized flue gas conditioning and flow distribution system at the
IRF. Four independent systems, such as the one illustrated in Figure 3-2, were in place so that
the appropriately conditioned sample gas from four separate locations was routed to the
respective monitors in Table 3-1. The CEM setup described in Table 3-1, with appropriate gas
conditioning per Figure 3-2, was employed throughout this test program. CEM data was
recorded continuously on strip charts and also by an automatic data acquisition system.
Test program samples were analyzed for matrix-specific combinations of SVOCs, VOCs,
PCDDs/PCDFs, contaminant trace metals, and chloride. Sample analysis procedures are
outlined in Table 3-2. The number of test program samples analyzed is summarized in Table 3-3.
The numbers of method blank, split sample, and matrix spike/matrix spike duplicate QA analyses
are also given in Table 3-3. The large numbers of fluff and soil feed split sample analyses for
SVOC and trace metals, and kiln ash split sample analyses for trace metals, were at the request
of Region HI. The Region HI Remediation Project Manager (RPM) requested that the
precision of the feed and ash trace metal and feed SVOC concentration measurements be well
characterized.
Table 3-4 summarizes the sample aliquoting schedule for dividing samples taken for each
test among the various analytical procedures. Each sample was divided among the various
analytical procedures according to Table 3-4. Aliquots analyzed as noted in Table 3-4
corresponded to respective method-recommended sample sizes.
3-5
-------
TABLE 3-1. CONTINUOUS EMISSIONMONITORS USED AND LOCATIONS MONITORED
Monitor
Location
Kiln exit
Afterburner
exit
Baghouse
exit
Stack
Constituent Manufacturer
O2 Beckman
O2 Rosemount
CO2 Horiba
NOX Thermo
Electron
O2 Beckman
CO Horiba
CO2 Horiba
TUHC Beckman
NOX Thermo
Electron
O2 Teledyne
CO Horiba
Model
755
755
PIR 2000
10 AR
755
VIA 500
PIR 2000
402
10 AR
326A
VIA 500
Principle
Paramagnetic
Paramagnetic
NDIR
Chemiluminescent
Paramagnetic
NDIR
NDIR
FID
Chemiluminescent
Fuel cell
NDIR
Range
0-10 percent
0-25 percent
0-100 percent
0-10 percent
0-25 percent
0-100 percent
0-20 percent
0-80 percent
0-75 ppm to
0-10,000 ppm in
multiples of 2
0-10 percent
0-25 percent
0-100 percent
0-50 ppm
0-500 ppm
0-20 percent
0^80 percent
0-10 ppm
0-100 ppm
0-1,000 ppm
0-75 ppm to
0-10,000 ppm in
multiples of 2
0-5 percent
0-10 percent
0-25 percent
0-50 ppm
0-500 ppm
3-6
-------
FILTER
HIGH
BAY
CONTROL
ROOM
PUMP
FILTER
CHILLED WATER
MPINGER
HEATED
FLTERS'
CONDENSATE
REMOVALE
r
r
]«__/Ot5frU_ SAMPLE
SAMPLE
PORT
r
-.STORE ROOM
PUMP
AIR COOLED
COIL
PORT
-H
CALIBRATION
GAS
VENT
H
-MX!-
VENT
HEATED
SAMPLE LINE
HEATED
TUHC
MONITOR
PERMA PURE
DRYER
CO CO2 NO.
-------
TABLE 3-2. ANALYSIS PROCEDURES
Sample
Test feed
material
Parameter
Proximate analysis
(moisture, volatile matter,
fixed carbon, ash)
Elemental analysis
C, H, 0, N, S
a
Heating value
Analysis method
ASTM D-5142
ASTM D-3176
ASTME-442
ASTM D-3286
Frequency
1 composite for
each test material
1 composite for
each test material
1 composite for
Test semivolatile POHCs
Test volatile organic
contaminants
Soxhlet extraction by Method 3540A, GC/MS
analysis by Method 8270A*
Purge and trap GC/FID of methanol extract by
Method 8015A*
each test material
I/test
I/test
Test feed TCLP
leachate
Feed packaging
material
Kiln ash
Kiln ash TCLP
leachate
PCDDs/PCDFs
Trace metalsb
TCLP extraction
Trace metals"
Proximate analysis
(moisture, volatile matter,
fixed carbon, ash)
Elemental analysis
C, H, 0, N, S
Cl
Heating value
Test semivolatile POHCs
Test volatile organic
contaminants
PCDDs/PCDFs
Trace metalsb
Test semivolatile POHCs
Test volatile organic
contaminants
PCDDs/PCDFs
Trace metalsb
TCLP extraction
Trace metals"
GC/MS by Method 8290"
Digestion by the multiple metals filter method0,
ICAP analysis by Method 6010A"
Method 1311*
Digestion by Method 3010A, ICAP analysis by
Method 6010A*
ASTM D-S142
ASTM D-3176
ASTME-442
ASTM D-3286
Soxhlet extraction by Method 3540A, GC/MS
analysis by Method 8270A*
Purge and trap GC/FID of methanol extract by
Method 8015A*
GC/MS by Method 8290*
Digestion by the multiple metals filter method6,
ICAP analysis by Method 6010A*
Soxhlet extraction by Method 3540A, GC/MS
analysis by Method 8270A*
Purge and trap GC/FID of methanol extract by
Method 8015A*
GC/MS by Method 8290*
Digestion by the multiple metals filter method0,
ICAP analysis by Method 6010A*
Method 1311"
Digestion by Method 3010A, ICAP analysis by
Method 6010A*
1 composite for
each test material
I/fluff test,
1 composite soil
I/fluff test,
1 composite soil
I/fluff test,
1 composite soil
1 composite
1 composite
1 composite
1 composite
1 composite
1 composite
1 composite
I/test
I/test
I/test
I/test
I/test
I/test
'Reference 3, SW-846.
bAs, Sb, Ba, Cd, Cr, Cu, Pb, Ni, Ag, and Zn.
Reference 2, 40 CFR 266, App. IX.
(continued)
3-8
-------
TABLE 3-2. (continued)
Sample Parameter Analysis method Frequency
Pre-test Test semivolatile Extraction by Method 3520A, GC/MS analysis by Method I/test
scrubber liquor POHCs 8270A*
Test volatile organic Purge and trap by Method 5030A, GC/FID by Method 8015A* I/test
contaminants
Trace metalsb Digestion by Method 3010A, ICAP analysis by Method 6010A* I/test
PCDDs/PCDFs GC/MS by Method 8290* 1 sample
before the
first test
Post-test Test semivolatile Extraction by Method 3520A, GC/MS analysis by I/test
scrubber liquor POHCs Method 8270A*
Test volatile organic Purge and trap by Method 5030A, GC/FID by Method 8015A* I/test
contaminants
PCDDs/PCDFs GC/MS by Method 8290* I/test
- Trace metalsb Digestion by Method 3010A, ICAP analysis by Method 6010A* I/test
TCLP extraction Method 1311* I/test
Scrubber liquor Trace metalsb Digestion by Method 3010A, ICAP analysis by Method 6010A* I/test
TCLPleachate
Baghouse ash Test semivolatile Soxhlet extraction by Method 3540A, GC/MS analysis by I/test
POHCs Method 8270A*
Test volatile organic Purge and trap GC/FID of methanol extract by I/test
contaminants Method 8015A*
PCDDs/PCDFs GC/MS by Method 8290* I/test
Trace metalsb Digestion by the multiple metals filter method0, ICAP analysis I/test
by Method 6010A"
TCLP extraction Method 1311* I/test
Baghouse ash
TCLP leachate
Baghouse exit
flue gas
Stack gas
Trace metalsb
Semivolatile TCL
constituents
Volatile TCL
constituents
PCDDs/PCDFs
Trace metalsb
Paniculate
HC1
Paniculate
HC1
Digestion by Method 3010A, ICAP analysis by Method 6010A*
Soxhlet extraction of Method 0010A samples by
Method 3540A, GC/MS analysis by Method 8270A*
Purge and trap of Method 0030 samples by Method 5040,
GC/MS analysis by Method 8240A
GC/MS of Method 23 samples by Method 23°
Digestion of multiple metals train samples by multiple metals
procedure6, ICAP analysis by Method 6010A*
Method 5"1
ICAP analysis of combined impinger solution by Method 9057°
Method 3d
1C analysis of combined impinger solution by Method 9057°
I/test
I/test
3 trap
pairs/test
I/test
I/test
I/test
I/test
I/test
J/test
"Reference 3, SW-846.
bAs, Sb, Ba, Cd, Cr, Cu, Pb, Ni, Ag, and Zn.
Reference 2, 40 CFR 266, App. IX.
Reference 4, 40 CFR 60, App. A.
3-9
-------
TABLE 3-3. TEST PROGRAM SAMPLE ANALYSIS SUMMARY
Sample matrix
Fluff Waste Feed
Test sample
Split sample
Matrix spike
Spike duplicate
Soil Feed
Test sample
Split sample
Matrix spike
Spike duplicate
SVOCs
4
16
1
1
2
8
1
1
Number of analyses
VOCs PCDDs/PCDFs
4 1
1
1
1
2 1
1
1
1
Trace
metals Chloride
4
16
1
1
1
4
1
1
Packaging Container Material
Cardboard + packaging tape +
HDPE bottle + bottle cap +
polyethylene liner + plastic tie
Kiln Ash
Test sample*
Split sample
Matrix spike
Spike duplicate
Pre-test Scrubber Liquor
Test sample
Post-test Scrubber Liquor
Test sample
Split sample
Matrix spike
Spike duplicate
Baghouse Ash
Test sample
Split sample
Matrix spike
Spike duplicate
7
1
1
1
7
1
1
1
6
1
1
1
7
1
1
1
7
1
1
1
6
1
7
1
6
22
1
1
7
1
1
1
7
1
1
1
*No kiln ash resulted from the blank burn test.
(continued)
3-10
-------
TABLE 3-3. (continued)
Sample matrix
Trace
SVOCs VOCs PCDDs/PCDFs metals Chloride
TCLP Leachate
Fluff feed
Soil feed
Kiln ash
Scrubber liquor
Baghouse ash
Method blank
Split sample
Matrix spike
Spike duplicate
Method 0010 Train
Test sample
Method blank
Matrix spike
Spike duplicate
Method 0030
Test sample trap paii*
Field blank
Trip blank
Matrix spike
Method 23 Train
Test sample
Method blank
Multiple Metals Train
21
7
1
9
4
1
6
7
7
2
2
2
2
Front half
Test sample
Method blank
Matrix spike
Spike duplicate
Back half
Test sample
Method blank
Matrix spike
Spike duplicate
Method 5 Train Impingers
Test sample
Matrix spike
Spike duplicate
7
/
1
i
i
1
1
4 A
14
1
1
81 S? 35 140
"Tour trap pairs sampled per test, three trap pairs analyzed; fourth trap pair for breakage contingency.
3-11
-------
TABLE 3-4. SAMPLE ANALYSIS ALIQUOT SCHEDULE FOR EACH TEST
Total quantity
of each sample Analyte/
Sample collected
Fluff waste feed 1 kg
Soil feed 1 kg
Packaging 50 g
container
material
Kiln ash 1 kg
'
Pre-test scrubber 4 L
liquor
Post-test scrubber 8 L
liquor
procedure
SVOCs
VOCs
PCDDs/PCDFs
Trace metals
TCLP extraction
SVOCs
VOCs
Trace metals
TCLP extraction
SVOCs
VOCs
PCDDs/PCDFs
Trace metals
SVOCs
VOCs
PCDDs/PCDFs
Trace metals
TCLP extraction
SVOCs
VOCs
PCDDs/PCDFs
Trace metals
SVOCs
VOCs
PCDDs/PCDFs
Trace metals
TCLP extraction
Aliquot size
10 g
4g
10 g
lg
100 g
10 g
<»g
lg
100 g
10 g
«g
10 g
lg
10 g
4g
10 g
lg
100 g
1L
80mL(two
40-mL
aliquots)
1L
100 mL
1L
80mL(two
40-mL
aliquots)
1L
100 mL
2L
Number of aliquots
5 replicates each test + 1 MS
1 each test + 1 duplicate + 1
1 total
5 replicates each test + 1 MS
1 each test
5 replicates each test + 1 MS
1 each test + 1 duplicate + 1
needed
+ 1MSD
MS + 1 MSD
+ 1MSD
+ 1MSD
MS + 1 MSD
5 replicates total + 1 MS + 1 MSD
1 total
1
1
1
1
1 each test + 1 split + 1 MS
1 each test + 1 split + 1 MS
1 each test + 1 split
5 replicates each test + 1 MS
1 each test
1 each test
1 each test
1 total
1 each test
+ 1MSD
+ 1MSD
+ 1MSD
1 each test + 1 split + 1 MS + 1 MSD
1 each test + 1 split + 1 MS + 1 MSD
1 each test + 1 split
1 each test + 1 split + 1 MS + 1 MSD
1 each test
(continued)
3-12
-------
TABLE 3-4. (continued)
Sample
Total quantity
of each sample
collected
Analyte/
procedure
Aliquot
size
Number of aliquots needed
Baghouse ash
As collected
SVOCs 10 g
VOCs 4 g
PCDDs/PCDFs 10 g
Trace metals 1 g
1 each test + 1 split + 1 MS + 1 MSD
1 each test + 1 split + 1 MS + 1 MSD
1 each test + 1 split
1 each test + 1 split + 1 MS + 1 MSD
TCLP extraction 100 g 1 each test
TCLP leachate
Method 0010 train
Method 0030 train
Method 23 train
2L
As collected
As collected
As collected
Trace metals
SVOCs
VOCs
PCDDs/PCDFs
100 mL
Total
Total
Total
25 test samples + 2 method blank +
2 split + 2 MS + 2 MSD
1 each test + 1 method blank + 1 MS
+ 1MSD
4* each test + 7 field blanks + 1 trip
blank + 9 MS
1 each test + 1 method blank
Multiple metals train
Front half
Back half
As collected Trace metals Total 1 each test + 1 method blank + 1 MS
+ 1 MSD
As collected Trace metals Total 1 each test + 1 method blank + 1 MS
+ 1MSD
Method S train impinger As collected Cl 100 mL 2 each test + 1 MS + 1 MSD
"Three of four analyzed; fourth represents breakage contingency.
Table 3-5 summarizes the containers used for sample aliquot storage until analysis,
preservation methods used, and analysis hold times required. Only new containers were used
for sample storage. They were purchased, precleaned to meet EPA standards, from a laboratory
supply vendor and are certified by the vendor as appropriate for use in storing samples for the
respective analyte class. No containers or preservation is shown in Table 3-5 for Method 0010
train samples. The procedure at the IRF is to transfer samples recovered from Method 0010
trains directly into the extraction apparatus immediately after a test and begin overnight
extractions the day of each test.
Filters and other sampling train components for Method 0010, Method 23, the multiple
metals method train, and the Method 5 trains were cleaned according to the procedures
3-13
-------
TABLE 3-5. SAMPLE CONTAINERS, PRESERVATION METHODS, AND HOLD TIMES
Sample
Solid samples (fluff
waste, soil, packaging
container material, kiln
ash, baghouse ash)
Aqueous liquid samples
(scrubber liquor, TCLP
leachates)
Method 0010 train
Method 0030 traps
Method 23 train filter
Filter
Rinses and impinger
solutions
Analyte
SVOCs
VOCs
PCDDs/PCDFs
Trace metals
SVOCs
VOCs
PCDDs/PCDFs
Trace metals
SVOCs
VOCs
PCDDs/PCDFs
Sample
container*
G.T
G, T, zero
headspace
G, T
GorP
G,T
G, T VGA vial
G, T .
GorP
None
Sealed glass
traps
Glass petri dish
G, T
Sample
preservation
method
Cool to 4°C
Cool to 4°C
Cool to 4°C
None
Cool to 4°C
Cool to 4°C
Cool to 4°C
HNO3 to pH <2
None
Cool to 4°C
Cool to 4°C
Cool to 4°C
Analysis hold time
Extraction: 14 days
Analysis'": 40 days
14 days
Extraction: 30 days
Analysis": 45 days
6 months
Extraction: 7 days
Analysis": 40 days
14 days
Extraction: 30 days
Analysis": 45 days
6 months
40 days
42 days
Extraction: 30 days
Analysis": 45 days
Multiple metals train
Filter
Rinses and impinger
solutions
Trace metals
Glass petri dish None
G or P None
6 months
Method 5 train
impinger solution
Chloride
GorP
None
28 days
*G = glass, P = polyethylene, T = Teflon-lined cap.
"After extraction.
3-14
-------
documented in the respective methods. Sorbent resin for use in Method 0010 and Method 0030
trains was cleaned prior to use according to the procedures in the respective methods.
Method 23 sorbent resin cartridges were cleaned and charged with clean sorbent, spiked with
method surrogates, by the analytical laboratory that performed the PCDD/PCDF analyses.
A single container was used to store each sample collected for each analysis. Aliquots
were taken from this container as needed. MS and MSD samples were prepared from aliquots
from this container as well. After preparation, however, MS and MSD samples were stored in
separate containers until analyzed.
Unused sample collected was stored in appropriate containers with appropriate
preservation until the expiration of method hold times. After method hold time expired, unused
samples were archived.
32 ANALYSIS METHODS
Table 3-2 summarizes the analytes determined in each test program sample, and the
analysis procedures used. As indicated in the table, the fluff feed samples for each fluff test, a
composite soil feed sample, the packaging container material, and the kiln ash, pre-test and
post-test scrubber liquor, and baghouse ash samples for each test analyzed for the site
contaminant trace metals. Trace metal analyses were by ICAP spectroscopy in accordance with
Method 6010A. Solid samples (feed material, packaging container material, kiln ash, and
baghouse ash) were digested using the HNO3/HF procedure specified for use with filter
particulate in the EPA multiple metals method (Reference 2). Liquid samples (pre-test and
post-test scrubber liquor) were digested using a minor variation of Method 3010A. This minor
variation consists of using concentrated HNO3 instead of 1:1 HC1 in the last step of Section 7.2
of Method 3010A. The 10 site contaminant metals measured in the test samples were antimony,
3-15
-------
arsenic, barium, cadmium, chromium, copper, lead, nickel, silver, and zinc. Omission of the HCI
in the last Method 3010A step allows analysis for silver.
Each fluff test's fluff feed, a composite soil feed sample, and each test's kfln ash,
baghouse ash, and post-test scrubber liquor samples were subjected to TCLP extraction by
Method 1311. The TCLP leachates were analyzed for the 10 site contaminant trace metals by
Method 6010A. The minor variation of Method 3010A, noted above, was used for leachate
digestion.
In addition, each fluff test's fluff feed, each soil test's soil feed, the packaging container
material, and the kiln ash, baghouse ash, and pre-test and post-test scrubber liquor samples for
each test were analyzed for the test semivolatile POHCs (BEHP, DNOP, and naphthalene).
Semivolatile POHC analyses were by gas chromatography/mass spectrometry (GC/MS) in
accordance with Method 8270A. Solid samples (feed, packaging container material, baghouse
ash, and kiln ash) were Soxhlet-extracted by Method 3540A. Pre-test and post-test scrubber
liquor samples were extracted via continuous liquid-liquid extraction by Method 3520A.
One composite fluff feed sample, a composite soil feed sample, the packaging container
material, the pre-test scrubber liquor sample taken before the first test program test, and the kiln
ash, post-test scrubber liquor, and baghouse ash samples for each test were also analyzed for
PCDDs/PCDFs by the high-resolution GC/MS method, Method 8290. The single composite
fluff feed sample was prepared by combining aliquots of the four test feed samples collected.
Each test's fluff feed or soil feed, the packaging container material, and each test's kiln
ash, baghouse ash, and pre-test and post-test scrubber liquor samples were also analyzed for the
test volatile organic contaminants by GC/FTD in accordance with Method 8015A. Sample
introduction was by Method 5030A.
3-16
-------
The Method 0010 samples for each test were analyzed for the semivolatile organic TCL
constituents listed in Table 3-6. The target analytes were the semivolatile test POHCs, BEHP,
DNOP, and naphthalene. However, the other TCL constituents were also quantitated. Sample
preparation was performed according to Method 0010, with final GC/MS analysis by
Method 8270A. The Method 23 samples for each test were analyzed for PCDDs/PCDFs by the
method.
TABLE 3-6. SEMIVOLATILE ORGANIC TCL CONSTITUENTS
Acenaphthene
Acenaphthylene
Anthracene
Benz(a)anthracene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Benzo(ghi)perylene
Benzyl butyl phthalate
Bis(2-chloroethyl) ether
Bis(2-chloroethoxy) methane
Bis(2-chloroisopropyl) ether
Bis(2-ethylhexyl) phthalate
4-Bromophenyl phenyl ether
2-Chloronaphthalene
4-Chlorophenyl phenyl ether
Chrysene
Dibenzo(a,h)anthracene
Di-n-butyl phthalate
1,2-Dichlorobenzene
1,3-Dichlorobenzene
1,4-Dichlorobenzene
3,3'-Dichlorobenzidine
Diethyl phthalate
Dimethyl phthalate
2,4-Dinitrotoluene
2,6-Dinitrotoluene
Di-n-ocryl phthalate
Fluoranthene
Fluorene
Hexachlorobenzene
Hexachlorobutadiene
Hexachloroethane
Indeno(l,2,3-cd)pyrene
Isophorone
Naphthalene
Nitrobenzene
N-Nitrosodi-n-propylamine
Phenanthrene
Pyrene
1,2,4-Trichlorobenzene
4-Chloro-3-methylphenol
2-Chlorophenol
2,4-Dichlorophenol
2,4-Dimethylphenol
2,4-Dinitrophenol
2-Methyl-4,6-dinitrophenol
2-Nitrophenol
4-Nitrophenol
Pentachlorophenol
Phenol
2,4,6-Trichlprophenol
3-17
-------
As noted in Section 3.1, four Method 0030 trap pair samples were collected for each
test. Three trap pair samples for each test were analyzed for the test volatile organic TCL
constituents listed in Table 3-7 by purge and trap GC/MS via Methods 5040 and 8240A. The
fourth trap pair was collected for breakage contingency, so that the probability that three trap
pair analyses could be done for each test was increased, given the inevitability of trap breakage.
The target analytes were the volatile site material organic contaminants, tetrachloroethene,
trichloroethene, and 1,1,2-trichloroethane. However, the other TCL constituents were .also
quantitated.
Multiple metals train samples were analyzed for the 10 site contaminant trace metals.
Sample preparation was performed according to the method, with final ICAP analysis by
Method 6010A. Flue gas HC1 levels were determined by analyzing the combined Method 5 train
impinger solutions for chloride via 1C according to Method 9057.
One composite fluff feed sample, the composite soil feed sample, and the packaging
container material sample were, also subjected to proximate, elemental, and heating value
analyses by the ASTM procedures noted in Table 3-2.
TABLE 3-7. VOLATILE ORGANIC TCL CONSTITUENTS
Acetone trans-l,2-Dichlorothene
Benzene 1,2-Dichloropropane
Bromodichloromethane cis-l,3-Dichloropropene
Carbon disulfide trans-l,3-Dichloropropene
Carbon tetrachloride Methylene chloride
Chlorobenzene Tetrachloroethene
Chlorodibromomethane Toluene
Chloroform 1,1,1-Trichloroethane
1,1-Dichloroethane 1,1,2-Trichloroethane
1,2-Dichloroethane Trichloroethene
1,1-Dichloroethene Trichlorofluoromethane
3-18
-------
Proximate and elemental analyses were performed by Galbraith Laboratories in
Knoxville, Tennessee. SVOC (Method 8270A), VOC (Method 8015A), HC1 (Method 9057), and
TCLP (Method 1311) procedures were performed in the IRF analytical laboratories. Trace
metal analyses (Method 6010A) were performed by the American Interplex Laboratories in
Little Rock, Arkansas. Method 0030 sample and PCDD/PCDF (Methods 8290 and 23) analyses
were performed by Triangle Laboratories in Research Triangle Park, North Carolina.
3-19
-------
SECTION 4
TEST RESULTS
The results of the test program are discussed in this section. Test results are grouped
by analyte class. Thus, Section 4.1 presents the fluff waste and soil feed proximate and elemental
analysis results. Section 4.2 discusses the SVOC measurements. Section 4.3 discusses the VOC
measurements. Section 4.4 discusses the PCDD/PCDF measurements. Each of the sections, 4.2,
4.3, and 4.4, includes discussion on the effectiveness of incineration in removing the contaminants
of interest in the fluff waste and contaminated soil. Where appropriate, contaminant destruction
removal efficiencies (DREs) are presented and discussed. The concentrations of contaminants
of interest in the RKS discharge streams, kiln ash, baghouse ash, and scrubber liquor, are also
discussed. Section 4.5 discusses the trace metals measurements. Section 4.6 discusses the results
of the flue gas paniculate and HC1 measurements, as well as the flue gas paniculate size
distribution results. For the reader who is interested in studying the analytical results in more
detail, the analytical laboratory reports are given in Appendix C of this report.
4.1 PROXIMATE AND ULTIMATE ANALYSIS RESULTS
The proximate and elemental analysis results for the fluff waste, soil, and packaging
container material samples analyzed are presented in Table 4-1. As shown in the table, the fluff
waste was distinctly organic in nature as evidenced by the high level of volatile matter at
39.1 percent and its higher heating value of 12.4 MJ/kg (5,330 Btu/lb). The fluff was also quite
moist, with 46.8 percent moisture. The high moisture content was consistent with the fact that
4-1
-------
TABLE 4-1. PROXIMATE AND ELEMENTAL ANALYSIS RESULTS FOR
COMPOSITE FLUFF AND SOIL FEED SAMPLES
Proximate Analysis (as received)
Moisture, %
Ash, %
Fixed carbon, %
Volatile matter, %
Higher heating value, MJ/kg
(Btu/lb)
Elemental Analysis, % (dry
basis)
C
H
O
N
S
Cl
Ash
Fluff waste
46.8
5.2
8.9
39.1
12.4
(5,330)
44.2
6.2
7.4
<0.5
0.2
32.2
9.8
Contaminated
soil
23.0
64.4
2.6
10.0
0.58
(250)
7.3
1.1
5.8
<0.5
<0.04
2.3
83.6
Packaging
container
material
4.8
1.4
13.3
80.5
__a
46.4
7.0
45.0
<0.5
0.2
<0.5
1.4
. a - Not measured.
the fluff had been accumulated and stored in large piles outdoors, thereby being exposed to
precipitation. The fluff waste contained 32.2 percent chlorine (dry basis), a level suggesting the
presence of chlorinated plastics (e.g., polyvinyl chloride) and possibly other chloro-organic
solvents, both of which were present or used at the site.
The character of the contaminated soil was distinctly different from the fluff, although
a small amount of fluff-like material was found to have commingled into the soiL The heating
value of the soil was low, as expected at 0.58 MJ/kg (250 Btu/lb). Its moisture content, at
4-2
-------
23 percent, and ash content, at 64.4 percent are typical of soils. The soil chlorine content, at
2.3 percent (dry), could have been due to the presence of a small amount of fluff or other
chlorine containing organic contaminants.
Table 4-2 summarizes the cumulative weights of the fluff waste and contaminated soil
«
fed for each test and the total amount of corresponding kiln ash collected. As indicated in (the
table, for Tests 1 and 2 (average kiln exit gas temperature at 875° to 883°C [1,608° and 1,622°F],
respectively), the collected ash weights were equal to about 5 percent of the amount of fluff fed.
The collected ash amounts accounted for 98 to 101 percent of the theoretical ash amount that
could be expected. For Tests 5 and 6, during which the average kiln exit temperatures were at
762 and 767°C (1,403° and 1,412°F), respectively, the collected ash amounts were equal to 5.7
and 6.7 percent of the amount of fluff fed. These amounts of collected ash were greater than
the theoretical ash quantity in the fluff fed. The amounts of. ash collected were 128 and
109 percent of the theoretical ash amount. The greater-than-100-percent ash collected for these
TABLE 4-2. WEIGHTS OF TEST MATERIAL FED AND KILN ASH COLLECTED
Total fed
Test
Fluff Waste Tests
1
2
5
6
Soil Feed Tests
3
4
Date
11/9/93
11/16/93
11/18/93
11/23/93
12/1/93
12/2/93
kg
303
304
307
305
288
290
Ob)
(666)
(669)
(675)
(671)
(634)
(638)
Kiln
Weight
kg
15
16
20
17
150
145
Ob)
(34)
(35)
(45)
(38)
(329)
(320)
ash collected
Fraction Fraction of
of feed expected ash
5.1
5.2
6.7
5.7
52
50
98
101
128
109
81
78
4-3
-------
tests would be consistent with incomplete fluff oxidation for these lower kiln exit gas temperature
tests.
For the soil tests (Tests 3 and 4), the kiln ash weights were about 50 percent of the fed
soil weights, which corresponds to about 80 percent of the theoretical ash amounts. Evidently,
about 20 percent of the theoretical ash in the soil tests was entrained in the kiln exit combustion
gas and carried out of the kiln.
4.2 SVOC ANALYSIS RESULTS
Table 4-3 summarizes the measured concentrations of the target SVOC analytes in test
program samples collected. For the entries in the table noted as less than values, the value
represents the MDL of the analysis procedure. Laboratory analysis reports are given in
Appendix C-3. For each test performed, Table 4-3 also indicates the average kiln exit gas
temperature measured over the flue gas sampling period corresponding to each test.
The data in Table 4-3 show that the BEHP concentrations in the actual fluff waste fed
for each fluff waste test, at 48,300 to 53,300 mg/kg, were about half the level measured in the
pretest characterization sample as reported in Table 2-3, as well as being below the lowest
concentration reported in the ROD. Similarly, the DNOP levels in actual test fluff waste, at
1,850 to 2,870 mg/kg, were also substantially lower than the 17,800 mg/kg level measured in the
pretest characterization sample, and were at the low end of the range of concentrations reported
in the ROD. Nevertheless, contamination levels of these two constituents in the test fluff waste
were still significant. The 20,200 mg/kg naphthalene concentration noted in incinerator feed
samples in the table represents the quantity of naphthalene spike added to feed containers. No
fluff waste or soil sample contained naphthalene at an MDL of 25 mg/kg before spiking.
The data in Table 4-3 show that the contaminated soil tested contained 9,440 to
9,810 mg/kg of BEHP and 550 to 580 mg/kg DNOP. These levels are substantially greater than
4-4
-------
TABLE 4-3. SEMIVOLATILE ORGANIC CONTAMINANT ANALYSIS RESULTS
Concentration
Sample
Test 0 (10/27/93), kiln temperature:
871°C (1,599°F)
Packaging container material, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /ig/dscm
Fluff Waste Tests
Test 1 (11/9/93), kiln temperature:
883 °C (1,622°F)
Fluff feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, jig/dscm
Test 2 (11/16/93), kiln temperature:
876°C (1,608°F)
Fluff feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /zg/dscm
Test 5 (11/18/93), kiln temperature:
762°C (1,403 °F)
Fluff feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /*g/dscm
Test 6 (11/23/93), kiln temperature:
767°C (1,412°F)
Fluff feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /zg/dscm
BEHP
<1.3
< 0.013
6.6
8.4
48,800
<1.3
< 0.013
14.3
7.0
53,300
<1.3
<0.013
4.5
9.9
48,300
<1.3
< 0.013
21.1
9.8
49,000
<13
< 0.013
18.7
6.2
DNOP
<0.4
< 0.004
4.1
<0.9
1,850
<0.4
< 0.004
9.9
<1.2
2,610
<0.4
< 0.004
2.2
<1.3
2,870
<0.4
< 0.004
13.4
<1.1
2,810
<0.4
<0.004
12.1
<1.2
Naphthalene
<0.3
< 0.003
<0.3
<0.8
20,200a
<0.3
< 0.003
<0.3
<0.9
20,200a
<0.3
< 0.003
<0.3
<1.1
20,200a
<0.2
< 0.003
<0.3
<0.9
20,200a
<0.3
<0.003
<0.3
<1.0
aSpiked concentration.
(continued)
4-5
-------
TABLE 4-3. (continued)
Concentration
Sample
Soil Feed Tests
Test 3 (12/1/93), kiln temperature:
876°C (1,609°F)
Soil feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /zg/dscm
Test 4 (12/2/93), kiln temperature:
874°C (1,606°F)
Soil feed, mg/kg
Kiln ash, mg/kg ^
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /tg/dscm
BEHP
9,810
< 0.013
23.5
7.8
9,440
< 0.013
14.2
7.0
DNOP
580
<0.4
< 0.004
17.0
547
<0.4
< 0.004
9.7
Naphthalene
20,200*
<03
< 0.003
<03
20,200a
<0.003
<03
Spiked concentration.
those measured in the pretest soil characterization samples analyzed, although they fall within
the concentration ranges reported in the ROD for these contaminants. Again, the naphthalene
concentrations in test soil feed samples correspond to spiked amounts.
The data in Table 4-3 also show that the native and spiked SVOC contaminants were
essentially completely removed from the fluff waste by incineration at both kiln temperatures
tested, as evidenced by their absence in the kiln ash discharge for all fluff waste tests at method
detection limits (MDLs) of 0.3 to 1.3 mg/kg. Similarly these contaminants were removed from
the contaminated soil for both soil tests at the single kiln temperature tested for this matrix. No
kiln ash concentration data are given for the blank burn test, Test 0, in Table 4-3 because no kiln
ash was discharged for this test.
4-6
-------
None of the three SVOC contaminants was found in the post-test scrubber liquor for
any test at MDLs of 0.003 to 0.013 mg/L.
Naphthalene was absent from the baghouse ash for all tests at an MDL of 0.3 mg/kg.
However, low levels of both BEHP (6.6 to 23.5 mg/kg) and DNOP (2.2 to 17.0 mg/kg) were
found in the baghouse ash for all tests, including the blank burn. No explanation as to why these
site contaminants are found at these levels in the baghouse ash is offered, other than the fact
that phthalates are commonly encountered laboratory contaminants. Neither naphthalene nor
DNOP was present in the baghouse exit flue gas for any test, at MDLs of about 1 /tg/dscm.
BEHP was found in the baghouse exit flue gas for all tests, including the blank burn, at levels
ranging from 6.2 to 9.8 /ig/dscm.
Feed SVOC contaminant concentration, feedrate, baghouse exit flue gas SVOC
contaminant concentration, and flue gas flowrate data can be combined to calculate SVOC
contaminants DREs for each of the tests. Calculated DREs are summarized in Table 4-4. As
shown in the table, the measured levels of BEHP in the baghouse exit flue gas corresponded to
BEHP DREs ranging from 99.99932 to 99.99962 percent for the fluff waste tests and 99.9974 to
99.9980 percent for the soil feed tests. Kiln temperature had no apparent affect on BEHP DRE
from fluff waste. Neither the spiked naphthalene nor the native DNOP contaminants were
detected in the baghouse exit flue gas for any test. The DREs corresponding to baghouse exit
flue gas MDLs, and noted with the ">" sign in Table 4-4, were 99.99982 to 99.99987 percent for
naphthalene for all tests, 99.9982 to 99.9987 percent for DNOP in the fluff waste tests, and
99.9933 to 99.9940 percent for DNOP in the soil feed tests. All DREs demonstrated were
greater than the 99.99 percent level required by the current hazardous waste incinerator
performance standard.
4-7
-------
TABLE 4-4. SVOC POHC DREs
Parameter
BEHP
DNOP Naphthalene
Fluff Waste Tests
Test 1 (11/9/93), kiln temperature: 883°C (1,622°F)
Feed concentration, mg/kg
Feedrate, kg/hr
Baghouse exit flue gas:
Concentration, /tg/dscm
Emission rate, mg/hr
DRE, %
Test 2 (11/16/93), kfln temperature: 876°C (1,608°F)
Feed concentration, mg/kg
Feedrate, kg/hr
Baghouse exit flue gas:
Concentration, /tg/dscm
Emission rate, mg/hr
DRE, %
Test 5 (11/18/93), kiln temperature: 762°C (1,403°F)
Feed concentration, mg/kg
Feedrate, kg/hr
Baghouse exit flue gas:
Concentration, /tg/dscm
Emission rate, mg/hr
DRE, %
Test 6 (11/23/93), kiln temperature: 767°C (1,412'F)
Feed concentration, mg/kg
Feedrate, kg/hr
Baghouse exit flue gas
Concentration, /zg/dscm
Emission rate, mg/hr
DRE, %
Soil Feed Tests
> Test 3 (12/1/93), kiln temperature: 876eC (l,6d9°F)
Feed concentration, mg/kg
Feedrate, kg/hr
Baghouse exit flue gas:
Concentration, pg/dscm
Emission rate, mg/hr
DRE, %
Test 4 (12/2/93), Icfln temperature: 874°C (1,606°F)
Feed concentration, mg/kg
Feedrate, kg/hr
Baghouse exit flue gas:
Concentration, /jg/dscm
Emission rate, mg/hr
DRE, %
48,800
2.93
7.0
11.9
99.99959
53300
3.15
9.9
19.4
1,850
0.11
20^00
48300
2.94
9.8
20.1
99.99932
49,000
2.98
6.2
113
99.99962
9,810
0.58
7.8
15.0
99.9974
9,440
0.56
7.0
113
99.9980
<2.0
>99.9982
2,610
0.15
<13
<2.5
20,200
1.19
99.99939 > 99.9984
2,870
0.18
<23
> 99.9987
2,810
0.17
> 9959982
20,200
9939985
20,200
<2.2
> 99.9987
580
0.034
99.9933
547
0.032
> 99^9985
20,200
1.19
>99J9984
20^00
1.19
>99.9940
> 99.99986
4-8
-------
As noted in Section 3.2, the flue gas Method 0010 train samples were analyzed for the
full list of SVOC TCL compounds given in Table 3-6. None were found at compound-specific
MDLs ranging from 0.4 to 8 /zg/dscm, with the exception of dimethylphthalate, which was found
in the flue gas for all tests (including the blank test, Test 0) at concentrations ranging from 1.1 to
2.1 /zg/dscm.
Also recall from the discussion in Section 3 that the five replicates of each fluff waste
and soil feed samples collected were to be analyzed for the SVOC POHCs in the test program.
This was done for the soil feed samples collected. However, only BEHP was quantitated in all
fluff waste replicate samples. In order to accurately quantitate the DNOP levels measured in
fluff waste samples, the analysis of undiluted sample extracts was required. However,, the
concentration of BEHP in undiluted extracts was so high that the instrument cleanup times
required after an undiluted extract analysis were quite lengthy. For this reason, it was decided
to quantitate DNOP and naphthalene in a composite undiluted extract, formed by combining
aliquots of each replicate fluff waste SVOC extract, to give a test composite analysis result for
these two analytes. Each replicate sample extract was then diluted and analyzed for BEHP. The
DNOP concentrations for fluff waste samples given in Table 4-3 represent these test-specific
composite extract analysis results. Naphthalene was not detected in any fluff waste composite
extract sample at an MDL of 130 mg/kg.
Table 4-5 summarizes the BEHP replicate sample analysis results for the fluff waste
samples. The average concentration noted for each test is the fluff waste concentration reported
in Table 4-3. The data in the table show that the percent relative standard deviation (% RSD)
of the BEHP concentration measured in the five replicate fluff waste samples analyzed for each
test ranged from 5.8 to 24.6. All are well within the precision data quality objective (DQO) for
this measurement of 50% RSD. The four test average fluff waste BEHP concentration, from
4-9
-------
TABLE 4-5. BEHP CONCENTRATIONS IN REPLICATE FLUFF WASTE SAMPLES
BEHP concentration, mg/kg
Test
1 (11/9/93)
2 (11/16/93)
5 (11/18/93)
6 (11/23/93)
4 test total (20 samples)
f"
o
Sample
27,800
55,400
51,300
54,000
Replicate 1
52,800
51,200
53,300
43,300
Replicate 2
57,200
49,000
43,200
51,900
Replicate 3
50,700
56,100
47,300
54,000
Replicate 4
55,600
54,900
46,200
42,000
Average
concentration,
mg/kg
48,800
53,300
48,300
49,000
49,900
%RSD
24.6
5.8
8.4
12.1
13.8
-------
the analysis of 20 separate fluff samples, was 49,900 mg/kg, with the 20-sample % RSD at
13.8 percent.
Table 4-6 summarizes the results of the replicate soil feed SVOC analyses. Again, the
average concentrations of BEHP and DNOP from the five samples analyzed for each test are
those given in Table 4-3. As shown in Table 4-6, naphthalene was not detected in any soil feed
sample at an MDL of 25 mg/kg. The data in Table 4-6 show that the % RSDs for the individual
test replicate soil feed analyses were 32.8 and 27.9 percent for BEHP and 48.7 and 30.2 percent
for DNOP. The two test average SVOC contaminant concentrations representing 10 separate
TABLE 4-6. SVOC CONTAMINANT CONCENTRATIONS IN REPLICATE
SOIL SAMPLES
Concentration, mg/kg
Soil sample
Test 3
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
Average
%RSD
Test 4
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
Average
% RSD
2 test total (10 samples)
Average
%RSD
BEHP
10,700
14,900
6,450
8,530
8,470
9,810
32.8
11,000
8,270 .
9,450
5,780
12,700
9,440
27.9
9,630
28.9
DNOP
508
614
296
440
1,040
580
48.7
728
598
417
335
655
547
30.2
563
38.8
Naphthalene
<25
<25
<25
<25
<25
<25
<25
<25
<25
<25
<25
<25
<25
4-11
-------
analyses were 9,630 mg/kg for BEHP with 28.9 % RSD, and 563 mg/kg for DNOP with
38.8% RSD. All % RSD variances achieved were within the precision DQO for this
measurement of 50% RSD.
43 VOC ANALYSIS RESULTS
Table 4-7 summarizes the measured concentrations of the target VOC analytes in test
program samples collected. As for the SVOC analysis data reported in Table 4-3, entries in
Table 4-7 noted as less than values were not detected at the MDLs noted with the "<" sign.
Complete analytical laboratory reports on the VOC analyses are given in Appendices CM
and C-2.
As shown in Table 4-7, no fluff waste sample contained 1,1,2-trichloroethane at an MDL
of 1 mg/kg. This contaminant was absent from one test soil sample, but found at 28 mg/kg in
the other test soil. Trichloroethene was not found in three of four fluff feeds at an MDL of
1 mg/kg. It was present in the fourth fluff feed at 2.4 mg/kg, and in the soil test feeds at 2.7 to
3.9 mg/kg. Tetrachloroethene was not detected in two tests' fluff feed (before spiking) at an
MDL of 4 mg/kg, though it was present at 4.9 and 17 mg/kg in the other two tests' fluff feed.
*'
These levels are substantially lower than the 146 mg/kg found in the pretest fluff feed
characterization sample indicated in Table 2-3, although they are comparable to levels reported
in the ROD, indicated in Table 2-2. The contaminated soil tested contained 50 to 93 mg/kg of
native (before spiking) tetrachloroethene, in the range of the levels measured in pretest soil
characterization samples, as well as within the range of concentrations reported in the ROD.
The addition of the tetrachloroethene spike to all test feed samples raised spiked fluff feed
concentrations to 3,100 mg/kg and spiked soil feed concentrations to the 3,200 to 3,300 mg/kg
range, as indicated in Table 4-7.
4-12
-------
TABLE 4-7. VOLATILE ORGANIC CONTAMINANT ANALYSIS RESULTS
Sample
Test 0 (10/27/93), kiln temperature: 870°C (1,599°F)
Packaging container material, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, fig/dscm
Fluff Waste Tests
Test 1 (11/9/94), kiln temperature: 883°C (1,622°F)
Fluff feed, mg/kg, native
Fluff feed, mg/kg, spiked
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /tg/dscm
Test 2 (11/16/93), kiln temperature: 876°C (1,608°F)
Fluff feed, mg/kg, native
Fluff feed, mg/kg, spiked
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /ig/dscm
Test 5 (11/18/93), kiln temperature: 762°C (1,403°F)
Fluff feed, mg/kg, native
Fluff feed, mg/kg, spiked
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /tg/dscm
Test 6 (11/23/93), kiln temperature: 767°C (1,412°F)
Fluff feed, mg/kg, native
Fluff feed, mg/kg, spiked
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /tg/dscm .
. Tetrachloro-
ethene
<4
< 0.015
<4
0.66
4.9
3,100
<4
< 0.015
<4
0.27
<4
3,100
<4
<0.015
<4
0.71
<4
3,100
<4
<0.015
<4
0.68
17
3,100
5.6
< 0.015
<4
0.61
Concentration
1,1,2-Trichloro-
ethane
<0.004
<0.09
<0.004
<0.14
<0.004
<0.09
<0.004
<0.09
<0.004
0.23
Trichloiro-
ethene
<0.004
0.15
2.4
<0.004
0.16
< 0.004
0.14
<0.004
0.23
< 0.004
0.09
(continued)
4-13
-------
TABLE 4-7. (continued)
Sample
Soil Feed Tests
Test 3 (12/1/93), kiln temperature: 876°C (1,609°F)
Soil feed, mg/kg, native
Soil feed, mg/kg, spiked
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, pg/dscm
Test 4 (12/2/93), kiln temperature: 874°C (1,606°F)
Soil feed, mg/kg, native
Soil feed, mg/kg, spiked
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /xg/dscm
Tetrachloro-
ethene
50
3,200
<4
<0.015
<4
1.57
93
3,300
<4
<0.015
<4
0.14
Concentration
1,1,2-Trichloro-
ethane
<1
<1
<0.004
<1
1.27
2.8
<1
<0.004
<1
<0.05
Trichloro-
ethene
2.7
<1
< 0.004
<1
0.73
3.9
<1
<0.004.
<1
0.17
As was the case for the SVOC contaminants, incineration treatment of the fluff waste
at both temperatures tested and of the contaminated soil at the one temperature tested was
essentially completely effective in decontaminating the feed materials of their native and spiked
VOC contaminants. The kiln ash discharge for all tests contained no detectable VOC
contaminants at MDLs ranging from 1 to 4 mg/kg with the single exception of a 5.6 mg/kg
concentration of tetrachloroethene in the kiln ash from one low temperature fluff waste test.
This detected level is just above the MDL of 4 mg/kg. In addition, neither the post-test scrubber
liquor nor the baghouse ash from any test contained detectable VOC contaminants at MDLs, of
0.004 to 0.15 mg/L in scrubber liquor and 1 to 4 mg/kg in baghouse ash. Pretest scrubber liquor
samples similarly contained no detectable VOC contaminants at the same MDLs.
The baghouse exit flue gas for all tests, including the blank burn test, contained low
levels of both trichloroethene, at 0.09 to 0.73 jig/dscm, and tetrachloroethene, at 0.14 to
4-14
-------
1.57 /ig/dscm. No 1,1,2-trichloroethane was found in the baghouse exit flue gas at MDLs of 0.05
to 0.14 ng/dscm for the blank burn test, either fluff test at the higher incinerator temperature,
one of the two fluff tests at the lower incineration temperature, and one of the two soil feed
tests. This contaminant was found in the baghouse exit flue gas from the two tests detected at
0.23 to 1.27 /xg/dscm. The baghouse exit flue gas concentration data noted represent averages
for the three Method 0030 trap pairs analyzed for each test. >
Feed contaminant concentration, feedrate, baghouse exit flue gas contaminant
concentration, and flue gas flowrate data can be combined to calculate spike tetrachloroethene
DREs for each of the tests. Calculated DREs are summarized in Table 4-8. As shown in the
table, the measured baghouse exit flue gas tetrachloroethene concentrations corresponded to
tetrachloroethene DREs of 99.9984 to 99.99988 percent over all tests. Comparable
tetrachloroethene DREs were measured for both fluff and soil, and for fluff treated at both
incineration temperatures. All measured DREs were greater than the 99.99 percent level
required by the current hazardous waste incinerator performance standard.
As noted in Section 3, the Method 0030 train samples taken at the baghouse exit were
also analyzed for the extended list of VOCs given in Table 3-7. The results of these analyses are
summarized in Table 4-9 for those VOCs not given in Table 4-7. Concentrations in Table 4-9
noted as less than values were either not detected at the MDL of the procedure used to measure
flue gas VOC concentration, or had a measured concentration not significantly different from
the method blank concentration. In these latter cases, the method blank concentration is noted
with the" <" sign.
The data in Table 4-9 show that acetone, bromodichloromethane, carbon tetrachloride,
and chloroform were found in the baghouse exit flue gas for all tests, including the blank test
(Test 0). Flue gas acetone concentrations were the highest for the blank test and the two fluff
4-15
-------
TABLE 4-8. TETRACHLOROETHENE DREs
Parameter
Tetrachloroethene
Fluff Waste Tests
Test 1 (11/9/93), kiln temperature: 883 °C (lj622°F)
Feed concentration, mg/kg 3,100
Feedrate, kg/hr 0.19
Baghouse exit flue gas:
Concentration, pg/dscm
Emission rate, mg/hr
DRE,'%
Test 2 (11/16/93), kiln temperature: 876°C (1,608°F)
Feed concentration, mg/kg
Feedrate, kg/hr
Baghouse exit flue gas:
Concentration, pg/dscm
Emission rate, mg/hr
DRE, %
Test 5 (11/18/93), kiln temperature: 762°C (1,403°F)
Feed concentration, mg/kg
Feedrate, kg/hr
Baghouse exit flue gas:
Concentration, jjg/dscm
Emission rate, mg/hr
DRE, %
Test 6 (11/23/93), kiln temperature: 767°C (1,412°F)
Feed concentration, mg/kg
Feedrate, kg/hr
Baghouse exit flue gas
Concentration, /ig/dscm
Emission rate, mg/hr
DRE, %
Soil Feed Tests
Test 3 (12/1/93), kiln temperature: 876°C (l,609eF)
Feed concentration, mg/kg
Feedrate, kg/hr
Baghouse exit flue gas:
Concentration, fig/dscm
Emission rate, mg/hr
DRE, %
Test 4 (12/2/93), kiln temperature: 874eC (l,606eF)
Feed concentration, mg/kg
Feedrate, kg/hr
Baghouse exit flue gas:
Concentration, ;tg/dscm
Emission rate, mg/hr
DRE, %
0.27
0.46
99.99975
3,100
0.18
0.71
1.4
99.99924
3,100
0.19
0.68
1.4
99.99926
3,100
0.19
0.61
1.1
99.99941
3,200
0.19
1.57
3.0
99.9984
3,300
0.19
0.14
0.23
99.99988
4-16
-------
TABLE 4-9. FLUE GAS VOC CONCENTRATIONS
Baghouse exit flue gas concentration, (ig/dscm
Compound
Acetone
Benzene
Bromodichloromethane
Carbon disulfide
Carbon tetrachloride
Chlorobenzene
Chloroform
Dibromochloromethane
1, 1-Dichloroethene
c- 1,3-Dichlof opropene
Methylene chloride
Toluene
1,1,1-Trichloroethane
Trichlorofluoromethane
Blank test
TestO
10/27/93
130
63
0.48
<0.5
0.25
<0.19
1.1
<0.09
<0.09
<0.05
<2.5
39
<0.09
<1,0
Fluff waste tests
Testl
11/9/93
420
32
0.17
<18
0.83
<0.05
3.6
1.3
<0.09
<0.05
18
11
<0.09
<2.3
Test 2
11/6/93
460
300
0.15
<73
0.44
1-1
2.4
1.3
<0.09
<0.05
97
210
0.39
<2.4
Tests
11/18/93
23
8.3
1.2
<17
0.19
<0.04
2.3
0.94
<0.09
<0.04
15
<2.0
0.16
<2.6
Test 6
11/23/93
2.5
<6.4
1.9
<64
0.41
<0.05
3.8
1.2
<0.09
0.21
34
<2.1
0.39
<0.8
Soil
Tests
12/1/93
1.4
14
4.4
<23
1.1
0.60
12
1.9
<0.09
<0.05
100
9.2
6.1
<1.5
tests
Test 4
12/2/93
1.2
<5.2
1.6
<22
0.36
<0.05
4.2
0.74
<0.10
<0.05
72
<2.1
<0.10
<0.39
-------
waste tests at the higher incineration temperature tested; levels for the fluff waste tests at the
lower incineration temperature and for the soils tests were substantially lower. No explanation
for this observation is offered. Flue gas carbon tetrachloride concentrations were comparable
from test to test, including the blank test, and ranged from a few to several tenths of a /zg/dscm.
Hue gas chloroform concentrations were also comparable from test to test, but were higher, in
the 1 to 12 ng/dscm range. Methylene chloride was measured in the baghouse exit flue gas for
all tests except the blank test; concentratiqns ranged from 18 to 100 /ig/dscm.
The presence of bromodichloromethane, seen in the flue gas for all tests, and
dibromochloromethane, seen in the flue gas for all tests except the blank test, arises from the
trihalomethane (THM) compounds present in the recirculating scrubber liquor. The plant water
used for scrubber makeup is local well water subjected to a water treatment process that includes
disinfection. The disinfection process leaves low levels of THM compounds in the water. The
observation that dibromochloromethane was not detected in the Test 0 flue gas, but was at
concentrations substantially above the MDL for the fluff waste and soil tests suggests that EtCl
or organochlorine compounds, such as methylene chloride, need to be present in the flue gas
being scrubbed in order to form dibromochloromethane.
4.4 PCDD/PCDF ANALYSIS RESULTS
As noted in Section 3, incinerator feed, kiln ash, post-test scrubber liquor, and baghouise
ash samples for all tests were analyzed for PCDDs and PCDFs. In addition, the baghouse exit
flue gas was sampled, and collected samples correspondingly analyzed. Analyses were performed
for the total concentration of each homologue grouping of total tetra-, penta-, hexa-, hepta-, and
octa-chlorinated dibenzo-p-dioxins (TCDD, PeCDD, HxCDD, HpCDD, and OCDD) and
dibenzofurans (TCDF, PeCDF, HxCDF, HpCDF, and OCDF) as well as the concentration of
4-18
-------
each congener chlorinated in the 2, 3, 7, and 8 positions within each group. Analysis results are
given, by sample matrix, in Tables 4-10 through 4-14.
Two summary measures of dioxin/furan concentrations are commonly cited. The first
measure, total PCDD/PCDF, represents the sum of the homologue group total concentrations
analyzed. The second measure, 2,3,7,8-TCDD toxicity equivalent (TEQ), is a weighted sum of
each 2,3,7,8-chlorinated congener's concentration. In calculating TEQs, the measured
concentration of each specific 2,3,7,8-chlorinated congener is weighted by a toxicity equivalent
factor (TEF). The TEF is a measure of the congener's toxicity relative to 2,3,7,8-TCDD, which
has a TEF of 1. The TEFs used to calculate the TEQs here are those specified by EPA
(Reference 2) and given in Table 4-15.
Table 4-16 summarizes the chlorinated dioxin and furan concentrations in test program
samples in terms of the two summary measures. In many cases, concentrations in Table 4-16 are
reported as ranges. This arises out of the fact that analyzed concentrations for both homologue
group totals and specific congeners are often reported as being less than an MDL, as indicated
by the less than values in Tables 4-10 through 4-14. Thus, in cases where a concentration is
listed as a range in Table 4-16, the maximum value in the range corresponds to the assumption
that constituents not detected were present at the MDL, and the minimum value in the range
corresponds to the assumption that they were not present, i.e., at zero concentration.
The data in Table 4-16 show that the fluff feed contained 56 fig/kg of total PCE'D/
PCDF or 0.73 fig/kg on a TEQ basis (1 ng/kg, often reported as parts per billion, or ppb, equals
1,000 ng/kg, the unit used for solid samples in Table 4-16; 1 ng/kg is often reported as parts per
trillion, or ppt). Levels in the kiln ash discharge from the higher temperature incineration tests
were somewhat higher at 65 to 89 ng/kg total, or 1.2 to 2.0 /tg/kg TEQ. Levels in the kiln ash
discharge from the lower temperature incineration tests were substantially higher, at 8301 to
4-19
-------
TABLE 4-10. PCDDs AND PCDFs IN TEST FEED SAMPLES
Analyte
Total TCDD
2,3,7,8-TCDD
Total PeCDD
1,2,3,7,8-PeCDD
Total HxCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
Total HpCDD
1,2,3,4,6,7,8-HpCDD
OCDD
Total TCDF
2,3,7,8-TCDF
Total PeCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
Total HxCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
Total HpCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Test
Composite fluff
140
7.1a
180
31
1,360
45
110
150
3,160
1,590
10,700
2,660
110
2,740
250
220
4,660
1,580
470
530
180
9,360
4,180
2,240
22,100
feed concentration, i
Composite soil
170
2.8
310
18
680
28
54
77
790
430
2,290
1,360
34
1,220
51
100
1,260
420
100
150
7.2a
1,000
cen
120
920
ng/kg
Packaging container
material
1.6
0.20a
0.41
0.15a
3.2
<0.5
0.37
0.30a
20.2
10.0
126
6.3
0.50a
3.0
0.44
0.37
1.9
0.79
0.27
0.74a
<0.4
2.9
1 *3
2.6
<0.7
15.7
Estimated maximum possible concentration; see Appendix C-6.
4-20
-------
TABLE 4-11. PCDDs AND PCDFs IN KILN ASH SAMPLES
to
Kiln ash concentration, ng/kg
Fluff waste tests
Kiln exit gas temperature, °C
(°F)
Analyte
Total TCDD
2,3,7,8-TCDD
Total PeCDD
1,2,3,7,8-PeCDD
Total HxCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
Total HpCDD
1,2,3,4,6,7,8-HpCDD
OCDD
Total TCDF
2,3,7,8-TCDF
Total PeCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
Total HxCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
Total HpCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Testl
(H/9/93)
883
(1,622)
320
12
310
31
910
51
71
210
3,830
1,810
11,600
3,330
82
5,730
160
270
10,800
2,770
610
2310
25
15,800
6,180
1,360
12,200
Test 2
(11/16/93)
876
(1,608)
38
1.0
290
19
2,050
120
160
570
8,790
4,480
14,100
2,820
28
9,550
120
470
15,200
4,540«
1,220
4,110
83
21,200
6,210
3,810
15,400
TestS
(11/18/93)
762
(1,403)
3,190
230
10,500
990
40,400
1,850
3,100
8,300
117,000
56,100
109,000
64,300
760
110,000
3,450
9,520
101,000
54,800*
18,800
46,900
5,840
164,000
51,600
233,000
,114,000
Test 6
(11/23/93)
767
(1,412)
450
23"
7,120
400
53,900
2,080
3,650
9,770
107,000
107,000
739,000
72,200
500
179,000
2,370
15,500
448,000
325,000"
25,800
287,000
1,210
360,000
106,000
14,800
728,000
Soil tests
Test 3
(12/1/93)
876
(1,609)
3.4
0.09"
14
1.2*
47
31
3.6
14
110
57
230
ISO
3.2
300
7.2
24
430
120
29
80
1.7
610
320
47
510
Test 4
(12/2/93)
874
(1,606)
6.6
0.18
19
2.2"
96
6.5
7.4
36
160
88
180
310
3.6
600
11
44
830
230
54
140
4.6
910
120
95
500
Estimated maximum possible concentration; see Appendix C-6.
-------
TABLE 4-12. PCDDs AND PCDFs IN SCRUBBER LIQUOR SAMPLES
Post-test scrubber concentration, pg/L
Kiln exit gas temperature, *C
("F)
Analyte
Total TCDD
23,7,8-TCDD
Total PeCDD
1,2,3,7,8-PeCDD
Total HxCDD
1,23,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
Total HpCDD
1,2,3,4,6,7,8-HpCDD
OCDD
Total TCDF
2,3,7,8-TCDF
Total PeCDF
1,23,7,8-PeCDF
23,4,7,8-PeCDF
Total HxCDF
1,2,3,4,7,8-HxCDF
1,23,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
Total HpCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Blank test
Test 0 .
(10/27/93)
870
(1,599)
-------
TABLE 4-13. PCDDs AND PDCFs IN BAGHOUSE ASH SAMPLES
Baghouse ash concentration, ng/kg
Kiln exit gas temperature, °C
("*) .
Analyte
Total TCDD
23,7,8-TCDD
Total PeCDD
1,23,7,8-PeCDD
Total HxCDD
1,23,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,23,7,8,9-HxCDD
Total HpCDD
1,23,4,6,7,8-HpCDD
OCDD
Total TCDF
23,7,8-TCDF
Total PeCDF
1,23,7,8-PeCDF
2,3,4,7,8-PeCDF
Total HxCDF
1,23,4,7,8-HxCDF
1,23,6,7,8-HxCDF
23,4,6,7,8-HxCDF
1,23,7,8,9-HxCDF
Total HpCDF
1,23,4,6,7,8-HpCDF
1,23,4,7,8,9-HpCDF
OCDF
Blank test
TestO
(10/27/93)
870
(1,559)
0.17
0.08*
0.19
<0.1
13
<0.2
<0.1
036
10
53
38
1.1
0.70
2.5
0.28
0.55
4.0
1.0
0.41
1.0
<0.2
3.4
2.4
0.56
3.6
Fluff waste tests
Testl
(11/9/93)
883
(1,622)
0.90
<03
1.5
0.47
6.4
<0.4
0.69*
1.5
39
21
180
15
1.1
27
1.5
3.2
40
11
3.9*
9.1
<03
83
40
8.1
120
Test 2
(11/16/93)
876
(1,608)
<0.2
<0.2
0.62
<0.2
6.2
<0.2
0.85
1.7
40
21
180
12.
0.69
26 .
1.1
23
65
18
5.2
17
<0.2
120
79
15"
380
TestS
(11/18/93)
762
(1,403)
4.6
036
5.3
1.1
6.0
0.53
0.76*
1.6
20
11
51
39
1.9
50
3.4
4.7
46
10
4.7
8.9
1.9*
59
29
7.0
56
Test 6
(11/23/93)
767
(1,412)
0.6*
<0.6
3.9
<1.0
19
<0.9
1.8*
5.0
72
37
200
15
3.0
86
5.1
11
150
39
11
37
2.9*
250
110
34
230
Soil tests
Test 3
(12/1/93)
876
(1,609)
0.48
0.23
4.6
0.58
21
1.2
1.9*
1.6*
90
44
250
46
2.8
130
6.9
11
320
80
24
67
1.4
740
41
52
990
Test 4
(12/2/93)
874
(1,606)
03*
0.85*
<0.2
33
03*
0.68
1.4*
27
14
67
8.5
1.2
26
1.5*
3.5
61
15
5.5
15
038*
110
54
11
85
'Estimated maximum possible concentration; see Appendix C-6.
-------
TABLE 444. PCDDs AND PCDFs IN BAGHOUSE EXIT FLUE GAS
Baghouse exit flue gas concentration, ng/dscm
Kiln exit gas temperature, °C
CF)
Analyte
Total TCDD
2,3,7,8-TCDD
Total PeCDD
1,2,3,7,8-PeCDD
Total HxCDD
lA3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2^,7,8,9-HxCDD
Total HpCDD
1,2,3,4,6,7,8-HpCDD
OCDD
Total TCDF
23,7,8-TCDF
Total PeCDF
1,2,3,7,8-PeCDF
23,4,7,8-PeCDF
Total HxCDF
1,2,3,4,7,8-HxCDF
lA3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
lA3,7,8,9-HxCDF
Total HpCDF
1,2,3,4,6,7,8-HpCDF
1^,4,7,8,9-HpCDF
OCDF
Blank test
TestO
(10/27/93)
870
(1399)
< 0.002
< 0.002
<0.002
< 0.002
< 0.005
<0.005
<0.002
<0.005
0.005
0.005
0.017
0.017
0.002
0.012*
<0.002
<0.002
0.022
0.010
0.005
0.002"
<0.002
0.024*
0.012'
< 0.005
0.017
Fluff waste tests
Testl
(H/9/93)
883
(1,622)
0.006*
<0.002
0.006"
< 0.002
0.021
< 0.002
0.002
0.003
0.024
0.012
0.021
0.175
0.015
0.275
0.021
0.024
0.206
0.057
0.021
0.024
<0.002
0.067
0.051
0.006"
0.039
Test 2
(11/16/93)
876
(1,608)
0.002
< 0.002
0.006
< 0.003
0.006
< 0.002
0.002
0.002
0.021 '
0.009
0.027
0.246
0.012
0.249
0.024
0.021
0.224
0.058
0.024
0.024
<0.002
0.061
0.048
0.009
0.058
Tests
(11/18/93)
762
(1,403)
< 0.003
< 0.003
<0.006
< 0.006
< 0.003
<0.006
< 0.003
< 0.003
0.009"
0.006"
0.024
0.065
0.006
0.065
0.009
0.009
0.059
0.018
0.006
0.012
< 0.003
0.042
0.027
< 0.006
0.027
Test 6
(11/23/93)
767
(1,412)
0.003
<0.003
<0.006
<0.006
0.003
<0.006
<0.003
< 0.003
0.009"
0.006"
0.016
0.169
0.019
0.228
0.019
0.022
0.169
0.047
0.016
0.022
<0.003
0.056
0.047
<0.006
0.031
Soil tests
Test3
(12/1/93)
876
(1,609)
<0.002
< 0.002
<0.003
<0.003
0.013
<0.003
<0.002
<0.002
0.013
0.013
0.066
0.078
0.009
0.097
0.009
0.013
0.085
0.031
0.009
0.016*
<0.002
0.066
0.035
0.006
0.035
Test 4
(12/2/93)
874
(1,606)
0.001
<0.001
< 0.001
< 0.001
0.003
<0.001
0.002
0.001"
0.019
0.009
0.044
0.078
0.006
0.062
0.006
0.009
0.056
0.019
0.006"
0.012
0.001
0.044
0.025
0.006
0.025
"Estimated maximum possible concentration; see Appendix C-6.
-------
TABLE 4-15. 2,3,7,8-TCDD TOXICITY EQUIVALENT FACTORS
(Reference 2)
. Compound Toxicity equivalent factor
2,3,7,8-TCDD 1
Other TCDDs 0
2,3,7,8-PeCDD 0.5
Other PeCDDs 0
2,3,7,8-HxCDD 0.1
Other HxCDDs 0
2,3,7,8-HpCDD 0.01
Other HpCDDs 0
OCDD 0.001
2,3,7,8-TCDF 0.1
Other TCDFs 0
1,2,3,7,8-PeCDF 0.05
2,3,4,7,8-PeCDF 0.5
Other PeCDFs 0
2,3,7,8-HxCDFs 0.1
Other HxCDFs 0
2,3,7,8-HpCDFs 0.01
Other HpCDFs 0
OCDF 0.001
4-25
-------
TABLE 4-16. TOTAL DIOXINS AND TEQs IN TEST PROGRAM SAMPLES
Sample
Test 0 (10/27/93), kiln temperature:
870°C (1,599°F)
Packaging container material, mg/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghouse exit flue gas ng/dscm at 7% O2
Fluff Waste Tests
Fluff feed, ng/kg
Test 1 (11/9/93), kiln temperature:
883 °C (1,622°F)
Kiln ash, ng/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghouse exit flue gas, ng/dscm at 7% O2
Test 2 (11/16/93), kiln temperature:
876°C (1,608°F)
Kiln ash, ng/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghpuse exit flue gas, ng/dscm at 7% O2
Test 5 (11/18/93), kiln temperature:
762 °C (1,403 °F)
Kiln ash, ng/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghouse exit flue gas, ng/dscm at 7% O2
Test 6 (11/23/93), kiln temperature:
767°C (1,412°F)
Kiln ash, ng/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghouse exit flue gas, ng/dscm at 7% O2
Total PCDD/PCDF
180
68-170
64
0.21
56,000
65,000
370-380
520
1.3
89,000
730-750
740
1.3
830,000
290
340
0.44
2,700,000
520-540 '
1,000
0.96
TEQ
1.2-1.3
9.7-25
0.94-1.0
0.005-0.017
730
1,200
4.6-12
6.8-7.0
0.048-0.052
2,000
7.0-23
8.9-9.2
0.044-0.049
29,000
17-18
81
0.016-0.027
110,000
6.7-23
22-23
0.038-0.049
(continued)
4-26
-------
TABLE 4-16. (continued)
Sample
SoU Feed Tests
Soil feed, ng/kg
Test 3 (12/1/93), kiln temperature:
876 °C (1,609 °F)
Kiln ash, ng/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghouse exit flue gas, ng/dscm at 7% O2
Test 4 (12/2/93), kiln temperature:
874°C (1,606°F)
Kiln ash, ng/kg
Scrubber liquor, pg/L
Baghouse ash, ng/kg
Baghouse exit flue gas, ng/dscm at 7% O2
Total PCDD/PCDF
10,000
2,400
2,300-2,400
2,600
0.68
3,600
260-280
390
0.48
TEQ
210
55
46-54
39
0.025-0.032
98
1.3-15
8.2-8.4
0.018-0.020
2,700 /ig/kg total, or 29 to 110 /zg/kg TEQ. These data indicate that, not only was incineration
treatment ineffective in destroying contaminant dioxins and furans in the fluff waste, in fact
conditions experienced by the noncombustible fraction of the fluff waste during incineration
likely led to PCDD/PCDF formation at the lower temperature.
That PCDD/PCDF formation in the kiln ash discharge occurred, at least for the fluff
waste tests at the lower incineration temperatures, is further substantiated by the data in
Table 4-17. The total weight of fluff waste or soil fed and the total weight of kiln ash collected
for each test are combined with respective PCDD/PCDF concentrations from Table 4-16 to
ultimately give the ratios of the amounts of dioxins and furans discharged in the kiln ash to the
amounts introduced in the incinerator feed for each test. The data show that, for the fluff waste
tests at the target 870°C (1,600°F) kiln exit gas temperature, the amount of total PCDD/PCDF
discharged was 5.9 to 8.3 percent of the amount introduced to the incinerator in the fluff feed.
4-27
-------
TABLE 4-17. RATIO OF DISCHARGED DIOXINS AND FURANS TO FED AMOUNTS
Waste feed
Test
Fluff Waste Tests
Test 1 (11/9/93)
Kiln temperature:
883°C (1,622°F)
Test 2 (11/16/93)
Kiln temperature:
876°C (1,608°F)
Test 5 (11/18/93)
Kiln temperature:
762°C (1,403°F)
Test 6 (11/23/93)
Total weight
fed, kg
303
304
307
305
PCDD/PCDF fed, ng
Total
PCDD/PCDF TEQ
17,000 220
17,000 220
17,200 220
17,100 220
s=s::======:======s=======s=====================^^
Ratio of PCDD/PCDF
discharged to amount fed,
Kiln ash discharge %
Total weight
discharged, kg
15.4
15.9
20.4
17.3
PCDD/PCDF
discharged, jig
Total
PCDD/PCDF TEQ Total PCDD/PCDF TEQ
1,000 18 5.9 8.4
1,420 32 8.3 14.3
16,900 590 98.5 264
46,700 1,900 273 855
767°C
Soil Feed Tests
Test 3 (12/1/93)
Kiln temperature:
876°C (1,609'F)
Test 4 (12/2/93)
Kiln temperature:
874°C (1,606°F)
288
290
2.900
60
61
101
145
240
520
5.6
14.2
8.5
18.0
9.2
23.4
-------
This would correspond to an effectiveness of dioxin/furan decontamination by incineration at
this higher tested temperature of 91.7 to 94.1 percent. On a TEQ basis, the ratio of discharged-
to-fed dioxins/furans was 8.4 to 14.3 percent, corresponding to incineration decontamination
effectiveness or a TEQ basis of 85.7 to 91.6 percent at the higher incineration temperature.
However, for the fluff waste tests at the 760°C (1,400°F) target kiln exit gas
temperature, the amount of total PCDD/PCDF discharged was 98.5 to 273 percent of the
amount fed. In other words, the quantity of total PCDD/PCDF discharged for the lower kiln
temperature fluff tests was roughly the same to 2.7 times the amount fed to the incinerator. On
a TEQ basis the ratios of discharged to feed dioxins/furans were even larger, at 264 to
855 percent. Clearly, at the lower incineration temperatures, dioxins/furans were beingproduced
in the noncombustible fraction of the fluff waste feed ultimately discharged as kiln ash.
This should not be surprising, however. It has become recognized over the past few
years that dioxins and furans arising out of combustion processes result from the formation of
these compounds from precursor organic constituents and a chlorine source, such as HC1, at
relatively low temperatures (Reference 5). The presence of metal-containing solids, such as
particulate, appears to catalyze the process. Copper has specifically been shown to catalyze
reactions leading to dioxin/furan formation. The rate of dioxin/furan formation is highest at
temperatures near 300 °C (570 °F), and this rate decreases as the temperature at which
precursors, a chlorine source, and metal-bearing solids are held is either increased or decreased.
Evidently, the right combination of conditions were in place in the kiln solids bed before,
or shortly after, discharge from the kiln into the ash collection pit of the RKS during the
incineration of the fluff waste at the 760°C (1,400°F) target kiln temperature. Dioxin/furan
precursors were likely present in the near-bed combustion gas, and chlorine, likely in the form
of HC1 from the chloroorganic components of the fluff, was likely in abundance. The fluff waste
4-29
-------
tested contained 17 percent by weight chlorine. As discussed below, a major contaminant metal
in the fluff waste was copper, so this likely dioxin-formation catalyst was present. Apparently
kiln solids bed temperatures were sufficiently close to the peak reaction temperature of 300°C
(570 °F) to be within a "dioxin formation" window. The data clearly show that dioxin formation
occurred at the lower incineration temperature tested.
All other dioxin formation conditions would have been in effect for the fluff incineration
tests, at the 870°C (1,600°F) target kiln exit gas temperature. However, at this higher
incineration temperature, kiln solids bed temperatures were apparently above the window
associated with more rapid dioxin formation. Similar results were seen in the soil feed tests, also
performed at the higher, 870°C (1,600°F), target kiln exit gas temperature. Ratios of discharged
to feed PCDD/PCDFs noted in Table 4-17 for the soil tests are comparable to those experienced
for the fluff waste tests at the higher incineration temperature.
Returning to the data in Table 4-16, the scrubber liquor for the fluff waste tests
contained total PCDD/PCDF concentrations in the 290 to 750 pg/L (1 pg/L is often reported
as parts per quadrillion, or ppq). Scrubber liquor concentrations were in the 4.6 to 23 pg/L
ranges on a TEQ basis. No apparent difference in the scrubber liquor concentrations with
incineration temperature was seen. The scrubber liquor concentration measured during the
blank burn test was comparable to those for the fluff waste tests on a TEQ basis, though total
PCDD/PCDF concentrations were slightly lower. Scrubber liquor dioxin/furan concentrations
for one of the two soil feed tests were also comparable to those measured for the fluff waste
tests, although levels measured for the other soil feed test were substantially higher.
Baghouse ash total PCDD/PCDF concentrations ranged from 340 to 1,000 ng/kg (ppt)
for the fluff waste tests, with no apparent change associated with changing incineration
temperature. On a TEQ basis, the measured range was 6.8 to 23 ng/kg. Baghouse ash dioxin
4-30
-------
levels were lower for the blank burn test on both bases. As for the scrubber liquor, baghoese
ash dioxin levels for one of the two soil feed tests were comparable to those measured for the
fluff waste tests; they were higher for the other soil feed test.
Baghouse exit flue gas total PCDD/PCDF levels were 0.021 ng/dscm corrected to
7 percent O2 for the blank burn test. Measured levels were increased, at 1.3 ng/dscm at
7 percent O2, for the fluff waste tests at the 870°C (1,600°F) target kiln exit gas temperature.
Levels for the fluff waste test at the 760°C (1,400°F) target kiln exit gas temperature, at 0.44 to
0.96 ng/dscm at 7 percent O2, were slightly lower than for the higher temperature tests. Levels
for the soil feed tests were comparable, at 0.48 to 0.68 ng/dscm. All measured levels were
significantly lower than the EPA guidance announced in 1993 of 30 ng/dscm at 7 percent O2.
On a TEQ basis, baghouse exit flue gas dioxin/furan levels were 0.005 to 0.017 ng/dscm
at 7 percent O2 for the blank burn test, increased, at 0.044 to 0.052 ng/dscm at 7 percent O2 for
the fluff waste tests at the 870°C (1,600°F) target kiln exit gas temperature. Compared to these
latter levels, comparable to slightly decreased emissions, at 0.016 to 0.049 ng/dscm at 7 percent
O2, were measured for the fluff waste tests at the 760°C (1,400°F) target kiln exit gas
temperature. Levels measured for the soil feed tests were also comparable, at 0.018 to
0.032 ng/dscm at 7 percent O2. The European suggested dioxin emission limit for waste
incinerators is 0.1 ng/Nm3 TEQ corrected to 11 percent O2. Thus, while the temperature
correction for son is slightly different than for Nm3, and the O2 correction for the European
standard, at 11 percent O2, differs from the 7 percent O2 used in the Table 4-16 data, all
emission levels reported in Table 4-16 are lower than the suggested European standard
4.5 TRACE METAL AND TCLP ANALYSIS RESULTS
Trace metal concentrations measured in test program samples are summarized in
Table 4-18. The data in the table clearly show that the major metal contaminants in both the
4-31
-------
TABLE 4-18. TRACE METAL ANALYSIS RESULTS
Sample
Test 0 (10/27/93), kiln temperature: 870°C (1,599°F)
Packaging container material, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Fluff Waste Tests
Test 1 (11/9/93), kiln temperature: 883°C (1,622°F)
Fluff feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
^ Baghouse exit flue gas, /«g/dscm
»o Test 2 (11/16/93), kiln temperature: 876°C (1,608'F)
Fluff feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, pg/dscm
Test 5 (11/18/93), kiln temperature: 762eC (1,403'F)
Fluff feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /tg/dscm
Sb
Concentration
As
Ba Cd
Cr
Cu
Pb
Ni
Ag
Zn
<20
0.7
120
<20
<0.05
<20
6.7
8.5
18
<0.5
0.05
6.6
1.0
0.7
510
<2
0.6
58
<10
18
410
<4
030
150
<0.7
<0.007
<0.7
8.9
6.6
1,800
120
1,100
4.7
830
<21
180
940
3.7
400
<11
90
950
4.7
1,300
IJIIL1 "- '
<20
<20
0.12
24
<19
<20
30
0.08
<20
<22
<20
<20
0.20
<20
Ml .!_ .
74
270
2.4
38
50
70
220
1.8
22
6
47
240
1.5
35
6
*" i
1.4
<0.5
0.20
33
<50
1.5
<0.5
0.14
18
-------
TABLE 4-iS. (continued)
Concentration
Sample
Sb
As
Ba
Cd
Cr
Cu
Pb
Ni
Ag
Zn
fk
u>
Fluff Waste Tests (concluded)
Test 6 (11/23/93), kiln temperature: 767°C (1,412°F)
Fluff feed, mg/kg
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, pg/dscm
Soil Feed Tests
100
950
4.9
1,900
<10
<20
46
0.10
<20
<14
81
250
1.4
19
5
1.0
<0.5
0.20
70
<1
24
530
1.4
510
<4
8,400
176,000
180
77,000
26
900
5,700
610
38,000
38
4.6
340
0.9
160
<4
13
3.0
0.08
1.0
<2
120
250
12
5,000
44
Average soil feed, mg/kg
Test 3 (12/1/93), kiln temperature: 876°C (1,609°F)
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, jtg/dscm
Test 4 (12/2/93), kiln temperature: 874°C (1,606°F)
Kiln ash, mg/kg
Scrubber liquor, mg/L
Baghouse ash, mg/kg
Baghouse exit flue gas, /tg/dscm
66
190
1.5
1,400
<10
190
13
950
<13
<20
<20
<0.05
<70
<15
<20
<0.05
<20
<29
72
120
13
29
10
91
1.3
19
6
13
<0.5
0.10
57
<1
<0.5
0.20
43
<2
85
73
0.8
540
<3
56
1.0
520
<3
14,000
53,000
iio
64,000
51
35,000
160
52,000
620
3,100
4,100
120
48,000
190
4,100
180
41,000
2,030
29
62
03
190
<9
51
0.4
200
<6
<2
1.5
0.02
<0.7
<2
1.9
0.02
<0.7
<2
190
320
3
4,200
20
290
4
2,900
42
-------
fluff waste and the contaminated soil were copper and lead. Both of these metals were also
present in the kiln ash discharge for all tests. The presence of high concentrations of these
metals, especially copper, in the kiln ash discharge substantiates that presumed catalysts for the
relatively low temperature reactions in the dioxin formation pathway would be present in the kiln
ash so that dioxin formation in this matrix, especially as noticed for the lower incineration
temperature fluff waste tests, can be understood.
Fluff and soil feed, kiln ash, scrubber liquor, and baghouse ash samples from the test
program were subjected to the TCLP, and resulting TCLP leachates were analyzed for the test
program trace metals. Leachate analysis data are summarized in Table 4-19 For the six TCLP
metals with regulatory levels defined, the regulatory level is also given in the table. The data in
the table show that the fluff waste from two of the four tests would be a lead-contaminated TC
hazardous waste. Further, the lead concentrations in the leachates of the fluff for the other two
tests were very close to the regulatory level for lead. Despite this, no resulting kiln ash discharge
from the incineration of fluff waste would be a TC hazardous waste due to its leachable lead, or
any other metal analyzed, concentration. Similarly, the scrubber liquor from all fluff waste tests
was not TC hazardous. However, the baghouse ash for all fluff waste tests would be a lead-
contaminated TC hazardous waste, and for three of the four tests a cadmium-contaminated TC
hazardous waste.
Although the contaminated soil tested was not a TC hazardous waste, conclusions
regarding the TC status of the residual discharges from its incineration were the same as for the
fluff waste. Namely, neither the kiln ash discharge nor the scrubber liquor resulting from its
incineration under the conditions tested would possess the TC, and the baghouse ash for both
tests performed would be considered both cadmium- and lead-contaminated TC hazardous waste.
4-34
-------
TABLE 4-19. TCLP LEACHATE ANALYSIS RESULTS
Leachate concentration, mg/L
Sample leached
Regulatory Level
Test 0 (10/27/93), kiln temperature: 870°C (1,599°F)
Scrubber liquor
Baghouse ash
Fluff Waste Tests
Test 1 (11/9/93), kiln temperature: 883°C (1,622°F)
Fluff feed
Kiln ash
Scrubber liquor
Baghouse ash
Test 2 (11/16/93), kiln temperature: 876°C (1,608°F)
Fluff feed
Kiln ash
Scrubber liquor
Baghouse ash
Test 5 (11/18/93), kiln temperature: 762°C (1,403°F)
Fluff feed
Kiln ash
Scrubber liquor
Baghouse ash
Test 6 (11/23/93), kiln temperature: 767°C (1,412°F)
Fluff feed
Kiln ash
Scrubber liquor
Baghouse ash
Sb
__«
<0.03
33
0.23
<0.03
0.55
0.85
0.26
0.05
0.42
0.43
0.26
0.24
0.60
<0.2
0.26
0.28
0.71
<0.2
As
5
<0.05
0.34
<0.05
<0.05
<0.05
0.20
<0.05
<0.05
<0.05
0.08
<0.05
<0.2
<0.05
<0.2
<0.05
<0.2
<0.05
<0.2
Ba
100
0.17
0.25
0.25
1.2
0.93
0.23
0.26
13
0.76
0.05
0.19
2.2
0.60
0.4
0.55
1.2
0.6
0.6
Cd
1
< 0.004
030
0.03
< 0.004
0.03
1.4
0.04
< 0.004
0.03
0.9
0.03
< 0.005
0.03
1.8
0.03
<0.005
0.02
1.8
Cr
5
0.052
4.5
< 0.007
0.32
0.06
0.29
< 0.007
0.41
0.04
0.20
<0.007
0.05
0.04
0.13
< 0.007
0.01
0.05
0.2
Cu
0.05
1.4
120
0.14
0.91
720
130
0.05
0.09
340
130
<0.02
13
1,400
130
0.072
1.2
1,400
Pb
5
<0.04
0.07
3.6
0.42
0.52
3,800
5.4
0.09
0.40
1,900
3.7
<0.1
2.2
5,200
5.8
050
0.6
4,400
Ni
_
<0.01
1.7
0.02
<0.01
0.08
2.0
0.02
0.01
0.06
28
0.02
<0.01
0.05
23
0.02
<0.01
0.06
2.8
Ag
5
< 0.007
< 0.007
<0.007
< 0.007
0.08
< 0.007
< 0.007
<0.007
0.09
0.02
< 0.007
< 0.007
0.06
0.02
<0.007
< 0.007
0.08
0.02
r=^^==
Zn
_,
0.12
84
3.2
0.03
0.16
150
4.1
0.07
0.13
100
3.7
0.02
0.10
180
4.6
0.02
0.10
200
g"
No regulatory level; not a TCLP metal.
(continued)
-------
TABLE 4-19. (continued)
O\
Leachate concentration, mg/L
Sample leached
Regulatory Level
Soli Feed Tests
Average soil feed
Test 3 (12/1/93), kiln temperature: '8760C (1,609°F)
Kiln ash
Scrubber liquor
Baghouse ash
Test 4 (12/2/93), kiln temperature: 874°C (1,606°F)
Kiln ash
Scrubber liquor
Baghouse ash
m Nrt rponfatArv l*nM»1- tint o TV'T P Miafaf
Sb
a
0.09
<0.2
0.09
0.90
<0.2
0.08
0.80
As
5
<0.05
<0.2
<0.05
0.2
<0.2
<0.05
0.24
Ba
100
0.91
0.26
0.16
0.50
'0.70
0.09
0.2
Cd
1
0.02
< 0.005
<0.004
2.2
<0.005
.< 0.004
1.7
Cr
5
< 0.007
0.05
0.04
03
0.03
0.10
03
Cu
21
0.25
0.02
760
0.2
0.09
640
Pb
5
0.67
0.08
6,600
0.2
039
5,700
Ni
_
0.02
<0.01
<0.01
2.7
<0.01
0.24
3.2
Ag
5
< 0.007
< 0.007
< 0.007
0.03
< 0.007
< 0.007
0.03
===:
Zn
H
1.1
13
0.01
120
0.04
0.03
100
___
-------
The scrubber liquor TCLP leachate metals content data given in Table 4-19 deserve
some discussion, especially when compared to the scrubber liquor metals content data given in
Table 4-18. The scrubber liquor metals data in Table 4-18 correspond to complete scrubber
liquor samples, including the suspended solids in the liquor. For liquid samples containing
suspended solids, the TCLP specifies filtering the sample. If the resulting filtered solids content
of the sample is less than 0.5 percent (the case for all scrubber liquor samples collected in this
test program), then the filtrate is defined to be the sample TCLP leachate.
Comparing the scrubber liquor data in Table 4-19 to the data in Table 4-18 shows that
the metals concentrations in the scrubber liquor TCLP leachate are almost always less than, and
in many cases much less than, the corresponding concentrations in the complete scrubber liquor.
This suggests that most of the scrubber liquor's metals content was accounted for in the
suspended solids fraction of the liquor.
Special attention to the lead concentrations is warranted. Lead concentrations in bulk
scrubber liquor samples were in the 120 to 789 mg/L range for the fluff waste and soil feed tests.
These levels far exceed the regulatory level for lead of 5 mg/L. However, lead concentrations
in scrubber liquor TCLP leachates (scrubber liquor filtrate after removal of the suspended solids)
ranged from 0.08 to 2.2 mg/L over the fluff waste and soil feed tests, all below lead's regulatory
level.
4.6 PARTTCULATE AND HC1 EMISSIONS
The baghouse exit flue gas particulate and HC1 emission data developed in the test
program are summarized in Table 4-20. The data show that baghouse exit particulate
concentrations were less than 10 mg/dscm corrected to 7 percent O2 for all but one test for
which they were 14 mg/dscm at 7 percent O2. All measured levels were well below the current
4-37
-------
Baghouse exit
Test
Test 0 (10/27/93)
Fluff Waste Tests
Test 1 (11/9/93)
Test 2 (11/16/93)
Test 5 (11/18/93)
Test 6 (11/23/93)
Soil Feed Tests
Test 3 (12/1/93)
Test 4 (12/2/93)
Cl feedrate,
kg/hr
0.28
9.48
9.48
9.48
9.48
1.1
1.1
gJ"!
Paniculate
concentration,
mg/dscm at 7%
°2
7
7
4
6
14
5
9
HCI emission
rate, g/hr
<0.2
1.7
2.0
2.0
2.3
2.6
0.7
Apparent
system HCI
collection
efficiency, %
> 99.93
99.98
99.98
99.98
99.98
99.76
99.94
hazardous waste incinerator performance standard of 180 mg/dscm at 7 percent O2, and even
substantially below the EPA's announced 1993 guidance of 34 mg/dscm at 7 percent O2.
Baghouse exit flue gas HCI emission rates were at most 2.6 g/hr. Apparent system
collection HCI efficiencies were greater than 99.9 percent for all except one soil feed test for
which the apparent system HCI collection efficiency was 99.76 percent.
Particle size distribution measurements were also performed for each test using an
Andersen cascade impactor train in the afterburner extension. The cascade impactor particle
size distribution data analysis worksheets are presented in Appendix D-6. Figure 4-1 shows the
size distribution data in the form of log-probability plot of cumulative mass percent less than
particle diameter (y-axis, probability scale) versus particle diameter (x-axis, log scale). A straight
line on such a plot corresponds to a log-normal size distribution.
4-38
-------
Cumulative percent less than size
p
en
00
(71
CO
09
CO
33
t
i
"§
a
g'
a.
01
ro
O.
CD
CO
N*
CD
01
ro
o
to
0>
en
CO
IV)
tpl
-------
The distribution data shown in Figure 4-1 indicate that the size distributions of the
afterburner exit particulate were comparable for 5 of the 6 tests, with the particulate for these
5 tests being relatively fine, with 50 percent less than 1 jim. The distribution for Test 6 was
distinctly shifted to much larger particle size, with over 90 percent greater than 1 ^m. No
explanation for this shift is offered here.
4-40
-------
SECTION 5
CONCLUSIONS
Results of the test program conducted to evaluate the incineration treatment of fluff
waste and contaminated soil from the M. W. Manufacturing Superfund site confirm that
incineration represents an effective treatment option, but several cautions regarding its use need
emphasis. Indeed, incineration of the fluff waste offers several benefits including substantial
waste volume reduction, and effective, near complete, decontamination and destruction of both
the VOC and SVOC contaminants in the waste. While the volume reduction benefit is less
significant in the incineration treatment of the contaminated soil, the benefit of effective and
near complete decontamination and destruction of organic POHC contaminants remains.
Both site materials can be incinerated in compliance with the current hazardous waste
incinerator performance standards in a rotary kiln incineration system of the type in place at the
IRF with an APCS consisting of a wet scrubber for acid gas control and a baghouse for final
particulate control. Specifically:
Greater than 99.99 percent POHC DREs were uniformly measured
HC1 emissions were well below 1.8 kg/hr and system HC1 control efficiencies well
above 99 percent
In addition, compliance with the more recent incinerator emissions guidance announced in 1993
was demonstrated. Specifically:
5-1
-------
Paniculate emissions measured were well below 34 mg/dscm corrected to
7 percent O2
Total PCDD/PCDF emissions measured were well below 30 ng/dscm corrected
to 7 percent O2
In fact, measured dioxin/furan emissions on a TEQ basis were well below the suggested
European emission limit of 0.1 ng/Nm3 dry at 11 percent O2.
However, the kiln ash discharge from the incineration of both site materials remains
dioxin-contaminated. The kiln ash discharge from the incineration of contaminated site soil at
a kiln temperature of nominally 870°C (1,600°F) contained total PCDD/PCDF concentrations
of 2.4 to 3.6 /ig/kg. Levels in the kiln ash discharge from the incineration of fluff waste at a
nominal kiln temperature of 870°C (1,600°F) were higher, at 65 to 89 /ig/kg. Levels in the kiln
ash discharge from the incineration of fluff waste at a nominal kiln temperature of 760°C
(1,400 °F) were substantially higher, at 830 to 2,700 Mg/kg.
Thus, with respect to fluff waste, incineration offers substantial volume reduction,
however the resulting treated waste discharge (kiln ash) may still need to be managed as a
dioxin-contaminated material. Dioxin contamination levels were decreased at higher incineration
temperatures, but they remained significant nonetheless. Perhaps even higher incineration
temperatures, with or without the use of an ash water quench system, would give a kiln ash
discharge relatively free of dioxin contamination. However, further tests are needed to
investigate this possibility.
In addition, the flue gas particulate collected as baghouse ash in essentially all tests was
a cadmium- and lead-contaminated TC hazardous waste. Thus, this discharge would need to be
appropriately managed as a hazardous waste.
5-2
-------
All quality assurance (QA) objectives for the test program were met, with the exception
of:
The MDL objectives for:
Tetrachloroethene in solid residues
Trichloroethehe in aqueous liquids
2-nitrophenol in flue gas
Zinc in aqueous liquids
The accuracy and precision objectives for antimony, barium, and silver as assessed
by analyte recovery from MS samples and the RPD of MS/MSD analyses
The accuracy objective for the other seven test trace metals as assessed by analyte
recovery from MS samples
The MDLs achieved for the above four analyte/sample matrix combinations were not
significantly greater than the respective objectives, so no measurable effects on test program
conclusions resulted.
Failure to meet the precision and accuracy objectives for the antimony, barium, and
silver analyses leads to the conclusion that test program results for these three metals are
compromised. The reported data for these three metals should be treated with caution, and test
program conclusions regarding these three metals must be viewed as tentative.
The accuracy objective of 70 to 130 percent recovery from MS samples was not met for
the other seven test trace metals. However, an objective of 60 to 140 percent recovery would
have been met. This suggests that test program results and conclusions regarding these seven
analytes are valid and defensible, but are just not as certain as had been planned.
5-3
-------
SECTION 6
QUALITY ASSURANCE
This test program was carried out as outlined in the Quality Assurance Project Plan
(QAPP) for Pilot-Scale Incineration Testing of Fluff Waste and Contaminated Soil from the
M. W. Manufacturing Superfund Site. Thus, all QA aspects of the program were completed as
specified in the QAPP. FJxcept as noted, all tests were performed in accordance with the
procedures documented in the QAPP.
All samples analyzed to obtain data reported in this report were taken at the IRF by
members of the IRF operating staff. All samples were collected and/or recovered in accordance
with the methods appropriate to their eventual analysis. After appropriate preservation, the
samples were relinquished to the custody of the onsite Sample Custodian. The Sample
Custodian subsequently directed the splitting of samples and the transport of these to the
appropriate laboratories for analysis. The sample chain-of-custody procedures described in the
QAPP for these tests were followed. No compromise in sample integrity occurred, with one
exception as noted below.
Numerous QA procedures were followed to assess the data quality of laboratory
9
analytical measurements performed in this test program. These included blank sample analyses,
duplicate analyses, and matrix spike (MS) and matrix spike duplicate (MSD) sample analyses.
Method blank samples were analyzed for all sample matrices for which logical matrix blanks
6-1
-------
could be prepared. Results of QA procedures performed for the critical laboratory
measurements are discussed, by analyte group, in the following subsections.
6.1 VOC ANALYSES
A total of 50 solid and aqueous samples was analyzed for VOCs by GC/FID using
Method 8015A. Included in this group were 5 MS/MSD sample sets and 5 duplicate analyses
of test samples. Table 6-1 lists sample collection date, analysis date, and analysis hold time for
these samples. The data in Table 6-1 show that 49 of the 50 samples were analyzed within the
method hold time limit of 14 days. Table 6-2 provides an analogous listing for flue gas samples
analyzed for volatile organic constituents by GC/MS using Method 5040. The data in Table 6-2
show that 35 out of 36 samples were analyzed, and that'all of those analyzed were analyzed
within the method hold time limit of 42 days. One sample, the Test 3 field blank, was lost in
shipment (the compromise in sample integrity mentioned above). Still, analytical completeness
was 97 percent (35 of 36).
( Table 6-3 summarizes the VOC analysis quality assurance objectives (QAOs) for
precision, accuracy, and completeness. Table 6-4 shows the method detection limit (MDL)
objectives and the achieved values for the VOC analyses. As can be seen in Table 6-4 the MDL
objective was met for all primary target analytes except tetrachloroethene in solid residues and
trichloroethene in aqueous liquids. In addition, all secondary target analyte MDLs in flue gas
samples were met.
VOC analysis precision and accuracy were assessed for GC/FID analyses by preparing
one MS/MSD sample set for each of the fluff waste, contaminated soil, scrubber liquor, kiln ash,
and baghouse ash sample matrices and measuring spike recovery. One pair of VOST traps was
spiked with the primary target analytes for each test and analyzed by GC/MS. In addition, one
6-2
-------
TABLE 6-1. SAMPLE HOLD TIMES FOR THE VOC ANALYSES OF SOLID AND LIQUID
SAMPLES BY GC/FID
Sample
Test Feed
Test 0
Composite fluff
Composite fluff duplicate
Composite fluff MS
Composite fluff MSB
Testl
Test 2
TestS
Test 6
TestS
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
Scrubber Liquor
Test 0 pretest
Test 0 post-test
Test 0 post-test duplicate
Test 0 post-test MS
Test 0 post-test MSD
Test 1 pretest
Test 1 post-test
Test 2 pretest
Test 2 post-test
Test 3 pretest
Test 3 post-test
Test 4 pretest
Test 4 post-test
Test 5 pretest
Test 5 post-test
Test 6 pretest
Test 6 post-test
Method Requirement
Collection date
12/21/93
10/14/93
10/14/93
10/14/93
10/14/93
10/14/93
10/14/93
10/18/93
10/18/93
10/20/93
10/20/93
10/20/93
10/20/93
10/20/93
10/27/93
10/27/93
10/27/93
10/27/93
10/27/93
11/09/93
11/09/93
11/16/93
11/16/93
12/01/93
12/01/93
12/02/93
12/02/93
11/18/93
11/18/93
11/23/93
11/23/93
Analysis date
01/10/94
10/25/93
10/25/93
10/27/93
10/27/93
10/25/93
10/26/93
10/26/93
10/29/93
10/28/93
10/28/93
10/29/93
10/29/93
10/29/93
11/03/93
11/03/93
11/04/93
11/03/93
11/03/93
11/11/93
11/11/93
11/23/93
11/23/93
12/07/93
12/07/83
12/07/93
12/07/93
11/29/93
11/29/93
12/06/93
12/06/93
Analysis hold time, days
20
11
11
13
13
11
12
8
11
8
8
9
9
9
7
7
8
7
7
2
2
7
7
6
6
5
5
11
11
13
13
14
(continued)
6-3
-------
TABLE 6-1. (continued)
Sample
Kiln Ash
Test 1
Test 2
Test 3
Test 3 duplicate
Test 3 MS
Test 3 MSB
Test 4
TestS
Test 6
Baghouse Ash
TestO
Test 1
Test 2
Test3
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
TestS
Test 6
Method Requirement
Collection date
11/09/93
11/16/93
12/01/93
12/01/93
12/01/93
12/01/93
12/02/93
11/18/93
11/23/93
10/28/93
11/09/93
11/16/93
12/01/93
12/01/93
12/01/93
12/01/93
12/02/93
11/18/93
11/23/93
Analysis date
11/11/93
11/23/93
12/08/93
12/08/93
12/08/93
12/08/93
12/10/93
11/29/93
12/06/93
11/04/93
11/11/93
11/23/93
12/09/93
12/09/93
12/09/93
12/09/93
12/10/93
11/29/93
12/06/93
Analysis hold time, day:
2
7
7
7
7
7
8
11
13
7
2
7
8
8
8
8
8
11
13
14
6-4
-------
TABLE 6-2. SAMPLE HOLD TIMES FOR THE VOC ANALYSES OF METHOD 0030
SAMPLES BY GC/MS
Sample
Test 0, Set 1
Test 0, Set 2
Test 0, Set 3
Test 0, Field blank
Test 0, MS
Test 1, Set 1
Test 1, Set 2
Test 1, Set 3
Test 1, Field blank
Test 1, MS
Test 2, Set 1
Test 2, Set 2
Test 2, Set 3
Test 2, Field blank
Test 2 MS
Test 3, Set 1
Test 3, Set 2
Test 3, Set 3
Test 3, Field blank
Test 3, MS
Test 4, Set 1
Test 4, Set 2
Test 4, Set 3
Test 4, Field blank
Test 4, MS
Test 5, Set 1
Test 5, Set 2
Test 5, Set 3
Test 5, Field blank
Test 5, MS
Test 6, Set 1
Test 6, Set 2
Test 6, Set 3
Test 6, Field blank
Test 6, MS
Trip blank
Method Requirement
Collection date
10/27/93
10/27/93
10/27/93
10/27/93
10/27/93
11/09/93
11/09/93
11/09/93
11/09/93
11/09/93
11/16/93
11/16/93
11/16/93
11/16/93
11/16/93
12/01/93-
12/01/93
12/01/93
12/01/93
12/01/93
12/02/93
12/02/93
12/02/93
12/02/93
12/02/93
11/18/93
11/18/93
11/18/93
11/18/93
11/18/93
11/23/93
11/23/93
11/23/93
11/23/93 .
11/23/93
12/07/93
Analysis date
11/09/93
11/09/93
11/09/93
11/09/93
11/09/93
11/22/93
11/22/93
11/22/93
11/22/93
11/22/93
12/03/93
12/03/93
12/03/93
12/03/93
12/03/93
12/16/93
12/16/93
12/16/93
lost
12/16/93
12/17/93
12/17/93
12/16/93
12/16/93
12/16/93
12/08/93
12/08/93
12/08/93
12/03/93
12/03/93
12/16/93
12/16/93
12/16/93
12/16/93
12/16/93
12/16/93
Analysis hold time, days
12
12
12
12
12
13
13
13
13
13
17
17
17
17
17
15
15
15
15
15
15
14
14
14
20
20
20
15
15
23
23
23
23
23
9
42
6-5
-------
TABLE 6=3. VOC MEASUREMENT QAOs
Measurement parameter
Volatile organic contaminants
in feed, and residue samples
Volatile organic contaminants
in flue gas sampling trains
Measurement/
analytical method
Purge and trap
GC/FID
Method 0030 sampling,
GC/MS analysis
Reference Conditions %
SW-846 Methanol extract
Method 801SA of solid samples
SW-846 -
Methods 5040
and 8240A
Precision, Accuracy, Completeness,
USD or RPD % %
50 52 to 157* 70
70 52 to 157* 70
'Compound-specific criteria taken from Table 6, Method 8240A.
\
-------
TABLE 6-4. VOC MEASUREMENT MDLs: OBJECTIVES AND ACHIEVED LEVELS
MDL objective
Solid residues, mg/kg Aqueous liquids, ng/L, Flue gas, ng/dscm
Compound objective / achieved
Primary Target Analytes
Tetrachloroethene
1,1,2-Trichloroethane
Trichloroethene
Secondary Analytes
Acetone
Benzene
Bromodichloromethane
Carbon disulfide
Carbon tetrachloride
Chlorobenzene
Chlorodibromomethane
Chloroform
1,1-Dichlo'roethane
1,2-Dichloroethane
1,1-Dichloroethene
trans,l,2-Dichloroethene
1,2-Dichloropropane
cis-l,3-Dichloropropene
trans-l,3-Dichloropropene
Methylene chloride
Toluene
1,1,1-Trichloroethane
Trichlorofluoromethane
2/3.9
1/1
1/1
NA*
NA
NA
NA
NA
NA
NA
NA
NA
NA .
NA
NA
NA
NA
NA
NA
NA
NA
NA
objective / achieved
20 / 4.1
10 / 3.9
10 / 15.4
NA.
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA '
NA
NA
NA
NA
NA
objective / achieven
2 / 0.05
1 / 0.14
1 / 0.05
2 / 0.05
2/0.23
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.05
2 / 0.09
2/0.23
2 / 0.05
2 / 0.05
"NA = Not applicable; analyte not measured in this matrix.
MS/MSD VOST sample set (two pairs of VOST traps) was spiked with the full set of VOC
analytes listed in Table 3-7.
Table 6-5 summarizes VOC recoveries achieved from solid and liquid MS samples
analyzed by GC/FEX The data in Table 6-5 show 29 out of 30 measurements, or 97 percent,
were within the compound-specific recovery range. As the completeness QAO was 70 percent
6-7
-------
TABLE 6-5. VOC RECOVERIES FROM MS SAMPLES ANALYZED BY GC/FID
Spike recovery, %
Sample
Test Feed
Composite fluff MS
Composite fluff MSD
RPD, %
Test 3 soil MS
Test 3 soil MSD
RPD, %
Post-test Scrubber Liquor
Test 0 MS
Test 0 MSD
RPD, %
Kiln Ash
Test 3 MS
Test 3 MSD
RPD, %
Baghouse Ash
Test 3 MS
Test 3 MSD
RPD, %
Accuracy QAO
Tetrachloroethene
91.1
95.4
4.6
125
155
21.4
102
101
1.0
88.8
87.0
2.0
94.7
97.8
3.2
64-148
1,1,2-TrichIoroe thane
90.6
94.0
3.7
102
98.8
3.2
101
100
1.0
87.1
87,1
0
85.4
99.8
15.6
52-150
Trichloroethene
90.7
94.8
4.4
102
99.6
2.4
104
102
1.9
90.7
91.1
0.4
100
102
2.0
71-157
Precision
QAO, RPD
50
50
50
50
50
for this measurement, the accuracy QAO, as measured by spike recovery from MS/MSD
samples, was met.
The data in Table 6-5 also show that all 15 duplicate measurements were within the
precision QAO of 50 percent RPD. Thus, the VOC measurement precision QAO for the
GC/FID analyses, as measured by MS/MSD sample analyses, was met.
Table 6-6 summarizes the VOC spike recoveries from the VOST trap MS/MSD sample
analyses by GC/MS. The data in Table 6-6 show that 53 out of 61 measurements, or 87 percent,
were within the compound-specific recovery ranges. The completeness QAO for this
6-8
-------
TABLE 6-6. VOC RECOVERIES FROM MS SAMPLES
analytes Test 0
Trichloroethene 97
1,1,2-trichloroethane 51
Tetrachloroethene 85
Secondary analytes
Trichlorofluoromethane
1,1-Dichloroethene
Methylene chloride
trans- 1,2-Dichloroethene
1,1-Dichloroethane
Chloroform
1,2-Dichloroethane
1,1,1-Trichloroethane
Carbon tetrachloride
Benzene
Trichloroethene
1,2-Dichloropropane
Bromodichloromethane
cis-l,3-Dichloropropene
trans- 1,3-Dichloropropene
1,1,2-Trichloroethane
Dibromobhloromethane
Toluene
Tetrachloroethene
Chlorobenzene
Precision QAO, RPD
Testl
99
68
94
MS
82.6
922
97.6
882
75.0
71.8
87.8
66.8
72.6
97.4
762
80.4
84.6
78.2
812
72.6
78.6
87.6
71.0
77.2
^n tie A rpcfvv&'rv
W^IUW * VVUTCl. J]
Test 2 Test 3 Test
102 50 62
74 48 63
91 58 74
Spike recovery, %
MSD
69.4
88.8
1082
85.4
82.6
832
80.8
71.0
76.2
76.2
702
742
762
612
37.6
64.6
68.8
127
64.8
68.0
ANALYZED BY GC/MS
w
4 Test 6
66
52
51
QAO*
17-181
59-155
D-221
54-156
59-155
51-138
49-155
52-162
70-140
37.151
71-157
D-210
35-155
D-227
17-183
52-150
53-149
47-150
64-148
37-160
Test 6 QAO*
73 71-157
64 52-150
86 64-148
RPD, %
17.4
3.8
103
32
9.6
14.7 .
83
6.1
4.8
24.4
8.2
8.0
10.4
24.4
73.4
11.7
133
37.0
9.1
12.7
70
'Compound-specific criteria taken from Table 6, Method 8240A; D denotes detected.
measurement was 70 percent; therefore, the accuracy QAO, as measured by spike recovery, was
met. The data in Table 6-6 also show that 19 out of 20 RPD measurements, or 95 percent, were
within the precision QAO of 70 percent RPD. Therefore, the VOC measurement precision
QAO for the GC/MS analyses, as measured by MS/MSD sample analyses, was met.
6-9
-------
One sample from each of the fluff feed, soil feed, kiln ash, baghouse ash, and post-test
scrubber liquor matrices was analyzed in duplicate as a further check on measurement precision.
Neither of the kiln ash, baghouse ash, or scrubber liquor duplicate samples contained any
detectable volatile organic target analytes, so no precision information was obtained from these
analyses. Table 6-7 summarizes the duplicate sample analysis results for the two test feed
matrices. All precision measurements shown met the precision QAO of 50 percent RPD.
Table 6-8 summarizes the method surrogate recoveries achieved in the GC/FED analyses
of test samples. Table 6-9 presents an analogous summary for the GC/MS analyses. The data
in Table 6-8 show that 95 out of 100, or 95 percent, of the surrogate recoveries were within the
surrogate-specific accuracy QAO range. The data in Table 6-9 show that 105 out of 140, or
75 percent, of the surrogate recoveries were within the surrogate-specific accuracy QAO range.
Because the completeness QAO was 70 percent for this measurement, the accuracy QAO, as
measured by surrogate recovery, was met for both the GC/FID and the GC/MS analyses.
TABLE 6-7. DUPLICATE SAMPLE VOC ANALYSIS RESULTS
Concentration
Sample
Test Feed, mg/kg
Composite fluff
Tetrachloroethene
1, 1,2-Trichloroethane
Trichloroethene
Test 3 soil
Tetrachloroethene
1, 1,2-Trichloroethane
Trichloroethene
Precision QAO, RPD
Analysis
4.8
1.2
50
2.7
Duplicate analysis
<4
50
2.7
RPD,%
18
0
18
0
0
0
50
6-10
-------
TABLE 6-8. VOC SURROGATE RECOVERIES IN THE GC/FID ANALYSIS OF TEST
SAMPLES
Sample
Test Feed
TestO
Composite fluff
Composite fluff duplicate
Composite fluff MS
Composite fluff MSD
Testl
Test 2
TestS
Test 6
Test 3
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
Scrubber Liquor
Test 0 pretest
Test 0 post-test
Test 0 post-test duplicate
Test 0 post-test MS
Test 0 post-test MSD
Test 1 pretest
Test 1 post-test
Test 2 pretest
Test 2 post-test
Test 3 pretest
Test 3 post-test
Test 4 pretest
Test 4 post-test
Test 5 pretest
Test 5 post-test
Test 6 pretest
Test 6 post-test
Recovery QAO
Surrogate
1,1,1-
Trichloro-
ethane
97.5
93.6
672
81.9
82.1
86.4'
134
118
140
703
72.9
77.7
73.5
71.0
91.6
84.6
893
89.9
91.6
94.1
92.5
90.4
92.4
89.1
87.4
833
87.9
87.7
863
88.5
88.4
52-162
recovery, %
4-Bromo-
fluorobenzene
113
972
115
125
120
82.1
141
123,
150
85.2
85.7
87.0
90.7
94.5
105
96.7
101
103
106
104
106
103
109
102
100
93.0
100
101
97.9
103
100
74-121
Sample
Kiln Ash
Testl
Test 2
Test3
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
Test5
Test 6
Baghouse Ash
TestO
Testl
Test 2
Test3
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
TestS
Test 6
Recovery QAO
Surrogate
1,1,1-
Trichloro-
ethane
87.7
94.4
702
793
76.4
73.0
80.2
925
90.0
93.7
93.8
86.7
78.1
812
76.4
78.7
90.4
92.1
90.4
52-162
recovery, %
4-Bromo-
fluorobenzene
98.4
99.6
83.4
88.9
86.7
83.4
92.9
73.0
93.6
105
104
106
103
105
96.9
102
105
107
107
74-121
6-11
-------
TABLE 6-9. VOC SURROGATE RECOVERIES IN THE GC/MS ANALYSIS OF
METHOD 0030 SAMPLES
Surrogate recovery, %
Sample l,2-Dichloroethane-d4 Toluene-d8 Benzene-d«
TestO
Setl
Set 2
SetS
Field blank
MS
Testl
Set 1
Set 2
SetS
Field blank
MS
Test 2
Setl
Set 2
SetS
Field blank
MS
Tests
Setl
Set 2
SetS
Field blank
MS
Test 4
Setl
Set 2
SetS
Field blank
MS
Test 5
Setl
Set 2
SetS
Field blank
MS
Test 6
Setl
Set 2
SetS
Field blank
MS
Trip blank
Recovery QAO
98
98
99
96
101
128
128
115
111
119
20
104
100
108
104
175
256
134
126
128
127
131
131
128
118
126
108
98
111
128
122
123
131
121
135
70-121
90
88
89
98
97
84
88
93
104
98
80
121
105
98
106
90
90
98
102
97
97
98
101
103
88
85
97
97
105
98
100
100
100
105
103
81-117
84
89
64
65
57
96
96
98
100
99
96
107
130
116
119
118
127
108
Lo"t
107
109
109
108
108
108
91
94
88
110
132
110
106
105
108
113
105
74-121
4-Bromofl uorobenzene
92
61
61
62
45
90
65
85
84
76
152
94
93
80
109
168
204
86
75
72
83
56
94
82
49
48
53
76
68
101
57
62
64
94
46
74-121
6-12
-------
6.2 SVOC ANALYSES
A total of 101 samples was analyzed for SVOCs. Included in this group were 17 method
blanks, 1 field blank, 7 MS/MSD sample sets, 3 sets of duplicate test samples, and 6 sets of
replicate feed samples. Table 6-10 lists the sample collection date, extraction date, analysis date,
and analysis hold time for these samples. As shown in Table 6-10, 89 of 101 samples, or
88 percent were extracted within the specified method extraction hold time. The data also show
that all sample extracts were analyzed within the analysis hold time specified by the method.
Table 6-11 summarizes the SVOC measurement QAOs for precision, accuracy, and
completeness. Table 6-12 lists the MDL objectives and the levels achieved. As can be seen in
Table 6-12, the MDL objective was achieved for all of the analytes except 2-nitrophenol in flue
gas, a secondary analyte. SVOC measurement precision and accuracy were assessed by
preparing two MS/MSD sample sets for the test feed (one set for each feed type) and kiln ash
matrices, and one MS/MSD sample set for the baghouse ash, scrubber liquor, and Method 0010
train matrices. Table 6-13 summarizes the spike recovery data obtained for solid and liquid
samples. Table 6-14 presents an analogous summary for Method 0010 train samples.
The data in Table 6-13 show that all achieved spike recoveries were within the
compound-specific recovery objective ranges. Thus, the measurement accuracy QAO, as
measured by spike recovery from solid and liquid samples, was met. Table 6-13 also shows that
all 12 RPD measurements for MS/MSD analyses were within the precision QAO of 50 percent
RPD. Thus, the SVOC measurement precision QAO, as measured by solid and liquid MS/MSD
sample analyses, was also met.
The data in Table 6-14 show that all 112 spike recovery measurements from Method
0010 train samples were within the compound-specific recovery objective ranges! Thus, the
measurement accuracy QAO, as measured by spike recovery, was met. Table 6-14 also shows
6-13
-------
TABLE 6-10. SAMPLE HOLD TIMES FOR THE SVOC ANALYSES BY GC/MS
Sample
Test 1 Feed
Extract 1
Extract 2
Extract 3
Extract 4
Extract 5
MS
MSD
Test 2 Feed
Extract 1
Extract 2
Extract 3
Extract 4
Extract 5
Test 3 Feed
Extract 1
Extract 2
Extracts
Extract 4
Extracts
MS
MSD
Test 4 Feed
Extract 1
Extract 2
Extracts
Extract 4
Extract 5
Test 5 Feed
Extract 1
Extract 2
Extract 3
Extract 4
Extract 5
Method Requirement
Collection
date
10/14/93
10/14/93
10/14/93
10/14/93
10/14/93
10/15/93
10/15/93
10/15/93
10/15/93
10/15/93
10/15/93
10/15/93
10/20/93^
10/20/93
10/20/93
10/20/93
10/20/93
10/20/93
10/20/93
10/20/93
10/20/93
10/20/93
10/20/93
10/20/93
10/18/93
10/18/93
10/18/93
10/18/93
10/18/93
Extraction
date
10/26/93
10/26/93
10/26/93
10/26/93
10/26/93
11/05/93
11/05/93
10/27/93
10/27/93
10/27/93
10/27/93
10/27/93
11/04/93
11/04/93
11/04/93
11/04/93
11/04/93
11/05/93
11/05/93
11/03/93
11/03/93
11/03/93
11/03/93
11/03/93
10/28/93
10/28/93
10/28/93
10/28/93
10/28/93
Extraction
hold time,
days
12
12
12
12
12
21
21
12
12
12
12
12
15
15
15
15
15
16
16
14
14
14
14
14
10
10
10
10
10
14
Analysis
date
11/19/93
11/19/93
11/19/93
11/19/93
11/19/93
12/10/93
12/10/93
11/21/93
11/21/93
11/21/93
11/21/93
11/21/93
12/06/93
12/06/93
12/06/93
12/07/93
12/07/93
12/10/93
12/10/93
12/07/93
12/07/93
12/07/93
12/07/93
12/07/93
11/21/93
11/21/93
11/21/93
11/22/93
11/22/93
Analysis
hold time,
days
24
24
24
24
24
35
35
25
25
25
26
26
32
32
32
33
33
35
35
34
34
34
34
34
24
24
24
25
25
40
(continued)
6-14
-------
TABLE 6-10. (continued)
Sample
Test 6 Feed
Extract 1
Extract 2
Extract 3
Extract 4
Extract 5
Feed Packaging Container
Material (Test 0)
Sample 1
Sample 2
Feed Method Blanks
Blank 1
Blank 2
Blank3
Kiln Ash
Test 1
Test 2
Test 3
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
TestS
Test 6
Test 6 MS
Test 6 MSD
Baghouse Ash
TestO
Test 1
Test 2
Test 3
Test 3 duplicate
Test 4
TestS
Test 6
Test 6 MS
Test 6 MSD
Method Requirement
Collection
date
10/18/93
10/18/93
10/18/93
10/18/93
10/18/93
12/21/93
12/31/93
10/21/93
11/02/93
11/03/93
11/09/93
11/16/93
12/01/93
12/01/93
12/01/93
12/01/93
12/02/93
11/18/93
11/23/93
11/23/93
11/23/93
10/28/93
11/10/93
11/16/93
12/01/93
12/01/93
12/02/93
11/18/93
11/23/93
11/23/93
11/23/93
Extraction
date
10/29/93
10/29/93
10/29/93
10/29/93
10/29/93
01/05/94
01/05/94
10/22/93
11/03/93
11/04/93
11/16/93
11/18/93
12/03/93
12/08/93
12/07/93
12/07/93
12/08/93
11/24/93
12/01/93
12/09/93
12/09/93
11/09/93
11/16/93
11/18/93
12/03/93
12/08/93
12/08/93
11/24/93
12/01/93
12/07/93
12/07/93
Extraction
hold time,
days
11
11
11
11
11
15
5
1
1
1
7
2
2
7
6
6
6
6
8
15
15
12
6
2
2
7
6
6
8
14
14
14
Analysis
date
11/21/93
11/22/93
11/22/93
11/22/93
11/23/93
01/13/94
01/13/94
11/21/93
12/09/93
12/10/93
12/17/93
12/21/93
01/07/94
01/10/94
01/07/94
01/07/94
01/10/94
12/23/93
01/06/94
01/10/04
01/10/94
12/16/93
12/17/93
12/21/93
01/07/94
01/10/94
01/10/94
12/23/93
01/06/94
01/07/94
01/07/94
Analysis
hold time,
days
23
24
24
24
25
8
8
30
36
36
31
33
35
33
31
31
33
29
36
32
32
37
31
33
35
33
33
29
36
31
31 .
40
(continued)
6-15
-------
TABLE 6-10. (continued)
Sample
Ash Method Blanks
Blank 1
Blank 2
Blank 3
Blank 4
Blanks
Blank 6
Blank?
Blanks
Scrubber Liquor
Test 0 pretest
Test 0 post-test
Test 1 pretest
Test 1 post-test
Test 2 pretest
Test 2 post-test
Test 3 pretest
Test 3 post-test
Test 3 post-test duplicate
Test 4 pretest
Test 4 post-test
Test 4 MS
Test4MSD
Test 5 pretest
Test 5 post-test
Test 6 pretest
Test 6 post-test
Scrubber Liquor Method Blanks
Blank 1
Blank 2
Blank 3
Blank 4
Blanks
Method Requirement
Collection
date
11/08/93
11/15/93
11/17/93
11/23/93
11/30/93
12/02/93
12/07/93
12/08/93
10/27/93
10/27/93
11/09/93
11/09/93
11/16/93
11/16/93
12/01/93
12/01/93
12/01/93
12/02/93
12/02/93
12/02/93
12/02/93
11/18/93
11/18/93
11/23/93
11/23/93
11/01/93
11/15/93
11/22/93
11/29/93
12/09/93
Extraction
date
11/09/93
11/16/93
11/18/93
11/24/93
12/01/93
12/03/93
12/08/93
12/09/93
11/02/93
11/02/93
11/16/93
11/16/93
11/22/93
11/22/93
12/09/93
12/09/93
12/09/93
12/09/93
12/09/93
12/10/93
12/10/93
11/22/93
11/22/93
11/30/93
11/30/93
11/02/93
11/16/93
11/22/93
11/30/93
12/10/93
Extraction
hold time,
days
1
1
1
1
1
1
1
1
6
6
7
7
6
6
8
8
8
7
7
8
8
4
4
7
7
1
1
0
1
1
14
Analysis
date
12/10/93
12/21/93
12/21/93
12/23/93
01/06/94
01/07/94
01/10/94
01/10/94
12/09/93
12/09/93
12/17/93
12/17/93
12/21/93
12/21/93
01/11/94
01/11/94
01/11/94
01/11/94
01/11/94
01/11/94
01/11/94
12/23/93
12/23/93
12/23/93
12/23/93
12/09/93
12/21/93
12/23/93
12/23/93
01/11/94
Analysis
hold time,
days
31
35
33
29
36
34
32
31
37
37
31
31
29
29
33
33
33
33
33
32
32
31
31
23
23
37
35
31
23
31
40
(continued)
6-16
-------
TABLE 6-10. (continued)
Sample
Method 0010 Train
TestO
Test 1
Test 2
Test 3
Test 4
TestS
Test 6
Method blank
Held blank
Blank spike
Blank spike duplicate
Method Requirement
Collection
date
10/27/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
11/02/93
12/01/93
12/08/93
12/08/93
Extraction
date
10/28/93
11/10/93
11/17/93
12/02/93
12/03/93
11/19/93
11/24/93
11/03/93
12/02/93
12/09/93
12/09/93
Extraction
hold time,
days
1
1
1
1
1
1
1
1
1
1
1
14
Analysis
date
11/24/93
11/24/93
12/20/93
12/20/93
01/07/94
12/21/93
12/23/93
12/10/93
01/07/94
01/10/94
01/10/94
Analysis
hold time,
days
27
14
33
35
35
32
29
37
35
31
31
40
6-17
-------
o\
>-»
00
TABLE 6-ii. SVOC MEASUREMENT QAOs
Measurement/ Precision, Accuracy, Completeness,
Measurement parameter analytical method Reference Conditions % RSD or RPD % %
Semivolatile organic Extraction, SW-846 Methylene 50 D-262' 70
contaminants in feed, residue, concentration, Methods 0010, 3520A, chloride
and flue gas samples GC/MS 3540A, and 8270A extraction
'Compound-specific criteria taken from Table 6, Method 8270A.
-------
TABLE 6-12. SVOC MEASUREMENT MDLs: OBJECTIVES AND ACHIEVED LEVELS
MDL objective
Solid residues, mg/kg
Compound
Primary Target Analytes
Naphthalene
Bis(2-ethylhexyl)phthalate
Di-n-octylphthalate
Objective
2
2
2
Achieved
03
13
0.4
Aqueous liquids, /ig//L
Objective Achieved
20 3.1
20 13
20 3.8
Flue gas, pg/dscm
Compound
Secondary Analytes1
Phenol
Bis(2-chloroethyl)ether
2-Chlorophenol
13-Dichlorobenzene
1,4-Dichlorobenzene
1,2-Dichlorobenzene
Bis(2-chloroisopropyl)ether
N-nitroso-di-n-propylamine
Hexachloroethane
Nitrobenzene
Isophorone
2-Nitrophenol
2,4-Dimethylphenol
Bis(2-chloroethoxy)methane
2,4-Dichlorophenol
1,2,4-Trichlorobenzene
Hexachlorobutadiene
4-Chloro-3-methylphenol
2-Methylnaphthalene
2,4,6-Trichlorophenol
2,4,5-Trichlorophenol
2-Chloronaphthalene
Dimethylphthalate
Acenaphthylene
2,6-Dinitrotoluene
Acenaphthene
Objective
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
Achieved
4.5
13
7.1
1.5
. 1-8
13
1.0
1.6'
13
, 23
1.4
13.9
1.5
4.9
73
1.8
0.9
5.8
1.0
7.9
73
0.7
0.4
23
13
1.8
Compound
. Secondary Analytes"
2,4-Dinitrophenol
4-Nitrophenol
Dibenzofuran
2,4-Dinitrotoluene
Diethylphthalate
Huorene
4-Chlorophenylphenylether
4,6rDinitro-2-methylphenol
N-nitrosodiphenylamine
4-Bromophenylphenylether
Hexachlorobenzene
Pentachlorophenol
Phenanthrene
Anthracene
Di-n-butylphthalate
Ruoranthene
Pyrene
Butylbenzylphthalate
Benzo(a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Indeno(l,23-cd)pyrene
Dibenz(a,h)anthracene
Benzo(ghi)perylene
Flue gas,
Objective
10
10
10
Flue gas,
Objective
10
10
10
10
10
' 10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
Hg/dscta
Achieved
OS
33
12
pg/dscm
Achieved
33
2.5
2.1
3.9
1.7
13
1.5
2.8
43
0.7
0.6
1.7
0.7
0.8
53
0.4
13
6.7
0.5
0.7
0.7
0.8
0.7
12
13
0.9
Measurement not performed on solid and liquid matrices.
6-19
-------
TABLE 6-13. SVOC RECOVERIES FROM SOLID AND LIQUID MS SAMPLES
ANALYZED BY GC/MS
Sample
Test 1 Feed8
MS
MSD
RPD, %
Test 3 Feed"
MS
MSD
RPD,%
Test 3 Kiln Ash
MS
MSD
RPD, %
Test 6 Kiln Ash
MS
MSD
RPD,%
Test 6 Baghouse Ashc
MS
MSD
RPD, %
Test 4 Scrubber Liquor
MS
MSD
RPD, %
Accuracy QAO
Spike
Naphthalene
88.0
83.5
5.2
86.9
88.7
2.1
88.1
93.9
6.4
78.8
90.3
13.6
91.6
85.3
7.1
85.7
86.2
0.6
21-133
recovery, %
BEHP
NSb
NS
NS
NS
81.8
90.3
9.9
71.0
83.5
16.2
ISd
IS
74.0
59.9
21.1
8-158
DNOP Precision QAO, RPD
NS
NS
- 50
NS
NS
- 50
81.3
87.2
7.0 50
79.3
91.0
13.7 50
IS
IS
50
80.7
72.3
11.0 50
4-146
aThe amount of phthalates in the fluff and soil feed exceeded 1 percent therefore spiking
was not required.
bNS = Not spiked.
cThe phthalate spiking levels were insignificant compared to the native amount found in
the baghouse ash.
IS = Insufficient spike.
6-20
-------
TABLE 6-14. SVOC RECOVERIES FROM THE METHOD 0010 MS SAMPLES
ANALYZED BY GC/MS
Spike recovery, %
Compound
Phenol
Bis(2-chloroethyl)ether
2-Chlorophenol
1,3-Dichlorobenzene
1,4-Dichlorobenzene
1,2-Dichlorobenzene
Bis(2-chloroisopropyl)ether
N-Nitroso-di-n-propylamine
Hexachloroethane
Nitrobenzene
Isophorone
2-Nitrophenol
2,4-Dimethylphenol
Bis(2-chloroethoxy)methane
2,4-Dichlorophenol
1,2,4-Trichlorobenzene
Naphthalene
Hexachlorobutadiene
4-Chloro-3-methylphenol
2-Methylnaphthalene
2,4,6-Trichlorophenol
2,4,5-Trichlorophenol
2-Chloronapthalene
Dimethylphthalate
Acenapthylene
2,6-Dinitrotoluene
Acenaphthene
2,4-Dinitrophenol
4-Nitrophenol
Dibenzofuran
2,4-Dinitrotoluene
Diethylphthalate
Fluorene
4-Chlorophenylphenylether
4,6-Dinitro-2-methylphenol
Precision QAO, RPD
MS
75.6
84.6
83.5
84.4
87.0
83.7
70.2
89.2
84.5
89.3
86.8
88.5
37.2
84.3
87.3
95.2
90.2
96.3
93.2
88.4
87.2
95.8
85.2
85.7
80.7
89.7
89.5
64.1
80.9
83.5
89.3
84.5
82.1
88.2
69.4
MSD
82.3
88.2
88.2
85.3
87.8
90.4
74.9
96.6
82.3
88.9
88.9
90.0
52.8
87.5
93.5
92.1
87.8
95.1
102
91.6
103
101
93.6
96.3
88.6
101
95.1
87.2
91.5
94.0
103
94.8
91.7
98.3
87.5
QAO
5-112
12-158
23-134
D-172
20-124
32-129
36-166
D-230
40-113
35-180
21-196
29-182
32-119
33-184
39-135
44-142
21-133
24-116
22-147
21-133
37-144
37-144
60-118
D-112
33-145
50-158
47-145
D-191
D-132
27-133
39-139
D-114
59-121
25-158
D-181
RPD
8.5
4.2
5.5
1.1
0.9
7.7
6.5
8.0
2.6
0.5
2.4
1.7
34.7
3.7
6.9
3.3
2.7
1.3
9.0
3.6
16.6
5.3
9.4
11.7
9.3
11.9
6.0
30.5
12.3
1.8
14.3
11.5
11.1
10.8
23.1
50
6-21
(continued)
-------
TABLE 6-14. (continued)
Spike recovery, %
Compound
N-Nitrosodiphenylamine
4-Bromophenylphenylether
Hexachlorobenzene
Pentachlorophenol
Phenanthrene
Anthracene
Di-n-butylphthalate
Fluoranthene
Pyrene
Butylbenzylphthalate
Benzo(a)anthracene
3,3-Dichlorobenzidine
Chrysene
Bis(2-ethylhexyl)phthalate
Di-n-octylphthalate
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Indeno(l,2,3-cd)pyrene
Dibenzo(a,h)anthracene
Benzo(g,h,i)perylene
Precision QAO, RPD
MS
86.0
97.0
103
104
91.2
89.4
89.7
92.2
82.2
76.9
86.3
79.6
87.0
86.8
82.6
85.5
80.4
79.4
49.6
82.2
83.4
MSD
93.8
106
109
114
97.5
96.4
95.4
96.7
90.6
82.6
94.9
94.6
96.2
93.0
91.7
94.5
87.6
84.8
83.8
80.9
82.7
QAO
D-230
53-127
D-152
14-176
54-120
27-133
1-118
26-137
52-115
D-152
33-143
D-262
17-168
8-158
4-146
24-159
11-162
17-163
D-171
D-227
D-219
RPD
8.7
8.9
5.7
9.2
6.7
7.5
6.2
4.8
9.7
7.2
9.5
17.2
10.0
6.9
10.4
10.0
8.6
6.8
51.3
1.6
0.8
50
that 55 of 56 RPD determinations from MS/MSD sample analyses, or 98 percent, were within
the precision QAO of 50 percent RPD. As the completeness QAO for this measurement was
70 percent, the precision QAO for the Method 0010 train SVOC analyses, as measured by the
RPD of MS/MSD sample analyses, was met.
All samples extracted for SVOC analyses were spiked with method surrogates prior to
extraction, and surrogate recoveries were measured. Table 6-15 summarizes the surrogate
recoveries achieved for solid and liquid samples. Table 6-16 provides an analogous summary for
flue gas samples. The data in Table 6-15 show that 154 out of 159 surrogate recovery
6-22
-------
TABLE 6-15. SVOC SURROGATE RECOVERIES IN THE GC/MS ANALYSIS OF SOLID
AND LIQUID SAMPLES
Surrogate recovery, %
Sample
Feed Packaging Container Material
Sample 1
Sample 2
Kiln Ash
Testl
Test 2
TestS
Test 3 duplicate
Test 3 MS
Test 3 MSD
Test 4
TestS
Test 6
Test 6 MS
Test 6 MSD
Baghouse Ash
Test 0
Testl
Test 2
Test 3
Test 3 duplicate
Test 4
Test 5
Test 6
Test 6 MS
Test 6 MSD
Ash Method Blanks
Blank 1
Blank 2
Blank3
Blank 4
Blanks
Blank 6
Blank?
Blanks
Solid Sample Recovery QAO*
Nitrobenzene-dj
79
73
72
77
85
74
83
90
89
74
81
72
82
85
81
80
127
79
81
82
89
87
81
78
80
88
76
72
90
78
74
23-120
2-Fluorobiphenyl
71
67
77
83
80
76
79
84
92
75
83
77
79
85
82
85
112
78
80
87
84
79
73
82
85
91
78
73
85
83
67
30-115
4-Terphenyl-d14
100
116
82
94
84
79
77
86
92
76
86
75
84
95
88
91
120
81
81
94
86
93
77
86
95
98
95
84
89
82
78
18-137
*Compound-specific criteria taken from Table 8 of Method 8270A.
6-23
(continued)
-------
TABLE 6-15. (continued)
Sample
Scrubber Liquor
Test 0 pretest
Test 0 post-test
Test 1 pretest
Test 1 post-test
Test 2 pretest
Test 2 post-test
Test 3 pretest
Test 3 post-test
Test 3 post-test duplicate
Test 4 pretest
Test 4 post-test
Test 4 post-test MS
Test 4 post-test MSD
Test 5 pretest
Test 5 post-test
Test 6 pretest
Test 6 post-test
Scrubber Liquor Method Blanks
Blank 1
Blank 2
Blanks
Blank 4
Blanks
Liquid Sample Recovery QAO"
Nitrobenzene-dj
76
74
20
79
75
67
65
68
84
80
67
82
82
72
55
84
74
79
77
79
84
82
35-114
Surrogate recovery, 9
2-Fluorobiphenyl
63
69
19
89
74
69
71
68
79
81
71
83
82
72
66
73
63
83
76
76
81
81
43-116
fe
4-Terphenyl-dM
82
84
25
108
97
89
84
83
86
82
83
83
82
89
92
95
86
85
96
93
91
79
33-141
"Compound-specific criteria taken from Table 8 of Method 8270A.
6-24
-------
K
TABLE 6-16. SVOC SURROGATE RECOVERIES IN THE GC/MS ANALYSIS OF METHOD 0010 FLUE GAS SAMPLES
Surrogate recovery, %
Sample
TestO
Testl
Test 2
Test3
Test 4
TestS
Test 6
Method blank
Field blank
Blank spike
Blank spike duplicate
Recovery QAO
2-Fluoro-
phenol
57
36
40
74
74
66
70
71
69
84
88
21-100
Phenol-d<
43
25
35
75
75
57
64
73
70
89
95
10-94
Nitro-
benzene-d$
76
72
81
90
90
86
76
69
86
120
121
35-114
2-Fluoro-
biphenyl
76
64
82
89
79
87
74
71
82
106
115
43-116
2,4,6-Tribromo-
phenol
80
61
78
85
78
83
84
92
84
119
' 125
10-123
4-Terphenyl-d,,
78
69
91
93
83
101
83
78
83
108
118
33-141
Octafluoro-
biphenyl
87
73
55
103
98
95
102
NS'
NS
NS
NS
30-115*
9-PhenyI-
anthracene
86
84
106
115
110
102
96
NS
NS
NS
NS
18-137*
-S=S=S==
NS = Not spiked.
"Recovery QAO the same as for 2-fluorobiphenyl.
"Recovery QAO the same as for 4-terphenyl-d14.
-------
measurements, or 97 percent, were within the surrogate-specific recovery objective range.
Because the completeness QAO was 70 percent for this measurement, the accuracy QAO, as
measured by surrogate recovery, was met.for solid and liquid samples.
Table 6-16 summarizes surrogate recoveries achieved for flue gas samples. The data in
Table 6-16 show that 76 out of 80 surrogate recovery measurements, or 95 percent, were within
the surrogate-specific recovery objective range. Again, because the completeness QAO for this
measurement was 70 percent, the accuracy QAO, as measured by surrogate recovery from the
flue gas samples, was met.
One kiln ash, one baghouse ash, and one post-test scrubber liquor sample were analyzed
in duplicate as a further measure of analysis precision. The target SVOC analytes were not
detected in either duplicate kiln ash or baghouse ash sample, so no precision information was
obtained via this procedure. Both BEHP and DNOP were found in both duplicate baghouse ash
samples. The RPDs from the duplicate analyses were 37 percent for BEHP and 47 percent for
DNOP. Both measurements met the precision QAO of 50 percent RPD.
As discussed in Section 4, five replicates of each fluff waste sample were analyzed for
BEHP. The percent RSDs of the five analyses ranged from 6 to 25 percent, all within the
precision QAO of 50 percent RSD. In addition, five replicates of each soil feed sample were
analyzed for BEHP, DNOP, and naphthalene. Naphthalene was not detected in any soil feed
replicate analysis at an MDL of 25 mg/kg. The percent RSDs of the replicate sample analyses
were 33 and 28 percent, for BEHP, and 49 and 30 percent, for DNOP. All met the precision
QAO for the measurement of 50 percent RSD.
63 TRACE METAL ANALYSES
A total of 139 samples was analyzed by ICAP using Method 6010A. Included in this
number were 3 method blanks, 46 sample duplicates or replicates, and 9 MS/MSD sample sets.
6-26
-------
Table 6-17 summarizes the sample collection and analysis dates for these samples. As shown in
Table 6-17, all trace metal analyses were completed within the method-required hold time of
180 days.
Table 6-18 summarizes trace metal measurement QAOs for precision, accuracy, and
completeness. Table 6-19 shows the MDL objectives and the achieved values for the trace metal
analyses. As can be seen in Table 6-19, the MDL objective was met for all metals with the
exception of zinc. The zinc MDL was achieved for solid residues but not aqueous liquid or flue
gas matrices. ,
Three method blanks were analyzed for trace metals. Included in this group were one
TCLP extraction fluid blank and the front half and back half of a multiple metals train field
blank. Analysis results are shown in Table 6-20.
Measurement precision was assessed by performing duplicate or replicate sample
analyses. Table 6-21 summarizes the results of these analyses. The data in Table 6-21 show that
103 out of 143 precision calculations performed, or 72 percent, were within the precision QAO
of 25 percent RSD or RPD. As the completeness QAO was 70 percent for this measurement,
the precision QAO, as measured by duplicate or replicate sample analyses, was met.
Trace metal measurement accuracy was assessed by preparing and analyzing MS/MSD
samples. The MS/MSD sample analysis results are given in Table 6-22. The data in Table 6-22
show that only 79 out of 168 measurements, or 47 percent, were within the accuracy QAO range
of 70 to 130 percent recovery. Antimony, barium, and silver recoveries were particularly poor.
The reason for poor antimony recoveries likely lay with the digestion method used. The method
employed, heated HNO3/HF for solid samples and heated HNO3 for aqueous liquid samples,
may have caused evaporative loss of the relatively volatile antimony. The poor silver recoveries
may have been caused by the presence of chlorides in test program samples. The data in
6-27
-------
TABLE 6-17. SAMPLE HOLD TIMES FOR TRACE METAL ANALYSES BY ICAP
Collection/
Sample preparation date*
Test Feed
TestO
Test 1"
Test 2"
TestS"
Test 6"
Composite soil" (Tests 3 and 4)
Kiln Ash
Test 1"
Test 2b
Test 3C
Test4e
TestS"
Test6b
Baghouse Ash
Test 0
Test 1
Test 2d
Test 3
Test 4
TestS
Test 6
Scrubber Liquor
Test 0 pretest
Test 0 post-test
Test 1 pretest
Test 1 post-test"
Test 2 pretest
Test 2 post-test
Test 3 pretest
Test 3 post-test
Test 4 pretest
Test 4 post-test
Test 5 pretest
Test 5 post-test
Test 6 pretest
Test 6 post-test
Method Requirement
"Preparation date corresponds to TCLP leachates.
01/04/94
10/14/93
10/15/93
10/18/93
10/18/93
10/20/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
10/28/93
11/10/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
10/27/93
10/27/93
11/09/93
11/09/93
11/16/93
11/16/93
12/01/93
12/01/93
12/02/93
12/02/93
11/18/93
11/18/93
11/23/93
11/23/93
Analysis hold time,
Analysis date days
01/18/94
12/09/93
12/09/93
12/09/93
12/09/93
12/09/93
12/09/93
12/14/93
01/03/94
01/03/94
12/14/93
12/14/93
12/09/93
12/09/93
12/17/93
12/23/93
12/23/93
12/17/93
12/17/93
12/09/93
12/09/93
12/09/93
12/09/93
12/14/93
12/14/93
12/23/93
12/23/93
12/23/93
12/23/93
12/14/93
12/14/93
12/14/93
12/14/93
14
56
55
52
52
50
30
28
33
32
26
21
42
29
31
22
21
29
24
43
43
30
30
28
28
22
- 22
21
21
28 ,
28
21
21
180
(continued)
- . . nalyzed.
Tour split samples were prepared and analyzed.
i split samples were prepared and analyzed.
6-28
-------
TABLE 6-17. (continued)
Collection/
Sample preparation date*
Multiple Metals Train (front half)
Test 0
Test 1
Test 2
TestS
Test 4
TestS
Test 6
Multiple Metals Train (back half)
Test 0
Test 1
Test 2
TestS
Test 4
Test 5
Test 6
TCLP Leachates:
Test Feed
Test 1
Test 2
TestS
Test 6
Composite soil (Tests 3 and 4)
Kiln Ash
Test 1
t
Test 2
TestS"
Test 4
Test 5
Test 6
Method Requirement
"Preparation date corresponds to TCLP leachates.
10/27/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
10/27/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
10/14/93
10/15/93
10/18/93
10/18/93
10/20/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
Analysis hold time,
Analysis date
12/09/93
12/09/93
12/17/93
12/23/93
12/23/93
12/17/93
12/27/93
12/09/93
12/09/93
12/14/93
12/23/93
12/23/93
12/14/93
12/17/93
12/14/93
12/14/93
12/14/93
12/14/93
12/14/93
12/09/93
12/23/93
01/18/94
01/18/94
12/23/93
12/23/93
days
43
30
31
22
21
29
24 ,
43
30
28
22
21
26
24
61
60
57
57
55
30
39
48
47
35
30
180
(continued)
6-29
-------
TABLE 6-17. (continued)
Collection/
Sample preparation date*
TCLP Leachates (continued):
Baghouse Ash
Test 0
Test 1
Test 2
TestS
Test 4d
TestS
Test 6
Post-test Scrubber Liquor
TestO
Test 1
Test 2
Test 3
Test 4
TestS
Test 6
Blanks
Multiple metals train field blank front half
Multiple metals train field blank back half
TCLP extraction fluid
Spikes:
Test Feed
Test 1 MS
Test 1 MSB
Composite soil MS
Composite soil MSD
Kiln Ash
Test 1 MS
Test 1 MSD
Baghouse Ash
Test 1 MS
Test 1 MSD
Method Requirement
'Preparation date corresponds to TCLP leachates.
10/28/93
11/10/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
10/27/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
12/07/93
12/07/93
12/30/93
10/14/93
10/14/93
10/20/93
10/20/93
11/09/93
11/09/93
11/10/93
11/10/93
Analysis hold time,
Analysis date days
12/09/93
12/09/93
12/23/93
01/18/94
01/18/94
12/23/93
12/23/93
12/14/93
12/14/93
12/23/93
01/18/94
01/18/94
12/23/93
12/23/93
01/18/94
01/18/94
01/18/94
01/26/94
01/26/94
01/18/94
01/18/94
01/18/94
01/18/94
01/18/93
01/18/93
42
29
37
48
47
35
30
48
35
37
48
47
35
30
42
42
19
c
104
104
98
98
70
70
69
69
180
(continued)
6-30
-------
TABLE 6-17. (continued)
Sample
Spikes (continued):
Scrubber Liquor
Test 6 MS
Test6MSD
Multiple Metals Train (front half)
Blank spike MS
Blank spike MSD
Multiple Metals Train (back half)
Blank spike MS
Black spike MSD
TCLP Leachates:
Kiln Ash
Test 3 MS
Test 3 MSD
Baghouse Ash
Test 3 MS
Test 3 MSD
Method Requirement
Collection/ Analysis hold time,
preparation date* Analysis date days
11/23/93
11/23/93
01/11/94
01/11/94
01/11/94
01/11/94
12/01/93
12/01/93
12/01/93
12/01/93
01/18/94
01/18/94
01/18/94
01/18/94
01/18/94
01/18/94
01/18/94
01/18/94
01/18/94
01/18/94
56
56
7
7
7
7
48
48
48
48
180
Preparation date corresponds to TCLP leachates.
6-31
-------
TABLE 6-18. TRACE METAL MEASUREMENT QAOs
Measurement
parameter
Trace metals in solid
samples
Trace metals in
Method Reference
ICAP BIF methods, SW-846
Method 6010A
ICAP BIF methods, SW-846
Conditions %
Microwave digestion
by BIF methods
Conventional digestion
Precision, Accuracy, Completeness,
iRSDorRPD % %
25
25
70-130 70
70-130 70
aqueous liquid samples
Method 6010A by BIF methods
TABLE 6-19. TRACE METAL MEASUREMENT MDLs; OBJECTIVES AND ACHIEVED LEVELS
MDL objective
Measurement
parameter
Antimony
Arsenic
Barium
Cadmium
Chromium
Copper
Lead
Nickel
Silver
Zinc
Solid residues, mg/kg
objective / achieved
10 / 0.01
10 / 0.01
1 / 0.01
2 / 0.003
5 / 0.01
5 / 0.002
10 / 0.005
5 / 0.0049
5 / 0.0004
1 / 0.26
Aqueous liquids, ng/L
objective / achieved
100 / 30
100 / 50
10/3
20/4
50/7
50/23
100 / 77
50/10
50/7
10/25
Flue gas, /tg/dscm
objective / achieved
50 / 8.5
50 / 12.1
5/3.6
10 / 0.8
30/4.4
30 / 4.5
50 / 15.4
30 / 3.3
30 / 1.4
5 / 12.6
-------
TABLE 6-20. TRACE METAL ANALYSES OF METHOD BLANK SAMPLES
Concentration
Sample
TCLP extraction fluid, mg/L
Multiple metals tram field blank
Front half, mg
Back half, mg/L
Sb
<0.03
<0.01
<0.03
As
<0.05
<0.01
<0.05
Ba
0.56
0.010
0.0030
Cd
<0.004
< 0.0003
< 0.004
Cr
<0.007
0.010
<0.007
Cu
0.11
0.0023
0,023
Pb
0.87
<0.005
0.077
Ni
0.045
0.0049
<0.01
Ag
<0.007
< 0.0004
<0.007
Zn
98
0.026
0.025
o\
-------
TABLE 6-21. REPLICATE TRACE METAL SAMPLE ANALYSIS RESULTS
o\
Concentration
Sample
Test Feed:
Testl
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
RSD, %
Test 2
Sample
Replicate 1
. Replicate 2
Replicate 3
Replicate 4
RSD, %
Test 5
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
RSD, %
- = RSD, RPD not calculated.
Sb
62
200
110
94
110
45
290
190
130
140
130
39
98
80
91
120
63
23
As
48
<20
<20
<20
<20
*
<20
<20
<20
<20
<20
0
<20
<20
<20
<20
<20
0
Ba
43
87
120
75
47
42
76
44
72
70
90
24
52
50
48
37
48
12
Cd
2.0
2.2
<0.5
0.9
1.2
53
1.3
1.4
1.5
2.2
1.1
28
1.5
1.3
1.4
<0.5
1.8
37
Cr
27
32
31
40
40
17
37
36
45
34
38
11
33
23
32
21
27
2Q
Cu
8,800
9,000
13,000
8,400
5,000
32
8,200 *
7,100
8,900
8,000
9,800
12
7,600
28,000
9,800
7,600
9,000
71
Pb
1,300
2,400
1,600
2,800
3,800
42
3,000
1,400
5,100
1,300
1,200
70
1,200
1,100
1,100
980
1,000
8
Ni
5.2
4.5
<3.0
5.1
<3.0
26
<3.0
3.7
<3.0
4.3
<3.0
17
<3
<3
<3
<3
<3
0
Ag
<0.7
1.2
<0.7
1.1
<0.7
28
1.3
<0.7
2.6
1.0
<0.7
63
<0.7
1.2
<0.7
1.4
2.1
48
Zn
95
120
100
100
96
10
110
130
310
240
120
49
150
140
150
110
140
12
Precision
QAO
25
25
25
(continued)
-------
TABLE 6-21. (continued)
Concentration
Sample
Test Feed (continued):
Test 6
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
RSD,%
Composite Soil (Tests 3 and 4)
Sample
Replicate 1
Replicate 2
ReplicateS
Replicate 4
RSD, %
Kiln Ash:
Testl
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
RSD, %
' = RSD, RPD not calculated.
Sb
66
86
75
92
200
53
75
66
87
52
48
25
1,100
1,100
1,200
1,100
1,200
5
As
<20
<20
<20
<20
<20
0
<20
<20
<20
<20
<20
0
42
<20
<20
<20
, <20
Ba
110
42
56
100
98
37
66
69
76
80
67
9
280
260
270
230
290
9
Cd
<0.5
<0.5
1.5
1.1
1.3
47
1.5
1.2
1.4
1.6
0.9
21
<0.5
<0.5
<0.5
<0.5
<0.5
0
Cr
21
23
23
27
26
10
70
73
130
83
68
31
360
390
400
350
440
9
Cu
8,300
7,900
7,700
9,500
15,000
32
12,000
14,000
26,000
11,000
7,400
50
130,000
200,000
240,000
210,000
150,000
24
Pb
980
800
900
970
840
9
4,200
2,300
3,800
2,500
2,900
26
3,000
2,600
3,100
3,100
3,000
7
Ni
<3.0
9.0
<3.0
<3.0
5.1
57
19
27
46
28
24
36
,
230
280
250
220
410
28
Ag
3.6
<0.7
<0.7
<0.7
<0.7
«*
1.4
1.8
2.3
1.6
<0.7
38
1.9
1.3
1.6
1.7
2.0
16
Zn
130
120
150
120
89
!8
170
210
210
220
130
20
180
180
200
190
190
4
Precision
QAO
25
25
25'
(continued)
-------
TABLE 6-21. (continued)
Concentration
Sample
Kiln Ash (continued):
Test 2
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
RSD, %
Test 3
Sample
o\ _. ..
^ Replicate 1
<* Replicate 2
Replicate 3
RSD, %
Test 4
Sample
Replicate 1
Replicate 2
Replicate 3
RSD,%
Sb
880
870
1,000
930
1,000
7
180
200
180
190
5
190
190
190
200
3
As
<20
<20
<20
63
33
60
<20
<20
<20
<20
0
<20
<20
<20
<20
0
Ba
240
170
210
220
240
13
120
99
150
140
18
120
98
72
95
20
Cd
0.6
<0.5
<0.5
0.6
<0.5
10
<0.5
<0.5
<0.5
<0.5
0
<0.5
<0.5
<0.5
<0.5
0
Cr
370
430
600
410
600
23
67
66
79
70
8
41
60
56
50
16
Cu
83,000
190,000
150,000
99,000
190,000
35
46,000
69,000
32,000
67,000
33
18,000
21,000
67,000
50,000
60
Pb
3,600
3,300
3,800
3,600
4,500
12
4,000
4,300
4,400
3,800
7
4,000
4,000
3,700
4,000
4
Ni
320
750
1,300
450
1,400
58
65
59
66
70
7
42
60
56
48
16
Ag
3.0
4.8
3.9
3.5
7.0
35
2.1
15
1.7
13
21
1.7
1.8
2.3
2.2
15
Zn
220
270
290
270
260
10
320
350
340
310
6
290
300
300
300
2
W> "
Precision
QAO
25
25
25
« (continued)
-------
TABLE 6-21. (continued)
Concentration
Sample
Kiln Ash (continued):
TestS
Sample
Replicate 1
Replicate 2
Replicate 3
Replicate 4
RSD,%
Test 6
Sample
o\ Replicate 1
53 Replicate 2
Replicate 3
Replicate 4
RSD%
Baghouse Ash
Test 2 sample
Duplicate
RPD, %
Post-test Scrubber Liquor
Test 1 sample
Duplicate
RPD,%
= RSD, RPD not calculated.
Sb
1,000
980
790
1,000
1,000
10
1,100
820
940
890
1,000
13
400
340
16
0.47
0.65
32
As
<20
<20
<20
<20
<20
0
<20
<20
<20
120
48
95
<20
20
0.12
<0.05
Ba
270
290
140
240
240
24
270
210
270
220
270
12
-22
20
10
2.4
5.3
75
Cd
<0.5
0.8
<0.5
<0.5
0.6
22
1.0
<0.5
<0.5
<0.5
<0.5
*
18
17
6
0.20
0.25
22
Cr
470
480
500
440
420
7
550
520
520
570
510
5
320
310
3
1.9
2.9
42
Cu
110,000
110,000
85,000
160,000
110,000
24
170,000
180,000
170,000
190,000
170,000
5
14,000
14,000
0
210
230
9
Pb
5,500
5,800
6,000
5,600
5,600
4
5,700
5,600
7,100
5,500
5,800
11
19,000
44,000
79
780
900
14
Ni
160
140
140
160
140
7
350
330
360
640
310
34
130
110
17
1.2
1.7
35
Ag
5.0
2.4
2.6
2.4
1.0
54
23
3.6
2.3
5.6
2.7
48
<0.7
1.0
0.072
0.094
25
Zn
=====
250
250
180
260
260
14
280
260
240
230
250
8
2,100
2,100
0
19
23
19
. , , asseg
n *
Precision
QAO
===================
25
25
25
25
(continued1)
-------
TABLE 6-21. (continued)
Concentration
Sample
TCLP Leachate
Test 3 kiln ash sample
Duplicate
RPD, %
Test 4 sample
Duplicate
RPD, %
Sb
<0.2
<0.2
0
0.80
0.84
5
As
<0.2
<0.2
0
0.26
0.21
21
Ba
0.26
0.26
0
0.22
0.22
0
Cd
< 0.005
<0.005
o
1.7
1.8
6
Cr
0.046
0.044
4
0.27
0.30
11
Cu
0.28
0.22
24
640
650
2
Pb Ni
<0.1 <0.01
<0.1 <0.01
0 0
5,700 3.2
5,800 3.3
2 3
Ag
<0.007
<0.007
0
0.027
0.028
4
Zn
1.2
1.3
8
97
100
3
Precision
QAO
25
25
00
-------
TABLE 6-22. TRACE METAL RECOVERIES FROM MS SAMPLES ANALYZED BY ICAP
% recovery
Sample
Test 1 Fluff Feed
MS
MSD
RPD, %
Test 3 and 4 Soil Feed
MS
MSD
RPD, %
Test 1 Kiln Ash
o\
MS
*° MSD
RPD, %
Test 1 Baghouse Ash
MS
MSD
RPD, %
Test 6 Scrubber Liquor
MS
MSD
RPD, %
Sb
=====
17
0
200
40
103
88
62
16
118
52
95
59
0
0
0
As
65
68
5
66
38
54
56
72
25
66
>134
79
79
0
Ba
63
27
80
910
4
198
0
0
0
17
37
74
46
54
16
Cd
195
81
83
76
61
22
75
90
18
60
64
6
67
61
9
Cr
92
85
8
100
68
38
64
65
2
50
44
13
82
71
14
==
Cu
i in sza
NS'
NS
_b
NS
NS
NS
NS
NS
NS
112
112
0
5
Pb
.. . ,SS
30
57
62
87
63
32
19
4
130
NS
NS
99
63
44
X
Ni
5
9
8
12
61
63
3
84
80
5
44
42
5
75
69
8
=====
Ag
9
2
127
5
35
150
13
0
200
%
0
46
89
64
Zn Accuracy/precision QAO
108
94
14
63
50
23
95
70
30
53
44
19
71
234
107
70-130
70-130
25
70-130
70-130
25
70-130
70-130
25
70-130
70-130
25
70-130
70-130
25
NS = Not spiked.
b = RPD not calculated.
(continued)
-------
TABLE 6-22. (continued)
% recovery
Sample
Multiple Metals Train Blank Spike
Back half
MS
MSD
RPD, %
Front half
MS
MSD
RPD, %
£ Test 3 Kiln Ash TCLP Leachate
o
MS
MSD
Sb As
117 85
100 90
15 6
<10 - 68
<10 71
0 4
<10 80
<10 85
Ba
88
85
3
17
0
200
73
77
Cd
84
84
0
97
77
23
85
85
Cr
91
91
0
12
8
40
75
73
Cu
102
102
0
108
85
24
119
94
Pb
109
101
8
85
70
19
120
109
Ni
80
79
1
100
36
94
69
66
Ag
72
46
44
90
160
45
43
Zn Accuracy/precision QAO
131
131
0
95
47
68
ISC
IS
70-130
70-130
25
70-130
70-130
25
70-130
70-130
RPD, %
Test 3 Baghouse Ash TCLP
Leachate
23
10
5 -"
b = RPD not calculated.
IS = Spiked amount not significant compared to native sample amount.
25
MS
MSD
RPD, %
0
0
0
58
78
29
42
83
66
83
78
6
39
44
12
105
109
4
73
62
16
86
84
2
178
228
25
111
115
4
70-130
70-130
25
-------
Section 4.1 show that both test feed material matrices contained significant amounts of chlorine.
Thus, test program samples used to prepare the MS/MSD samples may have contained chlorine
in the form of chlorides. The presence of chlorides will definitely interfere with the sample
digestion method employed. The reason for the poor barium recoveries is not clear.
If antimony, barium, and silver are removed from consideration, then 67 out of 114
other metal spike recovery measurements, or 59 percent, fell within the accuracy QAO range of
70 to 130 percent recovery. This still fails the completeness objective of 70 percent. However,
had the accuracy QAO range instead been a slightly relaxed 60 to 140 percent recovery, then 89
of 114 other metal (antimony, barium, and silver excluded) recovery measurements, or
78 percent, would have been acceptable, a 70 percent completeness objective at this relaxes
accuracy QAO range would have been met.
Trace measurement precision was-also measured by calculating the RPD of each pair
of MS/MSD measurements. The data in Table 6-22 show that 55 out of 84 RPDs, or 65 percent,
met the precision QAO of 25 percent RPD. However, again, the precision measures for
antimony, barium, and silver were particularly poor. If these three metals are excluded, then 43
of the remaining 57 RPD determinations, or 75 percent, met the precision QAO of 25 percent
RPD. This would have satisfied the completeness objective of 70 percent.
Based on both the precision and accuracy checks employing MS/MSD sample analyses,
test program results for antimony, barium, and silver appear to have been compromised, and the
reported data should be treated with caution. Test program conclusions regarding the
concentrations of these three metals in incinerator discharges, and their distributions among
these discharges, must be viewed as tentative at best.
6-41
-------
6.4 CHLORIDE ANALYSES
A total of 17 samples was analyzed for chloride ion to support flue gas HC1
concentration measurements. Included in this number were 1 method blank and 1 MS/MSD
sample set. Table 6-23 lists the sample collection and analysis dates and the analysis hold times
for these samples. As the data in Table 6-23 show, all 17 samples were analyzed within the
method required hold time limit of 28 days.
Table 6-24 summarizes the flue gas chloride measurement precision, accuracy, and
completeness QAOs. The MDL objective for the measurement was 100 jzg/dscm. This objective
was met with an achieved MDL of 49 /ig/dscm.
Table 6-25 shows that the chloride recoveries for the MS/MSD sample set were both
within the accuracy QAO range of 75 to 125 percent recovery. Table 6-25 also shows that the
RPD of the MS/MSD sample set was within the precision QAO of 30 percent RPD. Thus, both
the accuracy and precision QAOs were met as measured by the MS/MSD sample analyses.
Table 6-26 summarizes the chloride analysis results for the duplicate test samples
analyzed. As can be seen from the data in Table 6-26, 9 of the 11 RPDs, or 82 percent, met the
precision QAO of 30 percent RPD. As the completeness objective for the measurement was
70 percent, the precision QAO, as measured by duplicate sample analyses, was met.
6.5 PCDD/PCDF ANALYSES
A total of 35 samples was analyzed for PCDDs and PCDFs by GC/MS using Method
8290 or Method 23. Included in this number were one Method 23 sorbent resin method blank,
one pretest scrubber liquor blank, and three duplicates of test samples. Table 6-27 lists the
sample collection, extraction, and analysis dates for these samples, and the corresponding analysis
hold times. As shown in Table 6-27, all but five samples were extracted within the specified
method limit. Three of the five samples not extracted within the method hold time were sample
6-42
-------
TABLE 6-23. SAMPLE HOLD TIMES FOR CHLORIDE ANALYSES BY ION CHROMATOGRAPHY
o\
4s
Sample*
Stack Exit Flue Gas
TestO
Test 1
Test 1 MS
Test 1 MSD
Test 2
TestS
Test 4
TestS
Test 6
Method blank
Baghouse Exit Flue Gas
TestO
Test 1
Test 2
TestS
Test 4
Test 5
Test 6
Method Requirement
"All samples were analyzed
Collection/preparation date
10/27/93
11/09/93
11/09/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
12/07/93
10/27/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
in duplicate.
TABLE 6-24. FLUE GAS CHLORIDE
Measurement
parameter Method
HClin
flue gas Ion chromatography
Reference
Analysis date Analysis
11/22/93
11/29/93
11/29/93
11/29/93
11/29/93
12/06/93
12/06/93
12/06/93
11/29/93
12/10/93
. 11/22/93
11/29/93
11/29/93
12/06/93
12/06/93
11/29/93
11/29/93
MEASUREMENT QAOs
Precision,
% RSD or RPD
40 CFR 60, Appendix A, Method 5; 30
BIF methods; Method 9057
hold time, days
26
20
20
'20
7
5
4
18
6
3
26
20
7
5
4
11
6
28
Accuracy, Completeness,
% %
75-125 70
-------
TABLE 6-25. CHLORIDE RECOVERIES FROM MS SAMPLES
ANALYZED BY ION CHROMATOGRAPHY
Sample
Chloride recovery,
% Precision QAO
Stack Exit Flue Gas
Test 1 MS
Test 1 MSD
RPD, %
Recovery QAO
105
109
3.7
75-125
30
TABLE 6-26. DUPLICATE
SAMPLE CHLORIDE ANALYSIS RESULTS
Chloride concentration, mg/L
Sample
Stack Exit Flue Gas
Test 1
Test 2
Test3
Test 4
Test 5
Test 6
Baghouse Exit Flue Gas
Test 1
Test 2
Tests
Test 4
Test 6
QAO
Analyses Duplicate analyses RPD, %
0.40
0.88
0.52
<0.29
<0.29
<0.29
19.0
123
28.3
19.6
42.0
<0.29
0.78
0.64
0.60
<0.29
<0.29
18.8
12.0
28.4
20.0
42.7
>31.9
12.1
20.7
>69.7
0
0
1.1
2.5
0.4
2.0
1.7
30
6-44
-------
TABLE 6-27. SAMPLE HOLD TIMES FOR THE PCDD/PCDF ANALYSES BY GC/MS
Sample
Test Feed
Packaging container material
Composite fluff feed
Composite soil feed
Kiln Ash
Testl
Test 1 duplicate
Test 2
TestS
Test 4
TestS
Test 6
Baghouse Ash
TestO
Testl
Test 1 duplicate
Test 2
Test.3
Test 4
TestS
Test 6
Post-test Scrubber Liquor
TestO
Testl
Test 1 duplicate
Test 2
Test3
Test 4
TestS
Test 6
Pretest Scrubber Liquor
Testl
Baghouse Exit Flue Gas Method 23 Train
TestO
Testl
Test 2
TestS
Test 4
TestS
Test 6
Method blank
Method Requirement
Collection
date
12/21/93
10/20/93
10/20/93
11/09/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
10/28/93
11/10/93
11/10/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
10/27/93
11/09/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
12/23/93
10/09/93
10/27/93
11/09/93
11/16/93
12/01/93
12/02/93
11/18/93
11/23/93
12/07/93
Extraction Extraction hold Analysis Analysis hold
date time, days date time, days
01/12/94
11/08/93
12/02/93
11/19/93
01/21/93
12/02/93
12/10/93
12/10/93
12/02/93
12/07/93
11/08/93
12/02/93
01/12/94
12/02/93
12/10/93
12/10/93
12/02/93
12/07/93
11/10/93
12/10/93
01/14/94
12/03/93
12/16/93
12/16/93
12/10/93
12/06/93
12/03/93
11/10/93
11/19/93
12/02/93
12/09/93
12/09/93
12/02/93
12/02/93
12/09/93
22
13
43
10
73
16
9
8
14
14
11
22
63
16
9
8
14
14
14
31
66
17
15
14
22
13
14
'l4
10
16
8
7
14
9
2
30
,01/20/94
11/16/93
12/05/93
11/22/93
01/24/93
12/05/93
12/17/93
12/17/93
12/05/93
12/17/93
11/16/93.
12/05/93
01/20/94
12/05/93
12/18/93
12/18/93
12/05/93
12/17/93
11/15/93
12/14/93
01/21/94
12/07/93
12/19/93
12/19/93
12/15/93
12/15/93
12/07/93
11/15/93
11/24/93
12/06/93
12/13/93
12/13/93
12/06/93
12/06/93
12/13/93
8
8
3
3
3
3
7
7
3
10
8
3
8
3
8
8
3
10
5
4
7
4
3
3
5
9
4
5
5
4
4 .
4
4
4
4
45
6-45
-------
duplicates for analysis; one of the five missed extraction hold time by 1 day.
Table 6-28 summarizes the PCDD/PCDF measurement QAOs for precision, accuracy,
and completeness. Measurement precision was assessed by analyzing split samples in duplicate.
Table 6-29 summarizes the results of these analyses and shows that 57 out of 75 RPD
measurements, or 76 percent, were within the precision QAO of 50 percent RPD. As the
completeness objective for the measurement was 70 percent, the precision QAO, as measured
by duplicate sample analyses, was met.
PCDD/PCDF measurement accuracy was assessed adding the method-specified internal
standards and surrogates to all test samples and measuring their recovery. Table 6-30 shows the
internal standards recoveries achieved from the test samples. As can be seen in Table 6-30,290
out of 315 individual internal standard recovery measurements, or 92 percent, were within the
compound-specific recovery ranges. Since the completeness objective for this measurement was
70 percent, the accuracy QAO, as measured by internal standards recovery, was met.
Table 6-31 lists the surrogate recoveries achieved from test programs samples. As
shown, 149 out of 210 individual surrogate recovery measurements, or 71 percent, were within
the method specified recovery ranges. Again, with a completeness objective of 70 percent, the
accuracy QAO, as assessed by surrogate recoveries, was met.
Table 6-32 shows the MDL objectives and the achieved values for the PCDD/PCDF
measurements. As indicated, all MDL objectives were achieved.
6-46
-------
TABLE 6-28. PCDD/PCDF MEASUREMENT QAOs
Measurement Measurement/ Precision, Accuracy, Completeness,
parameter analytical method Reference Conditions % % %
PCDDs/PCDFs in Extraction, 40 CFR 266, Appendix IX, Matrix-specific 50 25-130 70
feed, residual, and concentration, Method 23; SW-846 extraction
flue gas sampling GC/MS Method 8290
trains
-------
TABLE 6-29. DUPLICATE SAMPLE PCDD/PCDF ANALYSIS RESULTS
o\
Compound
23,7,8-TCDD
1,23,7,8-PeCDD
1,23,4,7,8-HxCDD
1,23,6,7,8-HxCDD
1,23,7,8,9-HxCDD
1,23,4,6,7,8-HpCDD
OCDD
23,7,8-TCDF
1,23,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,23,6,7,8-HxCDF
23,4,6,7,8-HxCDF
1,23,7,8,9-HxCDF
1,23,4,6,7,8-HpCDF
1,23,4,7,8,9-HpCDF
OCDF
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
Precision QAO
= m =»==
Test 1 kiln ash, ng/kg
analysis / duplicate analysis
12.0 / 1.8
31.1 / 6.5
50.8 / 57.5
71.1 / 67.7
212/286
1,810 / 2340
11,590 / 24,580
496 / 281
155 / 49.1
273 / 215
2,770 / 3,160
614 / 676
2,130 / 2,560
25.2 / 35.8
6,180 / 15,220
1,360 / 2,070
12,160 / 44,810
232 / 2.4
305 / 76.6
914 / 905
3,830 / 4,660
3,330 / 1,430
5,730 / 4,630
10,780 / 11,190
15,810 / 28,870
~
RPD,
148
131
12
5
30
26
72
55
104
24
13
10
18
35
84
41
115
196
120
1
20
80
21
4
58
50
2-^^^^2E
Test 1 baghouse ash, ng/kg
analysis / duplicate analysis
0.3 / 1.0
0.47 / 030
0.40 / 0.46
0.69 / 0.74
1.5 / 1.4
213 / 18.1
179 / 110
3.6 / 3.1
1.5 / 1.2
3.2 / 3.7
10.7/9.4
3.9/3.3
9.1 / 9.7
03 / 1.1
39.8 / 25.9
8.1 / 63
123 / 603
0.9 / 0.88
1.5 / 0.42
6.4 / 6.8
38.6 / 32.6
15.4 / 3.1
26.8 / 10.1
40.2 / 41.5
833 / 57.3
RPD,
108
44
14
7
7
16
48
15
22
14
13
17
6
114
42
25
68
2
113
6
17
133
91
3
37
50
Test 1 post-test scrubber
liquor, pg/L
analysis / duplicate analysis
. 2.8 / 2.0
43 / 3.8
4.4 / 3.8
3.4 / 3.0
to t t 1
3.8 / 3.3
12.4 / 13.1
51.2 / 77.5
43 / 4.4
3.1 / 2.6
3.0 / 2.5
7.8 / 8.3
- 33 / 3.0
11.8 / 13.1
3.0 / 2.8
31.8 / 40.0
17.1 / 16.7
185 / 219
2.8 / 2.0
43 / 3.8
3.5 / 33
12.4 / 18.8
43 / 4.4
5.9 / 8.9
27.6 / 9.8
81.8 / 84.1
RPD,
33
12
15
13
1 A
14
5
41
2
18
18
6
10
10
7
23
2
17
33
12
6
41
2
41
95
3
50
===
-------
TABLE 6-30. INTERNAL STANDARD RECOVERIES IN THE PCDD/PCDF ANALYSES
z
vo
% recovery
Sample
Test Feed
Packaging container material
Composite fluff feed
Composite soil feed
Kiln Ash
Test 1
Test 1 duplicate
Test 2
Test 3
Test 4
TestS
Test 6
Baghouse Ash
TestO
Testl
Test 1 duplicate
Test 2
TestS
Test 4
TestS
Test 6
Pretest Scrubber Liquor
Testl
Recovery QAO
13r
C12'
2,3,7,8.
TCDF
543
72.5
85.5
70.4
64.2
56.4
49.8
41.0
90.9
743
60.0
78.6
5.7
71.8
53.5
42.1
68.9
64.4
59.1
40-130
13r
L12-
23,7,8-
TCDD
53.6
79.7
97.0
75.8
62.3
55.5
48.4
42.0
81.2
84.9
63.0
76.5
6.5
71.5
52.0
45.1
68.1
63.0
57.2
40-130
13r
c,r
W.7,8-
PeCDF
58.2
82.2
94.4
83.2
69.4
65.9
47.7
48.9
99.4
773
69.6
86.6
17.5
80.9
58.0
46.6
75.7
64.4
63.3
40-130
13r
1-12"
W.7,8-
PeCDD
593
92.5
107
114
80.5
76.0
54.4
60.7
-90.7
77.2
883
103
33.9
97.4
68.0
63.8
93.0
67.6
66.7
40-130
13r
CI2'
1,23,6,7,8-
HxCDF
59.0
76.4
111
96.1
71.0
74.5
67.4
58.4
113
92.8
76.2
93.8
43.7
91.8
74.4
64.4
87.8
57.6
79.7
40-130
13r
C12'
1,23,6,7,8.
HxCDD
61.1
83.3
111
109
79.6
79.0
73.0
70.0
95.7
99.6
88.8
108
54.8
101
77.5
81.6
96.8
85.0
81.9
40-130
13r
c,2-
1,23,4,6,7,8-
HpCDF
47.2
77.7
117
107
82.2
86.1
612
62.2
164
392
70.9
110
57.5
95.4
69.6
61.2
95.2
66.0
76.7
25-130
13r
C,2.
1,23,4,6,7,8-
HpCDD
44.0
94.9
142
135
92.2
98.2
67.6
73.7
130
145
91.7
115
68.2
108
77.2
76.8
107
853
83.1
25-130
13CI2-OCDD
31.1
95.2
120
138
81.5
105
53.1
623
185
397
85.2
114
77.2
100
60.1
62.6
111
163
66.9
25-130
(continued)
-------
TABLE 6-30. (continued)
o\
6,
o
% recovery
Sample
Post-test Scrubber Liquor
Test 0
Testl
Test 1 duplicate
Test 2
Test3
Test 4
TestS
Test 6
Baghouse Exit Method 23 Train
TestO
Testl
Test 2
Test3
Test 4
TestS
Test 6
Method blank
Recovery QAO
13r
C,2-
23,7,8-
TCDF
52.0
52.2
36.1
41.0
56.0
47.8
20.0
34.3
83.0
56.9
65.0
61.8
63.9
42.7
69.4
69.6
40-130
13r
t-12-
23,7,8-
TCDD
59.6
48.3
30.1
39.0
59.9
48.2
193
25.6
94.1
57.2
593
56.5
59.6
38.7
60.1
65.3
40-130
13r
c,r
1,23,7,8-
PeCDF
58.5
51.9
28.4
42.4
65.9
51.5
21.7
25.2
87.2
613
62.4
60.9
71.0
38.9
60.1
71.6
40-130
13r
C12-
W,7,8-
PeCDD
55.0
57.4
28.9
47.5
55.5
37.5
24.0
25.3
96.6
75.7
65.0
64.7
87.9
44.5
59.6
77.0
40-130
13r
C12'
1,2,3,6,7,8.
HxCDF
73.6
58.3
30.9
53.0
90.1
74.5
30.6
39.5
108
72.4
853
72.4
84.4
57.4
81.7
893
40-130
I3r
C,2-
1,23,6,7,8-
HxCDD
75.6
62.6
33.4
55.7
79.2
62.1
31.5
39.2
112
77.9
82.4
743
88.0
56.7
83.8
89.9
40-130
13r
C,2-
1,23,4,6,7,8.
HpCDF
62.8
53.1
29.1
45.8
76.1
53.4
28.2
33.2
89.1
69.7
79.9
66.0
83.1
513
76.8
88.0
25-130
13r
C12-
1,23,4,6,7,8.
HpCDD
63.2
57.4
36.7
50.8
78.2
59.9
30.5
37.2
90.7
813
83.7
69.9
89.0
56.1
81.7
973
25-130
13C,2-OCDD
413
50.4
263
39.7
663
54.2
26.2
30.6
71.8
68.2
74.5
58.2
78.5
50.8
70.4
92.4
25-130
-------
TABLE 6-31. SURROGATE RECOVERIES IN THE PCDD/PCDF ANALYSES
ON
Sample
Test Feed
Packaging container material
Composite fluff feed
Composite soil feed
Kiln Ash
Testl
Test 1 duplicate
Test 2
Test3
Test 4
TestS
Test 6
BaghouseAsh
TestO
Testl
Test 1 duplicate
Test 2
Test 3
Test 4
TestS
Test 6
Pretest Scrubber Liquor
Testl
Recovery QAO
37CI4-23,7,8-
TCDD
49.5
78.6
74.6
813
60.5
61.0
52.8
46.5
73.2
87.7
66.0
63.8
6.6
58.5
53.9
48.5
56.7
65.7
63.6
70-130
13C,2-2,3,4,7,8- 1;
PeCDF
573
81.2
74.5
86.5
723
77.5
543
58.2
863
81.5
802
79.1
273
75.5
59.9
63.7
70.5
66.7
75.4
70-130
3C,2-1^3,4,7^
HxCDF
63.9
81.7
92.5
92.9
71.5
87.7
78.9
69.1
114 .
144
87.1
79.5
49.4
79.6
75.6
823
70.9
695
81.2
70-130
% recovery
I- 13C12-1,23,4,7,8-
HxCDD
65.1
84.1
91.7
89.5
81.3
83.7
77.1
753
81.6
79.7
90.8
82.1
57.5
80.2
77.7
85.7
75.1
77.4
85.4
70-130
13C,2-1^3,4,7^,9- »
HpCDF
47.3
89.4
110
107
88.7
107
67.2
78.8
118
122
90.4
93.5
70.4
95.6
75.6
83.8
90.4
74.4
95.0
70-130
3C12-1^3,7^,9-
HxCDF
50.5
79.1
893
89.0
74.6
85.4
723
69.5
98.7
85.5
85.6
82.6
57.7
84.4
703
795
76.4
65.6
85.1
70-130
(continued)
-------
TABLE 6-31. (continued)
o\
^
to
Sample
Post-test Scrubber Liquor
TestO
Testl
Test 1 duplicate
Test 2
Test3
Test 4
TestS
Test 6
Baghouse Exit Method 23 Train
TestO
Test 1
Test 2
Test3
Test 4
TestS
Test 6
Method blank
Recovery QAO
TCDD
71.1
58.8
56.2
683
59.7
58.7
49.0
45.7
102
66.4
122 »
119
114
124
. 115
113
70-130
13Cir23,4,7,8-
PeCDF
72.6
683
60.7
71.1
73.2
67.1
55.1
52.6
112
79.1
128
130
129
133
124
133
70-130
«
HxCDF
82.7
62.6
69.6
73.0
80.6
69.0
723
62.0
97.0 .
82.9
110
109
108
103
104
106
70-130
b recovery
HxCDI)'
86.1
74.4
88.4
77.0
90.8
73.9
76.8
66.4
107
88.2
121
110
108
107
103
117
70-130
13C12-1^3,4,7^,9-
HpCDF
75.0
80.0
86.6
833
93.8
81.0
73.5
81.1
97.1
96.1
137
139
131
138
129
138
70-130
HxCDF
75.4
75.9
71.8
81.5
913
80.8
71.1
68.8
79.6
74.0
84.4
64.1
71.8
54.6
723
75.6
70-130
-------
TABLE 6-32. PCDD/PCDF MEASUREMENT MDLs: OBJECTIVES AND ACHIEVED
LEVELS
Solid residues,
Measurement ng/kg
parameter objective / achieved
2,3,7,8-TCDD
1,2,3,7,8-PeCDD
1,2,3,4,7,8-HxCDD
1,2,3,6,7,8-HxCDD
1,2,3,7,8,9-HxCDD
1,2,3,4,6,7,8-HpCDD
OCDD
2,3,7,8-TCDF
1,2,3,7,8-PeCDF
2,3,4,7,8-PeCDF
1,2,3,4,7,8-HxCDF
1,2,3,6,7,8-HxCDF
2,3,4,6,7,8-HxCDF
1,2,3,7,8,9-HxCDF
1,2,3,4,6,7,8-HpCDF
1,2,3,4,7,8,9-HpCDF
OCDF
Total TCDD
Total PeCDD
Total HxCDD
Total HpCDD
Total TCDF
Total PeCDF
Total HxCDF
Total HpCDF
20 / 0.6
20 / 0.9
20 / 1.0
20 / 0.8
20 / 0.9
20 / 1.0
20 / 1.1
20 / 0.6
20 / 0.7
20 / 0.7
20 / 0.7
20 / 0.5
20 / 0.7
20 / 0.8
20 / 0.6
20 / 1.0
20 / 0.9
30 / 0.6
30 / 0.9
30 / 0.9
30 / 1.0
30 / 0.6
30/0.7
30 / 0.7
30 / 0.8
Aqueous liquids,
Pg/L
objective / achieved
200 / 1.3
200 / 2.2
200 / 2.3
200 / 1.8
200 / 2.0
200 / 2.2
200 / 4.7
200 / 1.0
200 / 1.5
200 / 1.5
200 / 1.6
200 / 1.2
200 / 2.7
200/1.7
200 / 1.4
200/2.3
200 / 2.6
300 / 1.3
300 / 2.2
300 / 2.1
300 / 2.2
300 / 1.0
300/1.5
300 / 2.6
300 / 1.8 .
Flue gas, ng/dscm
objective / achieved
0.2 / 0.0009
0.2 / 0.0012
0.2 / 0.0015
0.2 / 0.0012
0.2 / 0.0015
0.2 / 0.0015
0.2/0.0061
0.2 / 0.0009
0.2 / 0.0009
0.2 / 0.0009
0.2 / 0.0012
0.2 / 0.0009
0.2 / 0.0025
0.2 / 0.0012
0.2 / 0.0009
0.2 / 0.0015
0.2 / 0.0018
0.5 / 0.0009
0.5 / 0.0012
0.5 / 0.0015
0.5 / 0.0015
0.5 / 0.0009
0.5 / 0.0009
0.5 / 0.0021
0.5 / 0.0012
6-53
-------
REFERENCES
1. "Guidance on Setting Permit Conditions and Reporting Trial Burn Results, Volume II
of the Hazardous Waste Incineration Guidance Series," EPA/625/6-89-019 January
1989.
2. 40 CFR Part 266, Appendix IX.
3. "Test Methods for Evaluating Solid Waste: Physical/Chemical Methods," EPA SW-846,
3rd edition, Revision 1, July 1992.
4. 40 CFR Part 60, Appendix A.
5. Gullett, B., K. Bruce, and L. Beach, "The Effect of Metal Catalysts on the Formation
of Polychlorinated Dibenzo-p-dioxin and Polychlorinated Dibenzofuran Precursors,"
presented at the 9th International Symposium on Chlorinated Dioxins and Related
Compounds (Dioxin 89), Toronto, Canada, 1989.
R-l
------- |