EPA/540/R-93/507
SITE EMERGING TECHNOLOGIES PROJECT:
BABCOCK & WILCOX CYCLONE VITRIFICATION
by
Jean M. Czuctwa, James J. Warchol,
William F. Musiol. and Hamid Farzan
The Babcock & Wilcox Company
Contract Research Division
Alliance, Ohio 44601
Contract No. CR-815800-02-0
Project Officer:
Laurel J. Staley
Risk Reduction Engineering Laboratory
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268
RISK REDUCTION ENGINEERING 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 in part by the United
States Environmental Protection Agency under Cooperative Agreement NO. CR-
815800-02-0 to Babcock & Wilcox Co. The document has been subjected to the
Agency's administrative and peer review and 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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The U.S. Environmental Protection Agency (EPA) is charged by congress
with protecting the Nation's land, air, and water resources. As the enforcer
of national environmental laws, the EPA strives to balance human activities
and the ability of natural systems to support and nurture life. A key part of
the EPA's effort is its research into our environmental problems to find new
and innovative solutions.
The Risk Reduction Engineering Laboratory (RREL) is responsible for
planning, implementing, and managing research, development, and demonstration
programs to provide an authoritative, defensible engineering basis in support
of the policies, programs, and regulations of the EPA with respect to drinking
water, wastewater, pesticides, toxic substances, solid and hazardous
wastes,and Super fund-related activities. This publication is one of the
products of that research and provides a vital communication link between the
researcher and the user community.
Now in its eighth year, the Superfund Innovative Technology Evaluation
(SITE) Program is part of EPA's research into cleanup methods for hazardous
waste sites around the nation. Through cooperative agreements with
developers, alternative or innovative technologies are refined at the bench-
and pilot-scale level and then demonstrated at actual sites. EPA collects and
evaluates extensive performance data on each technology to use in remediation
decision-making for hazardous waste sites.
This report documents the results of laboratory and pilot-scale field
testing of the vitrification of soil contaminated with methods.
E. Timothy Oppelt, Director
Risk Reduction Engineering Laboratory
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ABSTRACT
The Babcock & Wilcox cyclone vitrification furnace appears well suited
to treating high inorganic content hazardous wastes and contaminated soils,
which exist at many Super fund sites. In a study performed under the U.S. EPA
Superfund Innovative Technology Evaluatron (SITE) Emerging Technologies
Program, the Babcock & Wilcox six million Btu/hr pilot cyclone furnace was
used to vitrify an EPA Synthetic Soil Matrix (SSM) spiked with 7,000 ppm lead,
1,000 ppm cadmium, and 1,500 ppm chromium.
During 1990 to 1992, pilot-scale testing of the Babcock & Wilcox six
million Btu/hr pilot cyclone furnace for the vitrification (immobilization) of
heavy metals from contaminated soil was conducted. The tests were conducted
on wet and dry contaminated soil (synthetic soil matrix) fed at several feed
rates ranging from 50 to 300 Ib/hr. The soil is captured and melted In the
molten slag layer that forms at the cyclone furnace wall, exits the cyclone
furnace, and is dropped into a water-filled slag tank where it solidifies.
The cyclone vitrification process successfully treated several tons of
SSH. The vitrified soil was non-teachable by the Toxicity Characteristic
Leaching Procedure (TCLP). The volume of the vitrified soil was reduced by
approximately 25-35% when compared to dry SSM.
This report was submitted in fulfillment of Cooperative Agreement
CR-815800-02-0 by the Babcock & Wilcox Research 4 Development Division under
the partial sponsorship of the U.S. Environmental Protection Agency. This
report covers a period from March, 1990, to February 28, 1992, and work was
completed as of February 28, 1992.
Subsequent to the SITE Emerging Technologies project described here, the
U.S. Environmental Protection Agency conducted a SITE Demonstration of the B&W
cyclone vitrification process in November, 1991. The results of this
Demonstration are expected to be published by the U.S. EPA in 1992.
1v
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TABLE OF CONTENTS
Foreword ________________________________iii
Abstract iV
Figures and Tables vi
Abbreviations and Symbols _______________________ vii
Acknowledgments ____________________________ viii
1 EXECUTIVE SUMMARY 1
A. The SITE Emerging Technologies program ___________ 1
B. Summary Results 1
2 INTRODUCTION AND BACKGROUND INFORMATION 3
3 PROCESS DESCRIPTION 6
A. Phase I (Dry Soil Processing) Configuration _________ 8
B. Configuration for Phase II (wet Soil Feed Processing) _ _ _ _ 11
C. Atomizer Design for Phase II Tests _____________ 15
D. Furnace Continuous Monitors __________________ 17
E. Applicable Wastes and Possible Technology
Configurations 18
4 EXPERIMENTAL DESIGN 20
A. Decription of Phase I and Phase II Tests 20
B. Description of Phase I (Dry SSM Feed) Tests _________ 21
C. Description of Phase II (Wet SSM Feed) Tests 23
D. Use of a Fluxing Agent to Increase
Metal Retention in the Slag 24
E. Synthetic Soil Matrix (SSM) 25
F. Sampling Methods 28
G. Analytical Methods 30
5 RESULTS 31
A. Vitrification as Measured by TCLP Test Results _______ 31
B. Volume Reduction _______________________ 36
C. Metals Retention 38
D. Mass Flowrates of the Fly Ash and Slag Streams 41
E. Relative Concentrations of Metals in the Slage
andFlyAsh 41
F. OJperability/Emissions 48
6 QUALITY ASSURANCE , 50
A. Systems Audits 50
B. Performance Audits for Critical Measurements *...... 51
C. Performance Audits for Non-Critical Measurements 53
7 CONCLUSIONS AND RECOMMENDATIONS 55
A. Conclusions 55
B. Recommendations for Future Work .55
8 REFERENCES 58
9 APPENDIX 59
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Figure PU3H
1 The Pilot Cyclone Test Facility.. ____________ 7
2 Schemation of Cyclone Vitrification Process 9
3 Phase 1 Cyclone Furnace Configuration- _________ 10
4 Phase II Cyclone Furnace Configuration ________ 12
5 Wet Soil Feed System ___________________ 14
6 Schemation of Wet Soil Atomizer.. ____________ 16
7 Sampling and Analysis Location 29
8 Vitrified Synthetic Soil Matrix-____________ 32
9 Toxicity Characteristic Leaching Procedure Results _ _ _ _ _ 33
10 Volume Reduction. _____________________ 37
11 Heavy Metal sand Ash Mass Balance ____________ 44
12 Heavy Metals Capture vs.FeedRate. ____________ 46
13 Heavy Metals Capture vs.Volatility Temperature. _ _ _ 47
LIST OF TABLES
Table
1 Phases and Specific Goals of the SITE
Emerging Technologies Program. 5
2 Typical Cyclone Furnace Test Conditions 21
3 Phase I Test Matrices 22
4 Phase II Test Matrices 23
5 Typical SSM Characterization Results(DryBasis) 27
6 Results of TCLP Tests for Untreated and Treated SSM ... 34
? Percent of Leachable Metals Before and After Treatment . . 35
8 Total Metals in the Soil,Slag and
Multiple Metals Train Particulates 42
9 Average Phase I CO,C02,and NOx Levels(Spiked SSM) 48
10 QC Data for TCLP Analyses 52
11 QC Data for Non-Critical Metals Determinations 54
V i
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LIST OF ABBREVIATIONS AND SYMBOLS
ABBREVIATIONS
ASTM -- American Society for Testing of Materials
Btu -- British thermal units
B&W -- Babcock & Wilcox
Cd - - cadmium
Cr - - chromium
cu ft -- cubic foot
DRE -- destruction and removal efficiency
EPA -- United States Environmental Protection Agency
kg -- kilogram
L -- liter
Ib/hr -- pounds per hour
MBtu -- Million British thermal units
mg -- milligram
MSW -- municipal solid waste
MW - - megawatt
Pb -- lead
PSIG -- pounds per square inch gage
QA -- quality assurance
QAPP -- quality assurance project plan
iPD -- relative percent difference
RREL -- Risk Reduction Engfneering Laboratory (EPA)
SBS -- small boiler simulator pilot facility
SITE -- Superfund Innovative Technology Evaluation
SSH -- synthetic soil matrix
TCLP -- toxicity characteristic leaching procedure
u -- microgram
Vii
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ACKNOWLEDGMENTS
This document was prepared under Cooperative Agreement No.
CR-815800-02-0 by the Babcock & Wilcox Company Research and Development
Division, Alliance, Ohio. Laurel Staley of the Risk Reduction Engineering
Laboratory (RREL) was the Project Officer responsible for the preparation of
this document and deserves special thanks for her helpful comments and advice.
SSM was obtained from the RREL Releases Control Branch (Edison, NJ). TCLP
analyses were performed by Aquatec (So. Burlington, VT). Technical assistance
was provided by B&K staff
R. Bailey, S. Boyce, L. Breyley, V. Burgess, J. Curtis, R. Huskins, J. Lyden,
K. Nevitt, R. Schreckengost, E. Stoffer, and T. Wilson.
Viii
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1. EXECUTIVE SUMMARY
The SITE Emerging Technologies Project
During 1990 to 1992, pilot-scale testing of the Babcock I Wilcox six
million Btu/hr pilot cyclone furnace for the vitrification of soil and
immobilization of heavy metals was conducted. The tests were conducted on wet
and dry contaminated soil (synthetic soil matrix) fed at several different
feed rates.
Summary Results
The pilot cyclone furnace was successfully used to vitrify an EPA
Synthetic Soil Matrix (SSM) spiked with 7,000 ppm lead, 1,000 ppm cadmium, and
1,500 ppm chromium. Tests showed 95 to 97% of the non- combustible portion of
the input SSM was incorporated within the slag. When operated at 50 to 150
Ib/hr of dry SSM feed, and from 100-300 Ib/hr of wet SSM feed, the cyclone
technology was able to produce a non-teachable product. Average lead,
cadmium, and chromium TCLP teachabilities in the untreated SSM were 104, 54,
and 2.3 mg/L, respectively. Average lead, cadmium, and chromium TCLP
teachabilities in the treated SSM from the 50 to 150 Ib/hr dry SSM tests were
0.20, 0.13, and 0.11 mg/L, respectively, and for the treated SSM from the 100
to 300 Ib/hr wet SSM tests were 0.20, 0.07, and 0.04 mg/L, respectively. All
of these TCLP results are close to the analytical detection limit and, hence,
the results for wet vs. dry soil are not likely significantly different. All
of these treated SSM TCLP results are well below the TCLP limits.
Using natural gas as the fuel, the CO and NO, stack emissions gases from
the process averaged 19 and 352 ppm at 3% 02, respectively. Stack C02
averaged 11.5%. These stack levels are within acceptable ranges. The capture
of heavy metals in the vitrified slag from all tests ranged from 8-17% for
cadmium, 24-35% for lead, and 80 95% for chromium. Addition of 10% of a Borax
flux did not significantly improve the heavy metals capture in the vitrified
slag despite lower cyclone temperatures (=100°F).
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The capture of heavy metals in the slag increased with increasing feed
rate, likely due to shorter cyclone furnace residence times. The capture of
metals in the slag increased with decreasing metal volatility. This suggests
the cyclone vitrification process would be well suited to treatment of low
volatility contaminants, such as many radionuclides.
The treatment of the synthetic soil matrix resulted in a volume
reduction of 25-35% (dry basis). The vitrification treatment results in an
easily-crushed, glassy product.
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2. INTRODUCTION AND BACKGROUND INFORMATION
The Superfund Amendments and Reauthorization Act of 1986 directed the
U.S. Environmental Protection Agency to establish an "Alternative or
Innovative Treatment Technology Research and Demonstration Program". In
response, the EPA Office of Solid Waste and Emergency Response and the Office
of Research and Development established a formal program called the Superfund
Innovative Technology Evaluation (SITE) Program to accelerate the development
and use of innovative cleanup technologies at hazardous waste sites across the
country.
This project was sponsored under the SITE Emerging Technologies Program.
Before a technology can be accepted into the Emerging Technologies Program,
sufficient data must be available to validate its basic concepts. The
technology is then subjected to a combination of bench- and pilot-scale
testing in an attempt to apply the concept under controlled conditions.
The Babcock & Wilcox cyclone furnace is a well-established design (over
26,000 M installed electrical capacity) for the combustion of high inorganic
(ash) coal. The combination of high heat release rates (450,000 Btu/cu ft for
coal) and high turbulence in cyclones assures the high temperatures required
for melting the high ash fuels. The inert ash exits the cyclone furnace as a
vitrified slag.
Taking advantage of the ability of the cyclone furnace to form a
vitrified slag from waste inorganics, the cyclone furnace was used in a
research and development project to vitrify municipal solid waste (MSW) ash
containing heavy metals. The cyclone furnace produced a vitrified MSW ash
which was below EPA teachability limits for all eight RCRA metals. The
successful treatment of MSW ash suggested that the cyclone vitrification
technology would be applicable to high inorganic content hazardous wastes and
contaminated soils that also contain organic constituents. These types of
materials exist at many Superfund sites, as well as sites where petrochemical
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and chemical sludges have been disposed. Our approach for establishing the
suitability of the cyclone vitrification technology relies on the premise that
for acceptable performance in treating hazardous waste mixtures containing
organic and heavy metals constituents, the cyclone furnace must melt EPA's
synthetic soil matrix (SSM) while producing a non-teachable slag and must
achieve the destruction and removal efficiencies (DRE's, currently 99.99%) for
organic contaminants normally required for RCRA hazardous waste incinerators.
The high temperature (>2,500 to 3,000°F), turbulence, and residence time in
the cyclone and main furnace are expected to result in high organics
destruction and removal efficiencies (DRE's).
A SITE demonstration was performed on the pilot cyclone furnace in
November of 1991. An EPA-supplied synthetic soil matrix spiked with heavy
metals (cadmium, chromium,and lead), organics (anthracene and dimethyl
phthalate), and simulated radionuclides (cold strontium, bismuth, and
zirconium) was used. Depending on the results of the SITE demonstration, the
next step for product development would be conceptualization, design,
construction, field testing, and economic analysis of a full-scale unit (e.g.,
80 tons per day).
This report will present the results of both the Phase I(1990-1991) and
Phase II (1991-1992) Emerging Technologies efforts. The two Phases had
specific goals as given in Table 1. Roth Phases used an EPA synthetic soil
matrix spiked with lead, cadmium, and chromium. The most important goal for
both Phases was to produce a vitrified soil that passes the Toxicity
Characteristic Leaching Procedure (TCLP) limits for lead, cadmium, and
chromium. Because the most significant difference between Phases I and II is
the use of a dry or wet soil feed system, Phases I and II nay also be referred
to in this report as "Dry Soil Feed System" and "Wet Soil Feed System,"
respectively. The wet soil feed system was used for the EPA Demonstration of
the technology and, thus, this report will emphasize the results for this
final system configuration.
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TABLE 1
Phases and Specific Goals of the
SITE Emerging Technologies Project
Phase
Specific Goals
Phase I (1990-91) -
Dry Soil Feed System
Phase II (1991-92) -
Wet Soil Feed System
• Determine synthetic soil matrix (SSM)
properties.
. Establish cyclone operability (e.g.,
feeding, melting behavior, operational
data).
. Determine slag leachability and volume
reduction.
. Determine preliminary heavy metals mass
balance for cyclone treatment process.
. Design of wet soil feed system and atomizer.
. Establish cyclone operability (e.g., feeding,
melting behavior, operational data).
. Determine slag leachability and volume
reduction.
. Optimize heavy metals capture and determine
metals mass balance for cyclone treatment
process.
Measurement of organics destruction efficiencies, thought to be less of
a technical challenge compared with metals capture, was reserved for a SITE
Demonstration performed in November 1991. The remainder of this report
describes the cyclone furnace used in this study, the tests that were
conducted, the results achieved and, finally, conclusions that can be drawn
about the usefulness of the cyclone furnace for the treatment of hazardous
waste.
,5.
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3. PROCESS DESCRIPTION
The Babcock & Wilcox six million Btu/hr cyclone furnace located in
Alliance, Ohio, was used to perform all pilot-scale vitrification tests
discussed in this report. The furnace is water-cooled and simulates the
geometry of B&H's front- wall fired cyclone coal-fired boilers. This cyclone
facility has been proven to simulate typical full-scale cyclone units in regard
to furnace/convection gas temperature profiles and residence times, NOx levels,
cyclone slagging potential, ash retention in the slag, unburned carbon, and
flyash particle size.
The pilot cyclone furnace, shown in Figure 1, is fired by a single,
scaled-down version of a cormnercial coal combustion cyclone furnace. The
furnace geometry is a horizontal cylinder (barrel). A summary of the process is
illustrated in Figure 2. Both the primary air and secondary air were heated to
approximately 820°F. Primary air, secondary air, and soil conveying air (150*F)
used to transport the soil into the furnace accounted for 25%, 72%, and 3% of
the total air input, respectively. For these tests, natural gas and preheated
primary combustion air enter tangentially into the cyclone burner. In dry soil
processing, preheated secondary air, the soil matrix, and a portion of the
natural gas enter underneath the secondary air and parallel to the cyclone
barrel axis. For wet soil processing, an atomizer is used to spray the soil
paste directly into the furnace.
Upon entering the cyclone furnace, soil is captured and melted, and
organics are destroyed in the molten slag layer that is formed and retained on
the furnace barrel wall by centrifugal action created by the tangentially fired
combustion air. The soil melts, exits the cyclone furnace from the tap at the
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STACK PARTICULATE
SAMPLING LOCATION
SSM FEED
SYSTEM
CONTINUOUS EMISSIONS
MONITOR (CEM)
SAMPLING LOCATION
SSM
SAMPUNG
LOCATION
SLAG AND
QUENCH
WATER
SAMPUNG
LOCATION
ID FAN
SCRUBBER
(NOT IN
BAGHOUSE
HEAT
EXCHANGER
SLAKER
(NOT IN
COMBUSTION
AIR
NATURAL GAS
IIIJ-l I WIXJ-ll— V-^
INJECTORS
FURNACE
STACK
I I II
FURNACE
SLAG
TRAP
NATURAL
GAS
SOIL
INJECTOR
^CYCLONE
SPOUT BARREL
SLAG
QUENCHING
TANK
FIGURE 1 Pilot Cyclone Test Facility
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cyclone throat, and is dropped into a water-filled slag tank where it
solidifies. Operation of the cyclone at a load of 5 million Btu/hr produced the
best slag tapping conditions. Operation at both 6 and 4 million Btu/hr load
conditions decreased slag tapping due to changes in cyclone flow patterns.
A small quantity of soil also exits as flyash with the flue gas from the
furnace and is collected in a baghouse. This flyash can be recycled to the
furnace as indicated in Figure 2 to increase the capture of metals and to
minimize the volume of the potentially hazardous fly ash waste stream.
Flue gas passes through a baghouse for purposes of particulate control.
To maximize the capture of metals, a heat exchanger is used to cool the stack
gases to approximately 200°F before entering the baghouse. Although the cyclone
facility is equipped with an acid gas scrubber, it was not used for these tests
because acid gas generation (e.g., HC1) from the vitrification of the SSH was
expected to be low.
Phase I (Dry Soil Processing) Configuration
The furnace configuration used in Phase I is-shown in Figure 3. Natural
gas and preheated primary combustion air enter tangentially into the cyclone
burner. Preheated secondary air, the soil matrix (fed into the furnace
pneumatically by a screw feeder), and natural gas enter parallel to the cyclone
axis into the cyclone furnace. The soil is captured and melted and organics
destroyed in the molten slag layer that is formed and retained on the furnace
wall by centrifugal action. Most of the soil melts, exits the cyclone furnace
from the tap at the cyclone throat, and is dropped into a water-filled slag tank
where it solidifies. A small quantity of soil exits as flyash with the flue gas
from the furnace and is collected in a baghouse.
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I
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o
I
AIB
AIB
GAS
SOIL
AIH
GAS
•L
FIGURE 3 Cyclone furnace Configuration for 1
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Particulate control was achieved by way of a MikroPul, Inc.baghouse
containing twenty-three 10-ft. Nomex bags and operated at an air-to-cloth ratio
of 2.8 at 150°F. A single-pass, water-cooled heat exchanger with seventy 1.5" x
8 ft U-tubes is used to cool the stackgases to approximately 200*F before
entering the baghouse. Although the cyclone facility is equipped with an acid
gas scrubber, it was not used because acid gas generation (e.g., HC1) from the
vitrification of SSM was expected to be low.
Configuration for Phase II (Wet Soil Feed Processing)
The primary difference between the cyclone furnace configurations for
Phase I and Phase II is in the feed system. While Phase I tests used dry soil,
Phase II used soil with a high moisture content and a muddy consistency. It is
generally thought that Superfund soils will range from very dry to wet or muddy.
Because feed system problems are often encountered at Superfund sites, it was
important to demonstrate that the cyclone furnace could operate with a wet soil
feed. In addition, it was not known how well the vitrification process would
tolerate a high moisture feed (e.g., possible heat losses due to evaporation or
entrainment of particulate by the generated steam). Thus, wet soil feed system
design and testing were a major goal of the Phase II effort.
The wet feed system furnace modifications are shown in Figure 4. The
modifications were performed not only to add wet soil feeding capability, but
also to improve the distribution of soil to the soil- melting surfaces of the
furnace barrel. Modifications made on the furnace to accomplish these two goals
included: (1) removal of the scroll so that no primary air or natural gas are
added at the furnace front location; (2) installation of natural gas jets at
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COMBUSTION
AIR
NATURAL GAS
INJECTORS
CYCLONE
BARREL
SLAG
SPOUT
SLAG
QUENCHING
TANK
FIGURE 4 CYCLONE FURNACE FOR WET SOIL INPUT
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the secondary air entrance. These were used together with the gas lighter; and
(3) installation of a soil atomizer using variable compressed air at the former
scroll burner location (see Section C, below).
To improve the feeding of wet soil to the cyclone furnace a Moyno
progressing cavity pump with speed controller (Frame 2J3, Type CDR AM) was used
to feed the high viscosity soil. A maximum feed rate of 620 Ib/hr is possible
with this pump model. The pump stator material is natural rubber and the rotor
is chromium steel. The speed controller is designed to maintain a constant
motor speed and, thus, a constant soil feed rate to the cyclone furnace (200
Ib/hr feed at a pump speed of 631 rpm).
The Phase II feed system was installed and tested using clean, wet SSM to
which water was added to produce a moisture content of 24% (the as-received $SM
was approximately 20% moisture). A schematic of the system is shown in Figure
5.
The soil was added to the feed hopper as follows: Yater was added to each
drum of SSM. After replacing the drum lid, the soil was mixed using a drum
tumbler operated for 1 hour. The drum lid was replaced by a discharge cone, and
the drum was emptied into the feed hopper by way of two valves. Particles
larger than 1/2* were screened from the soil during transfer to the feed hopper.
After loading the hopper, a two-blade mixer was turned on. The feed system was
calibrated and SSM was fed to the cyclone furnace for initial combustion
optimization. Several SSM moisture contents were tested, and the most effective
operation was found at 26% moisture. Therefore, the pump was recalibrated at
26% moisture and the remaining Phase II experiments were conducted at this
moisture level.
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SSM Feed System
"\"".A Vr% LrY 1C
in
(TYP.)
TO
W (? t :> o 11 Feed S v s t e m
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Atomizer Design for Phase II Tests
To optimize the distribution of wet feed inside the cyclone furnace,
preliminary testing with simple nozzles was performed to determine the
atomization design for SSM. An externally-mixed atomizer appears to work well
for the SSM. High-velocity air was used to achieve atomization. The objective
for this project was to evenly spray SSM to the cyclone furnace barrel walls
where combustion and melting will take place. The droplet size must also be
large enough to avoid merely entraining the SSM in the combustion gases exiting
the furnace, but not so large as to form deposits in the furnace.
An atomizer was designed, modified, and tested during Phase II. For
successful vitrification of the soil paste, the atomizer has to meet the special
requirements associated with the soil material and furnace geometry. Commercial
atomizers or nozzles of the required flow capacities have flow passages that are
too small to pass the soil paste or the expected small pebbles in the soil. The
specific parameters deemed important to the operation of the atomizer are as
follows: (1) atomize a high soli(14 soil slurry consisting of approximately 75%
to 80% solids; (2) accommodate flow rates up to about 400 Ib/hr of slurry; (3)
permit passage of pebbles or agglomerates up to about 3/8 inch in diameter; (4)
have a compressed air consumption of about 200 Ib/hr or less (pilot-scale only);
(5) minimize flow constrictions that would tend to plug; (6) provide a
directional spray that could be pointed toward the hottest surfaces in the
interior of the cyclone combustor; and (7) have an overall diameter of 1 to 1
1/2 inches to accommodate installation through existing ports in the cyclone
combustor.
The atomizer, shown in Figure 6, was-developed to inject and disperse the
soil paste into the cyclone combustor. Photographs of the atomizer are enclosed
in the Appendix. The atomizer consists of two concentric tubes. The inner tube
provides the flow passage for the soil paste, while compressed air is supplied
in the annular space between the two tubes. At the outlet end of the atomizer,
flow passages between the soil tube and the annulus provide the high velocity
air streams for atomization of the soil. The outlet end of the soil paste tube
is shaped in a rectangle and attached to a tungsten carbide insert. This insert
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of the
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/'
AIR
/„../_
SOIL
AIR
JiC 6 Scheaiatk: fit ay ram of the Wc-t So' 1 At
-------
is in the form of a billet with a machined slot. The tungsten carbide insert
forms three of the four walls of the rectangular opening, while a flow
distributor plate forms the fourth wall. Rectangular flow passages machined
into the flow distributor plate provide the high velocity air streams that
atomize the soil paste.
The flow passages are inclined at different angles relative to the axis of
the atomizer in order to distribute the soil particulate over a large area. The
tungsten carbide insert is used to minimize erosion due to the high velocity air
and soil particles impacting the wall of the tube opposite the air passages.
This style of atomizer provides a "straight through" passage of the soil
paste into the combustor to minimize pluggage problems due to agglomerates or
pebbles. Also, the flow of compressed air in the annulus surrounding the soil
paste tube provides cooling which minimizes the chance of the soil drying out in
the tube and plugging the atomizer. The atomizer designs were initially
cold-tested outside the cyclone furnace by spraying clean SSM into a 55-gallon
barrel to observe the SSM spray pattern and flow.
In final operation, atomizer air flow rates of 90 to 130 Ib/hr, and static
pressure of 15 to 100 PSI6 were used. The soil atomizer was inserted at two
locations; next to the gas lighter or at the middle of the cyclone using the
scroll burner initially and eventually replacing the scroll burner with a plate
(see picture in the Appendix). The latter configuration was the most optimal.
The direction of the dispersed soil can be controlled by adjusting the atomizer
direction. Soil atomizer direction was upward for the best results; when
pointed downward slag accumulation was observed.
Furnace Conditions Monitors
To monitor the operation of the cyclone furnace during Phase I and Phase
II tests, the following operating parameters were monitored. Carbon monoxide
and carbon dioxide were measured during both phases of cyclone testfng using
Beckman Model 864 Infrared Analyzers. Oxygen was measured using Beckman Model
755 and Bailey Model OC1530 Oxygen Analyzers. Nitrous Oxides were measured
using a Beckman Model 951A NO/NOx Analyzer.
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Calibration was performed before and after each day's test with SSM spiked
with heavy metals using calibration gases supplied by Linde (Somerset, NJ).
Fluke digital readout and Type K thermocouples were used for temperature
readings. Air flow rates were measured using ASTM orifices. Rosemont pressure
transducers were used. Data acquisition was by an IBM PC using a Keithley 570
system and LabTech software.
Applicable Wastes and Soils and Possible Technology Configurations
An advantage of vitrification over other thermal destruction processes is
that in addition to the destruction of organic constituents, the resulting
vitrified product captures and does not leach heavy metals or radionuclides.
The cyclone vitrification technology would be applicable to high inorganic
content hazardous wastes, sludges, and contaminated soils that contain heavy
metals and organic constituents. These types of materials exist at many
Superfund and Department of Energy sites, as well as sites where petrochemical
and chemical sludges have been disposed. These wastes may be in the form of
solids, a soil slurry (wet soil), or liquids. To be treated in the cyclone
furnace, the ash or solid matrix must melt and flow at cyclone furnace
temperatures (2800 to 3000°F).
Because of the technology's ability to capture heavy metals in the slag
and render these non-leachable, an important application of the technology is
contaminated soils which contain non-volatile radionuclides (e.g., strontium,
transuranics).
The cyclone furnace can be operated with gas, oil, or coal as the
supplemental fuel (the likely application for coal-fired use is waste treatment
at an existing electrical generating utility). The waste itself may also supply
a significant portion of the required heat input. Heat recovery is available,
but is unlikely to be a priority for the final design. Recycling of the small
volume of baghouse ash may be advantageous in field operation.
-18-
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Additional air pollution control devices, such as NOx reduction
technologies, can be applied as needed. An acid gas scrubber would be required,
for example, when chlorinated wastes are treated. The final process
configuration will determine the size of the full-scale system.
-19-
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4. EXPERIMENTAL DESIGN
The studies discussed in this document occurred in two phases. Both
phases will be described in more detail later in the report. For purposes of
describing the process, Phase I concerned feeding dry soil to the cyclone and
Phase II concerned feeding wet soil to the cyclone. The process configuration
used for each phase will be described below.
Description of Phase I and Phase II Tests
The most important goal for both Phases was to produce a vitrified soil
that passes the Toxicity Characteristic Leaching Procedure (TCLP) limits for
lead, cadmium, and chromium. Because the most significant difference between
Phases I and II is the use of a dry or wet soil feed system, Phases I and II may
also be referred to in this report as "Dry Soil Feed System" and "Wet Soil Feed
System," respectively. The wet soil feed system was used for the EPA
Demonstration of the technology. Thus, this report will emphasize the results
for this final system configuration. Both Phases used an EPA synthetic soil
matrix spiked with lead, cadmium, and chromium.
Typical run conditions for the Phase I and Phase II tests are given in
Table 2, below.
-20-
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TABLE 2
Typical Cyclone Furnace Tests Conditions
Condition Typical Range of Values
Heat Input (natural gas fuel) 5 million Btu/hr
SSM Feed Rate 50 to 300 Ib/hr
Excess Oxygen 1.0%
Primary and Secondary Air Temperature 820°F
Total Air Split - Phase I
Primary Air 25%
Secondary Air 72%
Feed Air 3%
Total Air Split Phase II
Primary Air not used
Secondary Air 96.5%
Soil Atomizer Air 3.5%
Slag Temperature (in cyclone barrel) 2370-2460°F
Gas Temperature (cyclone exit) 2800-3000°F
Furnace Exit Temperature 2100-2200°F
Baghouse Temperature 200°F
Flyash/Flyash + Slag Ratio Phase I 5%
Flyash/Flyash + Slag Ratio - Phase II 3%
Measurement of organics destruction efficiencies, thought to be less of a
technical challenge compared with metals capture, was reserved for a SITE
Demonstration performed in November 1991
A description of both Phase I and Phase II will be provided, below followed
by a description of the SSM used in each-test.
Description of Phase I (Dry SSM Feed) Tests
Phase I tests ranged from 3-1/4 to 14 hours. The cyclone furnace was
first fired on natural gas (with gradual addition of primary and secondary air)
for approximately 2-3 hours before adding the SSM. After the furnace barrel was
heated, SSM feed was started and soil melting and tapping was observed through
observation ports. Minor adjustments were made, as needed, to maintain soil
-21-
-------
melting and tapping. Sensors, emissions monitors, and sampling were initiated
after conditions stabilized. The test conditions for the preliminary
vitrification tests are given in Table 3
TABLE 3
Phase I Test Matrices
Test
Cyclone
Load
MBtu/hr
SSM
Feed
Rate,
Ib/hr
Stack %
Excess
Oxygen
Slag
leap.
*F
Flyash/
Slag
Primary &
Secondary
A1r Temp.
•F
Preliminary Vitrification Tests [Ory, Clean Soil]
10/25/90
10/26/90
10/26/90
10/26/90
4.8
4.6
4.9
4.7
50
100
150
200
1.1
0.8
0.5
0.7
2340
2430
2370
2380
813
<5%* 821
824
823
Heavy Netils Tests [Ory, Spikea Soil]
11/01/90
11/15/90**
11/16/90**
11/19/90
4.S
4.7
4.8
4.6
100
46
141
94
0.7
0.5
0.7
0.9
2350
2400
2375
2390
7.5%***
5. n***
5.8%***
830
817
826
*Amount of the SSM leaving the furnace as ash, preliminary
estimate.
**Tests used for TCLP and heavy metals mass balance.
***Includes estimate of amount of particulate deposited in the
convection pass.
The purpose of the preliminary tests was to optimize cyclone conditions
for the vitrification of the SSM. Because the purpose was to establish run
conditions, clean (unspfked) SSM was used. Furnace optimization included minor
adjustments in the thermal load, SSM inlet location, primary air temperature,
and damper settings to optimize soil melting and throughput. The SSM inlet
location was changed from the scroll burner at the furnace front to along the
secondary air inlet location on the furnace barrel side.
During the four days of tests, the cyclone operation remained very stable.
Soil input was increased from 46 to 141 Ib/hr with test durations of 3 to 6
hours. The slag tapped well, and no buildup of deposits was observed in the
-22-
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furnace. The surface slag temperature was measured using a two-color optical
pyrometer and ranged from 2340 to 2430°F. Measurements of the gas temperature
were not made during the tests. However, previous work with HSM flyash
vitrification showed gas temperatures in the range of 2840 to 2940°F at the
cyclone outlet. The cyclone temperature was adequate to melt the soil, but not
excessive, which could lead to increased metals volatilization.
Description of the Phase II (Wet SSM Feed) Tests
The Phase II test conditions for the preliminary vitrification tests and
heavy metals tests are given in Table 4.
TABLE 4
Phase II Test Matrices
Test
Preliminary
8/20/91
8/21/91
8/27/91
8/27/91
8/28/91
8/28/91
8/29/91
9/03/91
VdW
9/09/91
9/10/91
9/10/91
9/11/91
Cyclone
Load
MBtu/hr
SSM
Feed Stack X
Rate, Excess
Ib/hr Oxygen
Vitrfficatfon Tests [Met,
5.1
5:3
5.0
4.9
4.9
4.9
4.9
5.1
100 0.77
100 0.76
100 0.62
150 0.56
200 0.58
300 0.53
300 0.56
300 0.47
Slag
Temp.
°F
Flyash/
Slag (X)
Primary &
Secondary
Air Temp.
'F
Clean SoilJ*
2455
2420
2370
2410
2410
2390
2405
Metals Jests [wet, Spiked Soil]*
4.8 200 1.2 2430
4.9
4.9
4.9
4 -^***
200 1.0
100 Ofi.
300 0.7
200 4.7
2420
2470
2400
2320
1.77
2.01
1.73
04
0.4
1.49
1.89
1.94
2.32
2.63
3.53
814
794
814
814
810
813
810
807
823
825
813
822
810
*Atomizer air 90 to 130 Ib/hr, 15 to 100 PSIG static pressure.
**Atomizer air flow rates of 128 to 134 Ib/hr were used.
• **10% Borax was added to the SSM.
For Phase II tests the cyclone was operated at a nominal load of 5 MBtu/hr
and 1% excess oxygen. The SSM input was varied between 100 to 300 Ib/hr. The
cyclone operating conditions were relatively smooth, and the longest continuous
operation was six hours at 200 Ib/hr of SSM feed rate.
-23-
-------
The preliminary tests were mainly performed to observe the operational *
condition of the cyclone. Cyclone temperature, SSM feed rate, and slag tapping
conditions of the SBS are the operational variables that were monitored. If too
much SSM is fed to the cyclone, assuming the soil melts, the cyclone throat will
be flooded by the molten slag and slag will stay inside the cyclone and
adversely impact the cyclone operation. Larger particles in the SSM (3/8") will
stay in the cyclone until they melt, but if they do not melt, then they should
leave the cyclone encapsulated by the slag. The slag/large particle removal
from the cyclone essentially determines the maximum load. The cyclone was
operated at a nominal load of 5 MBtu/hr and about 3 to 10% excess air. The SSM
feed was gradually Increased from 100 Ib/hr to the maximum of 300 Ib/hr. The
critical factors were to observe whether the SSM indeed melts down to slag and
if the cyclone taps freely.
When the soil was evenly dispersed around the cyclone barrel, the slag
melted readily. Slag accumulated inside the cyclone (approximately 1.5 to 2
inches) until the slag started tapping. This behavior may be specific to a
small water-cooled cyclone. Cyclone tapping was good until the feed rate
increased to 400 Ib/hr. The cyclone was cold and slag tapping stopped or was
blocked.
Use of a Fluxing Agent to Increase metal Retention in the Slag.
Fluxing agents that cause the soil to melt and tap at lower temperatures
may decrease metals volatilization and, thus, increase the capture of the metals
in the slag. Borax was reported as a fluxing agent for MSW ash vitrification
[5]. For one of the tests during Phase II 10% by weight Borax (20 Ib/hr)
(B4Na20?/10H20)» was mixed with SSM. After Borax was added, the cyclone load
could easily be reduced to 4.1 MBtu/hr without any problem with slagging. With
the added Borax, the slag temperature was reduced from 2430°F (200 Ib/hr SSM
-24-
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feed rate) to 2320°F and NOx levels decreased from 318-337 ppm (200 Ib/hr feed
rate) to 260 ppm, as shown in the Appendix figures. The Borax appeared to
facilitate the movement of slag out of the cyclone furnace barrel. When Borax
was added, the flyash produced increased to 3.53% of the input SSM, presumably
due to vaporization of sodium from the Borax.
Synthetic Soil Matrix (SSM)
The synthetic soil matrix formulated by EPA was used for cyclone testing.
Both clean and spiked synthetic soil matrix (SSM) were obtained from the EPA
Risk Reduction Engineering Laboratory (RREL) Releases Control Branch in Edison,
NJ. SSM, used by EPA for treatment technology evaluations, has been well
characterized in previous studies [1]. The spiked SSM used in this study
contained 7,000 ppm (0.7%) lead, 1,000 ppm cadmium, and 1,500 ppm chromium. For
each project Phase, clean, unspiked SSM (up to 3 tons) was used for preliminary
-25-
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cyclone optimization, and then heavy metal spiked SSM (up to 2.5 tons) was used
for the heavy metals tests.
The SSM moisture content as-received was approximately 20%. For Phase !,
the small amount of spiked SSM used was passively dried in plastic-lined trays,
lumps crushed, and screened to minus 1/4". For Phase II, the moisture content
of the SSM was increased to 24-263 and a wet feed system was installed (see
below) to feed the SSM in this configuration.
Before Phases I and II, analyses were made to characterize SSM to
determine combustion conditions, ash melting behavior and need, if any, for a
slag fluxing agent. The results are given in Table 5. The Phase II results are
for the spiked rather than clean SSM. The soil contained mainly inert
components, low organic carbon (most carbon was present as carbonate), and a low
heat content (41 Btu/lb for clean SSM) . The soil was largely composed of
silicates (50.3%). A significant portion of the SSM consisted of small
particles; 21.4% of the particles were less than 149 microns and 7.4% of the
particles were less than 44 microns. Gravel of up to 1/4" was also present in
the SSM.
-26-
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TABLE 5
Typical SSM Characterization Results (Dry Basis)
Parameter
Moisture
Volatile Hatter
Fixed Carbon
Ash
Heating Value, Btu/lb
Total Sulfur
Total C (corr. for C02)
Total Carbonate, % 0)3
Silicon as Si02*
Aluminum as AljOj*
Iron as Fe2Q,*
Titanium as T102*
Calcium as CaO*
Magnesium as MgO*
Sodium as Na,0*
Potassium as ICO*"
Sulfur as SO,*
Phosphorous as PjQj*
Slag Viscosity (in *F at
250 poise, red. atm.)
Ash Fusion Temp. , *F
Atmosphere
A (I.D.)
B (S.T., SP)
C (S.T., HSp)
D (F.T., 1/16")
E (F.T., Flat)
Phase I
(Dry, Unspiked SSM)
1.2%
18.9%
--
80.3%
41
0.004%
0.64%
15.3%
50.3%
9.2%
3.0%
0:35x
16.8%
3.8%
1.1%
1.3%
0.41%
1.3%
2319'F
red. 0X1 d.
2220 2240
2250 2250
2260 2280
2420 2520
2540 >2750
Phase II
(Wet, Spiked SSM)
20.4%
81.7%
878
._
15.4%
47.0%
8.9%
2.2%
0.35%
15 . 1%
4.4%
0.6%
1.1%
0.70%
0 . 35%
23SO°F
red. OXld.
2250 2240
2280 2270
2290 2300
2600
—
* Ash analysis.
-- Showed no further physical change up to a maximum of 2750°F.
The chemistry of the SSM resulted in a low ash fusion temperature under
oxidizing and reducing conditions and low slag (melted soil) viscosity. This is
essential for the soil to melt and flow during furnace operation and ensure
encapsulation of hazardous constituents and continuous, controlled removal of
the molten slag from the cyclone furnace. The analysis results were similar for
the SSM used for both project Phases. For example, the slag viscosity (T,,
temperature at which the material has a viscosity of 250 poise) of the Phase I
SSM was 2319°F and for the Phase II SSM was 2350eF. The slag viscosity of the
clean, dry SSM enabled it to be treated in the cyclone furnace without the
addition of fluxing agents (coals with similar slag viscosities are known to
-27-
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readily melt in a cyclone furnace). The spiked soil gave slightly higher ash
fusion temperatures than the clean SSM.
Before the Phase I tests, spiked SSH samples were submitted wet
(as-received) and dry (oven-dried at -95oC) for TCLP testing (EPA 1311) for Pb,
Cd, and Cr by Aquatec, Inc. (So. Burlington, VT) to verify that the starting
soil failed the TCLP. The leachability of the lead averaged 81 mg/L; cadmium,
40 mg/L; and chromium, 2.8 mg/L. With the exception of chromium, the spiked
soil exceeded EPA limits for lead (5 mg/L) and cadmium (1 mg/L). This
below-EPA-limit (5 mg/L limit) result for chromium agrees with previous reports
for SSM [I] . The low chromium leachability may be caused by the clay component
of SSM, which may adsorb chromium.
>
Samp1i ng Methods
Sampling and analysis followed guidelines in the U.S. EPA SW-846 Manual,
and the Duality Assurance Project Plan (QAPP) [2] met RREL Category III
requirements. Performance criteria were set for critical measurements (TCLP)
and non-critical measurements (heavy metals mass balance, volume reduction).
Several systems conditions were monitored.
Sampling locations for the various measurements and analyzers are shown in
Figure 7. Duplicate soil and slag grab samples were obtained at approximately
one hour intervals during the heavy metals tests. The soil was collected by way
of a sampling valve in the soil feeder line (Phase I) and by sampling the feed
hopper using a plastic ladle (Phase II). The slag was collected with a steel
shove1.
Particulate loading was measured at a location after the convection pass
and before the baghouse using an EPA Method 5 Train [4]. Stack metals were
measured using the EPA Multiple Metals Train (BIF Method, see Reference 3) with
-28-
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CYCLONE TREATMENT OF CONTAMINATED SOIL
SAMPLING LOCATIONS AND ANALYSERS
CD
BAB
SOIL
ASH
1 5
%
TEMP
0>
AIR
{•'EfcDiiATfc
CO
CCh
ItMP
I
FLY ASH
WATER
SLAG
F1 OKt. ^ S jjiiiJ 11 n
-------
the exception that the HN03 and KMn04 impingers were not used. This exception
was made because previous sampling with the filter temperature held at 120 I
14*Cf as specified in the Multiple Metals Train Method [3], showed no more than
0.2% of the total lead, cadmium, and chromium were present In the impingers.
Metals levels determined using this method should be considered lower estimates.
Post-furnace CO, C02, and NOx levels were measured using continuous emissions
monitors.
*
Analytical Methods
TCLP analyses were performed by Aquatec, Inc. (So. Burlington, VT) using
EPA Method 1311. The metals in the TCLP extracts were determined by EPA Hethod
6010. Total metals In the SSM, slag, and particulates were determined using EPA
6000 and 7000 methods, with the exception that the total digestion of the
samples was performed using a modified ASTH E926-88 (the EPA digestion methods
do not completely dissolve the solid matrix). Preparation of stack samples for
metals determination followed the Multiple Metals Train method. The accuracy of
all metals analyses was verified using check standards from EPA or other
sources. Analyses of the soil for fuel properties, major constituents, and bulk
density were performed using standard ASTH methods. Particle size
determinations were made by way of standard U.S. sieve numbers. Quality
assurance results for the analytical measurements are given in Section 7.0.
-30-
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5. RESULTS
Four major results were obtained from the Phase I and Phase IIstudies.
They are as follows.
1. The Cyclone Furnace successfully vitrified the SSM feed and produced a
leachate that passed the TCLP test.
2. The Cyclone Furnace achieved a volume reduction of 25-35% when
treating SSM during Phase I and Phase II.
3. A majority of the heavy metals in the SSM were retained in the slag
during treatment in Phase II.
4. The Cyclone Furnace operated well during treatment of SSI and produced
no unusually high levels of gaseous emissions.
Each of these results is discussed in more detail below.
Vitrification as Measured by TCLP Test Results.
The pilot cyclone furnace was successfully used to vitrify an EPA
Synthetic Soil Matrix (SSM) spiked with 7,000 ppa lead, 1,000 ppm cadmium, and
1,500 ppm chromium. A photograph of the vitrified SSM is shown in Figure 8.
TCLP results for the Phase I and Phase II heavy metals tests are shown in Figure
9, and original analytical reports are presented in the Appendix. Table 6
Summarizes the results achieved.
-31-
-------
FIGURE 8 Vitrified Synthetic Soil Matrix
-32-
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f<
J 1i
ci
£
1 I
S
fcfcf
» s
CO -:-
to O
< I
3 '
yj ,
5
...
x ;
0
0
§
0
§
„
—
:
„
o
^
is
i
j
n
p
W-
y/K
W-
wx:
5551
^
§J SSM
p
Jw^ p.^*^^
M r^"™111""^ -~^\
SSJU SSM
ibUKt a
Tox i c i ty Cha ractftr i s t i c Leach i ng Procedure- {'!'Cl>') kesu 11 s
-------
Table 6
Results of TCLP Tests for Untreated and Treated SSM
UNTREATED SSM
Cadmium
Chromium
Lead
TREATED SSM
Cadmium
Chromium
Lead
Phase I
mg/L
54.2 ¥ 3.6
2.3 I 1.3
104 ¥34
0.13 ¥ 0.05
0.11 ¥ 0.09
0.20 1 0.06
Phase II
34.2 * 2.9
0.48 ¥ 0.08
74 ¥ 0.0
0.07 ¥ 0.03
0.04 ¥ 0.08
0.20 ¥0.11
With Borax
Flux
30.3 ¥ 0.57
0.20 ¥ 0.11
50.6 ¥ 3.5
0.27
0.02
0.39
Regulatory
Levels ^g/L
1.0
5.0
5.0
1.0
5.0
5.0
All of these treated SSM TCLP results are well below the TCLP regulatory
limits set by EPA. The results show that the cyclone vitrification process
succeeded in producing a non-leachable slag. All of these TCLP results are
close to the analytical detection limit and, hence, the results for both Phase I
and Phase II tests are not significantly different.
The laboratory blank submitted with these samples gave lead, cadmium,
and chromium levels below the detected levels. For two Phase I slag samples,
the measured chromium teachabilities were not significantly different from that
of the laboratory blank.
The reduced TCLP results shown in Table 6 for the SSM from the Borax test
suggest a small amount of stabilization of lead in the SSM occurs by the
addition of Borax. These differences still remain when the dilution of the
sample by Borax is taken into account. This slight trend would have to be
verified by additional sampling; nevertheless, it did not render the SSI
non-hazardous.
The vitrification treatment results in an easily-crushed, glassy product
which minimizes the volume required for landfilling. The slag from the tests
-34-
-------
appeared to be a black, glassy, obsidian-like mass as shown in Figure 8. Some
large, white, glass participates are readily visible in the slag fragments.
When viewed under a low-magnification microscope, both the slag (soil) matrix
and the embedded white particles appeared to have completely melted. Yhen
examined by a Scanning Electron Microscope-Energy Dispersive Spectroscopy, the
white particles are enriched in oxygen and silicon and, thus, may be composed of
silicon dioxide (quartz). The darker regions are enriched in aluminum, iron,
calcium, and magnesium, but also contain oxygen and silicon.
Did the Cyclone Furnace immobilize metal contamination in the vitreous
slag it produced, or did the high process temperatures volatilize all of the
metal contamination? This can be evaluated by calculating the percent of each
heavy metal that was teachable for the untreated and treated soil as given in
Table 7.
TABLE 7
Percent of Leachable Metals Before and After Treatment
(Phase I and Phase II)
Heavy
Metal
Lead
Cadmium
Chromium
Phase
% of Total
Metal Present
That Leached
Before
Treatment
(ssm
29
84
3.8
I
% of Total
Metal Present
That Leached
After
Treatment
(Vitr. SSM)
0.18
2
0.07
Phase
% of Total
Metal Present
That Leached
Before
Treatment
(SSM)
20
57
0.55
2
% of Total
Metal Present
That Leached
After
Treatment
(Vitr. SSM)
0.09
0.70
0.02
The percentage of metals that leached from the slag was less than that for
the SSM feed for each metal tested and for both phases of testing. These
-35-
-------
results indicate that the vitrification process has changed the
physical/chemical form of the soil in such a manner as to render the heavy
metals much less leachable.
Volume Reduction
The treatment of the synthetic soil matrix resulted in a volume reduction
of 25-35% as calculated on a dry basis. Figure 10 shows the volume per ton of
SSM or slag which must be sent for disposal. The volume for SSM (dry basis) and
-36-
-------
SSM VOLUME REDUCTION
CO
«w
o 2
1
u
c
»- 2
OT
u>
0 1
X '
O
1 t
w
1
_j
O
1
1
.
1
1
•'
_
—
***"
—
25%
3S%
SSM
SSM
I
SSM
i!
FIGURE 10
-------
Phases I and II vitrified slag are shown. Approximately 35% and 25% volume
reduction was obtained by vitrification of dry SSM and wet SSM, respectively.
The volume reduction is a combination of 22% mass reduction by calcination of
limestone component of SSM and the increased bulk density from 80 Ib/eu ft for
SSM to 86-92 lb/GU ft for slag. The resulting volume reduction estimate
calculated on a dry basis is conservative since the as-received SSM contained
approximately 25% water, which will be vaporized and contribute further to
volume reduction.
Differences in volume reduction calculated for Phase I and Phase II may
simply reflect the difficulty in obtaining representative samples of the wide
particle size ranges in the slag. Still, the Phase II (25%) volume reduction is
probably a more accurate measurement because special care was taken to assure
that water was removed from the collected slag after the test.
A specific volume reduction for the Borax test could not be calculated.
However, the total volume reduction is expected to decrease because of: (1) the
addition of Borax, and resulting ash, to the feed SSM; and (2) the lower bulk
density of the resulting slag (81 Ib/cu ft) compared with the non-Borax slag
(86-92 Ib/cu ft).
Metals Retention
A mass balance for total ash, cadmium, chromium, and lead was performed
for the cyclone furnace treatment process. A description of the way in which
metal mass balances are calculated as well as examples of the calculation tables
used for the Phase II mass balances are attached in the Appendix. The purpose of
-38-
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the mass balance was to determine the fate of the heavy metals during soil
treatment. During the thermal vitrification process, heavy metals partition
between the vitrified slag and the stack flyash. It is desirable to maximize
the capture of the heavy metals in the non-hazardous vitrified slag.
For the Phase I tests, the overall mass balance achieved was 79 to 103%
output divided by input, and the heavy metals mass balance accounted for 65 to
77% of the input lead, 56 to 61% of the cadmium, and 141 to 145% of the
chromium.
The lead and cadmium were below 100% consistently. Heavy metal deposits
on the wall and convection pass of the furnace were likely the most important
factor in lead and cadmium mass balances below 100%.
In the case of chromium, mass balances in excess of 100% were calculated.
The most likely source of excess chromium was a newly installed refractory which
contains 9.6% chromium oxide (Cr2Qj}( and "bake-out" or abrasion of the material
elevated the stack chromium levels.
Analytical accuracy is also a source of errors. As a part of analytical
quality assurance, spike samples, containing a known amount of heavymetals,
were measured. Cadmium and lead in the slag were detected within 15%.
An additional source of error may have been in the assumption that no
vapor phase metals exist after the Multiple Metals Train filter, operated at
120°C.
For the Phase II tests, the overall and heavy metals mass balance were
-39-
-------
closer to 100%. An overall balance achieved 102 to 107% input, and the heavy
metals mass balance accounted for 74 to 87.5% of the lead Input, 50.5 to 71.5%
of the cadmium, and 78.9 to 96.8% of the chromium. The use of chromium
refractory was minimized to prevent any chromium contamination.
Determining the fate of heavy metals in the cyclone furnace depends upon
determining the relative amounts of SSM that leave the cyclone furnace in the
slag and fly ash and a determination of the concentration of metals in each of
those streams. Since the exhaust gas from the cyclone is cooled to 120*F prior
to release to the atmosphere, all of the metals that escape the cyclone furnace
should be captured in one of these two solid streams. None of the metals should
be present In the exhaust gas in the gas phase. A discussion of the relative
mass flowrates of the fly ash and slag streams and of the relative metals
concentrations in each is presented below.
-40-
-------
Mass Flowrates of the Fly Ash and Slag Streams
Tests showed 95 to 97% of the non- combustible portion of the input SSM
was incorporated within the slag. The amount of SSM leaving the furnace as
flyash was approximately 5-7%. Because the generation of flyash will be partly
a function of fuel particle size, and because drying the SSM produced a finer
particulate, this 5%-7°/o estimate is higher than that found for a wet feed
system. A portion of the heavy metals from the SSM will condense on the flyash.
This flyash residue may be treated by another technology or simply be recycled
to the cyclone for further treatment.
The Borax flux added during one of the Phase II tests, appeared to
facilitate the movement of slag out of the cyclone furnace barrel. When Borax
was added, the flyash produced increased to 3.53% of the input SSM, presumably
due to vaporization of sodium from the Borax.
Relative Concentrations of Metals in the Slag and Fly Ash
During the Phase I and Phase II heavy metals tests, soil and slag samples
were collected, composited, and analyzed. The total metals results, averaged
and reported on a dry basis, are given in Table 8.
-41-
-------
TABLE 8
Total Metals in Soil, Slag, and Multiple Metals Train
Particulates
Total Metals, ppm (rag/kg)
Sample
Phise 1
CoiiiDOSltt Soil (Orv SSM)
46 Ib/hr
141 Ib/hr
reagent blank
Cadmium
1316 1 40*
1223 ? 34
<0.05
Chromium
1391 ?86
1339 ? 93
<0.05
Lead
8007 ? 248
73901214
<0.05
Composite Slag
46 Ib/hr
141 Ib/hr
reagent blank
HuUlole Heta1s_Tra1n Partlculates
46 Ib/hr
141 Ib/hr
filter blank
Phase II
Composite Soil (SSM.
100 Ib/hr
200 Ib/hr
300 Ib/hr
200 Ib/hr + Borax
reagent blank
Composite Slag
100 Ib/hr
200 Ib/hr
300 Ib/hr
200 Ib/hr + Borax
reagent blank
Drv Basis)
101
134 T 3.2
<0.05
15146
14816
15
1227
1261?17
1329
1259
<0.5
113
190 ? 6.
179
284
<0.2
1907
2169* 147
<0.05
12493
9893
108
1527
1550 ? 14
1594
1565
<0.5
1455
1488 ?10
1421
1208
<0.2
1624
2432T221
<0.05
80414
99880
149
7198
7708 ? 110
7701
7838
<0.5
2077
3592 T 56
2552
3834
-------
When compared with the soils metals levels, the slag was relatively enriched in
chromium and depleted in lead and cadmium. The capture of heavy metals in the
vitrified slag from all tests ranged from 8-17% for cadmium, 24-35% for lead,
and 80-95% for chromium.
Addition of 10% of a Borax flux did not significantly improve the heavy
metals capture in the vitrified slag despite a decrease in cyclone operating
temperature of approximately 10§*F.
Several other trends can be seen from this data. The capture of heavy
metals in the slag increased with increasing feed rate, likely due to shorter
cyclone furnace residence times. As expected, less volatile metals were more
readily captured in the slag. The capture of metals in the slag increased with
decreasing metal volatility. This suggests the cyclone vitrification process
would be well suited to treatment of low volatility contaminants, such as many
radionuclides.
Lower cadmium, chromium, and lead levels were observed in fly ash from the
Borax tests. More fly ash was generated for the Borax tests, however. Thus,
metals Missions rates were only slightly lower for the Borax test.
Figure 11 shows the estimated overall split of heavy metals betweenflyash
and vitrified slag. For the Phase I dry soil feed, from 8 to 17% cadmium, 24 to
35% lead, and 80 to 95% of chromium were retained in the slag. For the Phase II
wet soil feed system, from 12 to 23% cadmium, 38 to 54% lead, and 78 to 95% of
chromium were retained in the slag. The ranges were determined using
non-normalized and normalized concentrations of heavy metals as determined by
mass balance (see Section 5.0, D).
-43-
-------
INPUT
SLAQ
ASH
A. PHASE 1 (DRY SOIL, 141 LB/HR)
Cd
8 to 16
24 tO 35
TO
m
80 TOM
B. PHASE 2 (WET SOIL, 200 LB/HR)
12 to 23
ASH
CORY BASIS)
TO 54
Cr
S
TO
ASH
(DRY BASIS)
3.3
78 to 95 96.7
FIGURE 11 Heavy Metals and Ash Mass Salance
-44-
-------
Figure 12 shows that heavy metals content in the slag increases with
increasing SSH feed rate between 50 to 300 Ib/hr. Since fuel (natural gas) feed
was relatively constant, this suggests that increasing SSM feed rate reduces the
solid residence time (and/or slag temperature, see Appendix figures) in the
cyclone furnace and, consequently, reduces vaporization of heavy metals into the
flue gas. This increasing capture with feed rate shows some promise for further
metals capture optimization, and is an encouraging trend for process scale-up.
An attempt was also made to correlate the different behavior of the metals
during cyclone treatment with their volatility. The temperature at which the
metal vapor pressure was 100 iw Mercury was chosen as the volatility parameter.
Figure 13 shows the heavy metals retained in the slag as a function of
volatility of the metal. A marked trend was obtained, and we concluded that
increasing volatility is the dominant factor over the fate of heavy metals.
Figure 13 shows the volatility of the metal is inversely proportional to the
slag metal concentration. These results suggest that the cyclone vitrification
process may show very high capture for very low volatility contaminants, such as
many radionuclides. Conversely, high volatility metals are likely to be
concentrated in the flyash which may then be suitable for metals recovery.
Intermediate volatility species, such as lead, are captured to some degree in
the flyash and may be recycled to the furnace to increase the overall capture of
the metal in the slag.
Figures 11 and 13 suggest better capture of the metals in the slag for the
Phase II wet feed system compared with the Phase I dry soil feed system. The
reason for the improved capture may be a combination of any of the following:
(1) increased feed rates, resulting in lower slag temperatures and, thus, less
metals volatilization; (2) reduced soil residence time in the furnace and, thus,
less metals volatilization; or (3) larger particle size distribution in the wet
-45-
-------
FEED RATE AND HEAVY METALS CAPTURE
4.0
I-
Ifl
g 3d
2.0
I
0,2
i
i
-O
100 ISO
SStt
250
FiCtLWt 12 Heavy Me tils iip-Wre v^
-------
VOLATILITY & HEAVY METALS CAPTURE
90
I AMD II
w
m
1
s
z
50
30
10
D
A
O
Cr
O
A
I I t 1 1 1 1 1 i i 1 t 1 i t I.
_t__j_
§00 800
100 mm Mg
'IGURt 13 Hetdls Captyre vs. Volatility Temperature
-------
SSM, thus reducing the surface exposed for metals volatilization.
With the possible exception of cadmium, the addition of a 10% Borax
fluxing agent did not significantly improve the capture of the heavy metals.
For the Borax test; from 17.9 to 30.5% cadmium, 37.8 to 54.7% lead, and 62.8 to
91.7% of chromium were retained in the slag. The Borax flux reduced the slag
temperature from 2430°F to 2320°F by reducing the natural gas load from 5 to 4.1
MBtu/hr. Only for the most volatile metal, cadmium, does this temperature
difference appear to affect volatilization. This small improvement in cadmium
capture Is offset by an increase in volume to be processed (and, thus, decrease
in volume reduction for a given weight of SSM treated) and an Increase in the
weight of potentially hazardous flyash stream. Still, the Borax improved soil
melting and tapping from the furnace. If a small amount of Borax can improve
soil melting, the feed rate may be increased for a given heat input rate.
Operab i1i ty/Em i ss i ons
Stable cyclone operation was achieved during the pilot tests.
Post-furnace CO, C02, and NOX levels were measured using continuous emissions
monitors, Average levels measured during the heavy metals tests are given in
Table 9.
TABLE 9
Average Phase I CO, C02, and NOx Levels (Spiked SSM)
Measurements
Cyclone Stack CO, Stack Nox
Load Feed Rate , PIP at Stack 0)3 , ppm at 3%
Test MBtu/hr lb/ hr 3% 0, % Oz
11/15/90 4.7 46
11/16/90 4.8 141
18 11.4 365
19 11.5 319
-48-
-------
Although the NOx levels are relatively low, the measured NOx levels can be
further reduced, if desired, by application of NOx reduction technologies. This
may be necessary for wastes intrinsically high in nitrogen compounds which
produce higher levels of NOx emissions. Carbon monoxide (CO) levels were very
low, indicating stable combustion. The C02 levels measured are typical for
combustion of natural gas.
The slag did not appear homogeneously melted; larger particles appeared
unmelted, but after viewing under a microscope, the particles appeared
completely melted.
Average post-furnace NOx, C02, and CO levels for the five heavy metals
tests in Phase II were 322 ppm, 10.5%. and 27 ppm, respectively (see Appendix
for specific measured values). These levels are similar to those measured in
Phase I. The Appendix contains graphs of NOx levels and slag temperatures
plotted against feed rates for the preliminary and heavy metals tests. As
expected, the NOx levels decrease with increasing SSM feed rates (and, thus,
cyclone temperatures). The slag temperature was sensitive to the SSI feed rate;
it decreased from 2470 to 2400°F.when SSM feed rate increased from 100 to 300
Ib/hr, respectively (see Appendix figures). The flyash (measured at convection
pass exit) remained low, at approximately 2% of SSM input (See Appendix Dust
Loading data).
Some operability problems and feed rate will be improved by full-scale
design and operation. For example, the surf ace-area-to- volume ratio of the
pilot unit is much larger than that expected for a full-scale unit. This will
decrease the heat input required to melt a given amount of soil.
With the added Borax, the slag temperature was reduced from 2430°F (200
Ib/hr SSM feed rate) to 2320°F and NOx levels decreased from 318-337 ppm (200
Ib/hr feed rate) to 260 ppm, as shown in the Appendix figures.
49-
-------
6. QUALITY ASSURANCE
Quality assurance systems audits and a performance evaluation audit were
conducted by the B&W Quality Assurance Unit. The activities included an audit of
the instruments and calibrations, heavy metals tests soling procedures, and an
audit of the Aquatec laboratory (Phase I). Audit and performance results are
summarized below.
Systems Audits
During Phase I, the systems audit of the instrument calibration found that
the transducer used for the indication of secondary combustion air flow rate was
calibrated to an accuracy specification of 0.4% of span (0-5 volts). The
manufacturer's specification for accuracy deviation is 0.2% of span and, thus; the
instrument was out of calibration. Because secondary air flow rate is not a
critical measurement, this deviation had no impact on the project. During Phase
I, the sampling objective of 30-minute intervals for sequential soil (SSM) and
slag samples was not met because the sampling times required to obtain a given
weight of soil from the soil sampling valve were longer than anticipated (up to 35
minutes per sample). Thr impact of this deviation from the Quality Assurance
Project Plan (QAPP) was minimal because the soil sampling was nearly continuous.
A second sampling deviation was the use of a metal shovel to collect the slag from
the slag tank. Ideally, metals collection devices should be avoided for trace
metals sampling; however, plastic and glass devices could not be used. The effect
of metals introduced from the shovel, if any, would result in a more conservative
estimate of the metals teachability.
During Phase II, the systems audit found, for two multiple metals trains
(16:10 and 17:44 on 9/9/91), the pump was turned off before removing the probe
from the stack, while Method 5 specifies that the probe is removed before the pump
is shut off. The impact of this deviation is thought to be negligible. The train
performed at 16:10 (200 Ib/hr test) omitted the 0.1N HNOs probe rinse specified in
the Multiple Metals Train procedure [3]. For the train run at 17:44 (also 200
Ib/hr test), the percentages of the total cadmium, chromium, and lead found in the
0.1N HNOj rinse were 2.6, 4.9, and 2.4%, respectively. This can be compared with
-50-
-------
the relative percent difference for the total cadmium, chromium, and lead
collected by the two trains which was 25, 4 and 2.5%. respectively. Thus, for
chromium and lead, the differences in the total particulate metals found can be
completely explained, by losses due to omitting the 0.1N HNOj rinse (with an
overall impact of a few percent difference). The omission of the 0.1N HNOj rinse
explains only a small portion of the differences for cadmium. Thus, the effect of
omitting the 0.1M HNO| rinse is insignificant for cadmium. Bacause the
particulate stream is a small portion of the overall materials balance for the
cyclone process, the differences introduced by omitting the 0.1H HNOj rinse are
not thought to significantly affect the mass balance results for the project.
The QAPP specified that ASTN Method E886 be used for the digestion of soil
and slag samples for total metals. However, to achieve complete digestion of
these matrices, modifications to the ASTN method were required. The Modified ASTM
E886 Method is attached in the Appendix.
Performance Audits for Critical Measurements
The quality assurance results for the critical measurements, TCLP of the SSM
feed material, and the vitrified soil product are given in Table 10. The TCLP
analyses met Performance Evaluation objectives based on results for EPA check
standards of 97.2*91.5X, compared with an acceptance criteria of 90-110%.
Detection limits surpassed those specified in the QAPP. matrix spikes ranged from
79-152% recovery for Phase I and 25-118% for Phase II, which exceeded the cadmium
and lead QA objectives, but was within expected performance for environmental
matrices. Because the measured values were orders of magnitude above or below
the TCLP limit, exceeding this criterion should not affect conclusions made
regarding whether a sample met or exceeded TCLP limits.
For the TCLP leaching analyses, precision was determined by duplicate
determinations of one slag and one soil during each heavy metals test. The
precision for several of the measurements'exceeded the QA objective of 20%
relative percent difference (% RPD) . Precision objectives may have been higher
than can reasonably be expected of these samples (indeed, 50% is generally
considered excellent precision for environmental samples). The lack of precision
for certain soil TCLP analyses may have been due to the heterogeneous nature of
the soil matrix. The soil contains a wide range of particle sizes,
-51-
-------
TABLE 10
QA Data for TCLP Analyses
Cadmium
Quality assurance
Parameter
Phase 1
Accuracy , %
Precision, %
soil*
slag*
TCLP Detection
Limit, n/l
Phase II
Objective
50-150
20
20
10
Found
100-138
2,2
6,43
9.1
Chromium
Objective
50-150
20
20
20
Found
79-107
4,98
41,91
10.6
Lead
Objective
50-150
20
20
5
Found
108-152
11,64
9,25
1.3
Accuracy, %
Precision, %
50-150
39.7
50-150
100-118
50-150
25-50
soil*
slag*
TCLP Detection
Limit, fiq/L**
20
20
10
5,3
29,6
10
20
20
20
3,1
62,26
10
20
20
5
'6,10
22,3
5
• Data for two determinations (one for each heavy metals test).
**Data from blank determinations used.
which stratify in layers, making representative sampling more difficult. A relative
enrichment in smaller particles relative to the bulk sample would increase the detected
metals (small particles contain higher amunts of the contaminants because of their
relatively high surf ace-to-volume ratio). Because the soil samples already exceeded the
TCLP limits for lead and cadmium by 20-50 times, the higher-than-expected relative
percent difference has no impact on the project. For example, for lead in one soil
sample, a relative percent difference of 64% would still result in a soil which fails
the TCLP by one order of magnitude.
The precision for a number of slag TCLP leaching analyses also did not meet the QA
objectives. This was likely due to the very low levels of teachable metals in these
samples that gave results near the analytical detection limits. As measurements
approach the detection limit for an analytical method, the relative percent differences
between duplicates is expected to increase. This was especially evident for the
chromium measurements (up to 91% RPD). For example, for the three slag samples analyzed
from the Phase I 11/15 test, one sample was measured to be at the detection limit, one
at 1.5 times the detection limit, and one was at 4 times the detection limit. Because
the slag samples were below the TCLP limits for lead, cadmium, and chromium by one to
-52-
-------
two orders of magnitude, the higher-than-expected relative percent difference has no
impact on the project.
Performance Audits for Non-Critical Measurments
The quality assurance objectives and results for the non-critical measurements
(total metals analysis) are given in Table 11. The metals analysis met QA data quality
objectives for accuracy based on recovery of check standards added to matrix spike
samples. Precision, determined from duplicate (or more) analyses of samples, exceeded
the QA objective of 20% relative percent difference, with the exception of cadmium in
the multiple natals train in Phase II (the precision appears to be related to the
volatility of a given metal and may reflect differences in combustion conditions rather
than analytical differences). Laboratory blank levels were well below the detected
levels for the metals determinations. For the multiple metals trains, the acceptance
criterion for percent isokinetic sampling was 90-110%. For Phase I and Phase II tests,
percent isokinetic sampling was 99-101%, which exceeded the acceptance criterion.
The non-critical measurements included analyses of check standards during
continuing calibration. Recalibration was performed when continuing calibration
standards failed to meet the 90-110% acceptance criterion stated in theQA Project Plan
-53-
-------
TABLE 11
QA Data for Non-Critical Metals Determinations
Cadmium
Chromium
Lead
Quality
Assurance
Parameter
Phase /
Accuracy, %
soil
slag
Precision, %
soil
slag
MMTS
Phase //
Accuracy, %
soil
slag
Precision, X
soil
slag
MMT*
*Multiple Metals
Objective
50-150
50-150
20
20
20
50-150
50-150
20
20
20
Train
Found
81
114
2.6-4.3
1.9-6.4
5.9
107
92.0
0.7-5.5
0.5-4.4
25
Objective
50-150
50-150
20
ao
20
50-150
50-150
20
20
20
Found
106
88
1.6-12
4-13
5.2
103
96.9
0.3-3.4
1.1-4.7
4
Objective
50-150
50-150
20
20
20
50-150
50-150
20
20
20
Found
77
110
3.8-5
1.7-17
10
96.8
95.6
0.3-5.0
0,08-2.1
2.5
-54-
-------
7. CONCLUSIONS AND RECOMMENDATIONS
Conclusions
The following conclusions can be drawn about the ability of the cyclone
furnace to process organic and heavy metal contaminated soil based upon the
results of the Phase I and Phase II tests. These conclusions are as follows.
1. The Babcock & Wilcox six million Btu/hr pilot cyclone furnace was
successfully used to vitrify an EPA-Synthetic Soil Matrix (SSM) spiked
with 7,000 ppm lead, 1,000 ppm cadmium, and 1,500 ppm chromium. When
operated at 50 to 150 Ib/hr of dry SSM feed, and from 100-300 Ib/hr of wet
SSM feed, the cyclone technology was able to produce a non-teachable
product (well below TCLP limits).
2. The cyclone vitrification process would be well suited to treatment of low
volatility contaminants, such as many radionuclides. At least 95 to 97% of
the input SSM was incorporated within the slag. During the thermal
vitrification process, the heavy metals partition between the vitrified
slag and the stack flyash. The capture of heavy metals in the slag was
found to increase with increasing feed rate and with decreasing metal
volatility.
3. Stable cyclone operation was achieved during the pilot tests. Using
natural gas as the fuel, the CO and NOx, stack emissions gases from the
process were within acceptable ranges.
4. The treatment of the synthetic soil matrix resulted in a volume reduction
of 25-35% (dry basis). Vitrification results in an easily- crushed,
glassy product.
Recommendations for Future Work
The cyclone furnace may be best suited to the treatment of soils
contaminated by organics and either very high- or low-volatility
metals/radionuclides. This statement can be explained as follows:
(1) the high heat release rates and turbulence make the cyclone
vitrification process well suited for organics destruction;
(2) vitrification of very high-volatility metals or radionuclides would
tend to concentrate those elements in the relatively small flyash stream,
which may then be suitable for recovery;
(3) vitrification of very low-volatility metals or radionuclides would
tend to concentrate those elements in a non-teachable product (the slag)
-55-
-------
and produce only low flyash levels. Such elements are present at
Department of Energy and Department of Defense contaminated soil sites.
Feasibility for these elements will be verified in the SITE Demonstration.
For intermediate volatility metals/radionuclides, the best process option may be
to recycle the flyash to the furnace in order to maximize the capture of heavy
metals in the non-leachable slag and minimize the size of the flyash waste
stream.
The flyash recycling concept should be demonstrated on a pilot- scale
process to verify feasibility and potential advantages. The effect on the
percent capture of metals in the slag and TCLP performance should be evaluated.
Even if recycling proves undesirable, the heavy metals are contained in a
relatively small flyash stream that may then be stabilized for disposal. This
represents a much smaller stream requiring hazardous waste treatment and
disposal (3-5% of the original contaminated soil).
The heat input for a given rate of soil feed for the pilot-scale unit
should be improved in the field-scale design. This improvement will comefrom
lower cooling surf ace-to-furnace-volume ratios which will result in lower heat
losses from the unit. The feed rates achieved during this project are likely
minimum values because of the limits imposed by working with a cyclone furnace
designed for coal combustion rather than waste vitrification. Feed rates will
be increased by improved gas burner design and placement for a vitrification
application.
In addition to the Emerging Technologies effort, a U.S. EPA SITE
Demonstration of the cyclone furnace was performed in November of 1991. Heavy
-56-
-------
metals, volatile and non-volatile radionuclides, and organic hazardous
constituents were spiked into the synthetic soil matrix. Measurements will be
made to verify previous TCLP leachabilities, volume reduction, and heavy metals
capture in the slag. DRE's for organic contaminants will be measured. The
immobilization of radionuclides will be measured using American Nuclear Society
leaching procedures. Conventional air pollutants will be measured to test
regulatory compliance. Potential technology applications and estimated process
economics will be addressed.
Based on the results of the SITE Demonstration, BiW will assess the
further development/commercialization of the cyclone vitrification process.
Conceptualization and design of a full-scale system have not been performed. An
important next step is the design, fabrication, and demonstration of a
full-scale vitrification furnace. The operation of a full-scale unit can be
used to obtain accurate process economics.
-57-
-------
8. REFERENCES
1. P. Esposito, J. Hessling, B, Locke, M. Taylor, M. Szabo, R. Trumau. C.
Rogers, R. Traver and E. Earth, "Results of Treatment Evaluations of a
Contaminated Synthetic Soil," JAPCA. 39: 294 (1989).
2. RREL Quality Assurance Project Plan No. P-309-B. submitted by B&W to RREL
July 2, 1990, and Phase II modifications submitted by letter to RREL
August 28, 1991.
3. "Methodology for the Determination of Trace Metal Emissions in Exhaust
Gases From Stationary Source Combustion Processes," Subsection 3.1 of the
Methods Manual for Compliance with BIF Regulations (EPA/530-SW-91-010,
December 1990).
4. 40 CFR 60, Appendix A, July 1990, Method 5.
5. J. Nowok and S. A. Benson, University of North Dakota, Gas Research
Institute Report No. GRI-89/0078.
-58-
-------
9. APPENDIX
Calculation of Heavy Metals Mass Balance
A mass balance for total ash, cadmium, chromium, and lead was performed
for the cyclone furnace treatment process. The purpose of the mass balance was
to determine the fate of the heavy metals during Phase I (at 46 and 141 Ib/hr)
and Phase II (200 Ib/hr and Borax test). Proximate and ultimate analysis was
performed to determine the volatile compounds (e.g., CO, from CaCOj) In the SSM.
Each day the soil feeder was calibrated before and after the tests, and an
average feed rate was used. Each day's slag was collected and weighed. The.
weight was corrected for water. The particulate loading of flyash to the stack
was isokinetically measured and averaged. Some flyash also deposits in the
convection pass or on the furnace walls. The convection pass flyash deposit
could not be measured, but was estimated at 50% of the stack flyash. This was
based on the amount of convection pass deposit that has been measured previously
with Ohio #6 coal flyash (50% of stack flyash).
To determine the mass balance, total heavy metals analysis was performed
on the feed SSM, vitrified slag, and captured flyash. For each test, duplicate
Hultiple Metals Trains were collected and heavy metals were determined (with the
exception of the Borax test, where only one train was performed). Slag and feed
soil (SSM) samples were collected at approximately one hour intervals. The
samples collected were composited and analyzed for total heavy metals in
duplicate or triplicate. The volatile matter, slag, and flyash loading were
normalized to 100% of dry, C02-free SSM. The results consistently showed that
flyash loading was very small (5% or less of the SSM input).
-59-
-------
A normalized and non-normal!zed mass balance was calculated as follows:
(1) The amount of SSM, flyash, and slag was measured for each test,
(2) A material balance was performed on the SSM and combination of
flyash, slag, SSM water, SSM CO, in the flue gas (achieved 79 to 103%
input for Phase I and 102 to 107% input for Phase II).
(3) The flyash and slag streams were normalized to 100%, assuming the
average of the SSM feed rate measured before and after the test.
(4) Using the normalized ash and slag percentages, performed a mass
balance on lead, cadmium, and chromium (mass times concentrations).
This mass balance in Phase I accounted for 65 to 77% of the input
lead, 56 to 61% of the cadmium, and 141 to 145% of the chromium
(chromium result discussed in Section 6.0, H), and in Phase II
accounted for 74 to 87.5% of the lead input, 50.5 to 71.5% of the
cadmium, and 78.9 to 96.8% of the chromium.
(5) The mass balance was normalized to 100% (100% = amount of heavy
metals measured in input SSM using the SSM rate and the SSM metal
concentrations -- this assumes the SSM input rate and concentrations
were the most accurately measured parameters).
(6) The mass balance range reported was the percent mass balance for the
slag with the lower end of the range being the_non-normal 1 zed, data
and the upper limit being the normalized data to which 15% was added
to account for analytical error. The mass balance range for the
flyash was calculated from (100 the slag range).
-60-
-------
Dust Loading Data
Date
Soil Moisture Content (%)
SiacTAsHj^Torivut
Stack Pressure,* Water
Dust Sample, (g)
Flue Gas Sampled, (CuFl)
Temperature, (F)
Sample Flue Gas Mass, (to)
Total Flue Gas, fto/hr)
Barometric, "Hg
Stack Abs Pressure, (psl)
Gas Mol WetQht
920-91
25
1.77
0.55
046
3047
101
2.14
2793
28.76
14.14
29.64
i^ffc. *"•**/•••
6-21-91
25
201
055
0.51
30.42
103
214
2874
2892
14.21
2984
6-27-91
25
173
055
031
2594
114
179
3416
29.01
14.26
2964
w~* r\&jr
8-2791
25
04
055
007
2527
118
1.73
3360
2900
14,26
2984
82891
25
191
055
050
2507
114
1.73
3386
2903
14.27
2985
82891
25
1 49
055
051
2463
120
169
3361
2902
1427
2985
Identification Number
Dale
Soil Moisture Content (X)
Stack Ash,(%) of Input
Slack Pressure," Water
Dust Sample, (g}
Flue Gas Sampled, (CuFQ
Temperature, (f\
Sample Flue Gas Basi^ J6J__
Total Ftue Gas, (t»mr)
Baromeiric, "Hg
Siach Abs P'essurejjfwll
Gas Mol Weight
007-A10
82991
25
189
055
1.02
25.71
112
, 1.79
3383
2904
14.28
2965
009 A1 2
9391
25
1.94
055
1.02
2571
112
1.79
3474
29.04
1428
2966
•
*?
Identification Number
Date
Soil Moisture Content (%)
Stack Asn,(%) of Input
Stack Pressure,* Water
Dust Sample, (g)
Flue Gas Sanded, (CuFl)
Temperature, (F)
Sample Flue Gas Mast, (to)
Total Flue Gas, (IVhr)
BarometriCj, "HQ
Stack Abs Pressurej (psij
Gas Mol Wetght
-------
SBS DATA AVERAGES
ooT-Aca
Cyclone
W
OM
W"
CO
T
NOB
"iii"
!<}*
U
MO
~m
~w
is
¥
"SRT
_f_
adT-'tef
4 I
BO
WTO
IB
isr
in
a an
208
In
ggg;
111
Ps>
-------
SBS
CTk
-------
II Metals
Test
%
to 1
AO1
A02
A0S
201,90
186.15
2.32
2LK1
asa
68. n
«i 1 1
107^34
107.66
102.12
208
2.3S
3.42
61.02
60.75
57.12
• CO2 dry Hindi 10%
-------
en
SOIL
HEAVY METALS
TCLP
ASH MELT PROPERTIES
MAJOR CONSTITUENTS
% MOISTURE
BULK DENSITY
FEED RATE
CYCLONE
FURNACE
TEMP
92
COMB. AIR
SLAG QUENCH
WATER
POST FURNACE
HEAVY METALS
PARTICULATE LOADING
(ASH/SLAG SPLIT)
MAJOR CONSTITUENTS
GAS VELOCITY
FLUE GAS
CO
BAGHOUSE
TEMP
J
i
FT.Y ASH
SLAG
HEAVY METALS
TCLP
BULK DENSITY
MAJOR CONSTITUENTS
SLAG TEMPERATURE
rt .
7.
Sampling locations and analyses for the Phase I and Phase II heavy metala tests used for the heavy
metals mass balance, TCLP leachability, and volume reduction.
-------
II and for Soil,
and Fly Ash
Test
Sol Slag
% d Input
Stag
put,
Lead
Cadmium
?S36
1281
1S44
18?
11720
7874
38.0
ll.t
. 79.3 1
mo
i_ ms
14.21
74.0
50.5
83, S
SI .3
23.7^
84.8
_,_,,_,
I
m
— ]
?§SS
1246
1640
3S70
186
jfUfmr"* i
W sir ?r 1
LBad
Cadmium
Gtvanlunk
' ?838
125S
15611
3SS1
197
1461
we?
37-9
12.1
78.4
49 S
89.4
18.4
i?.sT
71.5
96.8
43,3
81.0
56.7
83.0
Lead
1261
1SSO
3K?
190
1466
64S1
37.6
12,3
ms
42.21
48.5
is. i
796
60.8
L 94.4
47.1
20.2
82.9
S2.9
79.8
17.1
ty| |^Q|
Tiaiwih
Lmml
GcvJbniuni
i»liyfiikjiri
&2i8
Id^l
t6l/
Joiii
2fW
1ZIU
/UWJV
V31O3
17.9
68,8
«i,5
1 j
16.0
79.3
67.S
78.9
47.6
28,5
79.7 :
S2.4
73.5
20,3
-------
CTl
~~l
I
On
(X,
N— '
1
m
O at
2
Clean Soil Testing
Soil
a
B3
Soil Feed Rate
-------
MTO
Clean Soil Testing
Slag Jemof ratu res
CD
I44t
S
w
MM
uw
Soil Disperser Air Range: 9CM3Q (fb/hr)
Total Load; 4J-5.3 (MBtu/hr)
K)
ca
Soil Feed Rite (LB/11R)
-------
H»
Heavy Metals Testina
o
Mo |M
12JB
*> 2f»
O
O
U
/ \
/
4.14 \
Air: 134 ' x,
lit
Soil feed
-------
JU*
E
2
Spiked Synthetic Soil Matrix
(ill)
No Ois Air 128
63
o
I
WJ
-2
t/i
.$Jr 134
oat
J*»
S<«1 Feed Rile
.M*
-------
71-
-------
72
-------
o
aquatec
KHVIHONHtHTAL ffUVfCffJ
75 Cron MountMi Dnvn, 5c. Buribifton, VT W403
ret, ao2/4Si-io?4
Babcock * Wilcox Company
R&D Division, Att: A/P
1562 Beeson Street
Alliance, OH 44601
Attention
Date : 12/07/90
ETR Number: 24003
Project No.: 90000
No. Samples: 24
Arrived : 11/16/90
P.O. Number: 537-OA247838
Jean Czuczwa
Page
Itondortf tnolyM* tor* porforaod In accordrc* wtth Nothodt for Analysis of W««r and UMtM, M
T««t H«Thod» for IvituBtinf Mitd UMt«, »-»**, or Stindvrd H»thod» for tit* iMMifwtion of y«t*r «rd
All rowlts *r« in ••/( unlots oth«m
Comments/Notas
73
-------
o
aquatec
smmmmorrM, sutmxs
75 Crws Moan*** Ortm So. fceitngK*. VT
TtL UZ/«a*. 10?4
Babcock 4 Wilcox Company
RtD Division, Att:A/P
1562 Beeson Street
Alliance, OH 44601
Attention : Jean Czuczwa
Dat* :
ETR Numb«r:
Project No.:
NO. Saapl**:
Arrived :
12/07/90
24003
90000
24
11/16/90
P.O. Nu*b«r: 537-OA247838
Page
Stindwd arw
for
Lab No./
Method NO.
in •ccardrc* wit* Method* for Wly»l» »f Mt«r wri UMIM, IM-600/4/79-020,
UMta, w-t*4r or *tirdw4 M*tNxt» for t»i
All rMuiu ar* tn >«/l in I Ma •ttwrwiM not«d.
Sample Description/
p«ram«t«r
R«»ult
124383
125162
Slag-Spik« 2, 1419:(TCLP Ext)
6010 Cadmium, Total
6010 Chromium, Total
7471 Lftad, Total
Slag-SpiKi
6010
6010
7421
2, 1419:[MS](TCLP Ext)
Cadaiiuai, Total
Chromium, Total
Laad, Total
124382DP Slag-Spike 2, 1419: [RZP] {TCLP Ext)
6010 CadmiUB, Total
6010 Chromiua, Total
7411 L«ad, Total
170 a
74 a
155 a
220 a
166 a
210 a
110 a
49 a
121 a
124384 Slag-Spike 2, 1534-1543:(TCLP Ext)
6010 Cadmium, Total
6010 Chromium, Total
7421 Laad, Total
124386 Slag-Spike 2, 1730-1750:(TCLP Ext)
6010 Cadmium, Total
6010 Chromium, Total
7421 Lead, Total
53 a
<20 a
125 a
166 a
36 a
132 a
ComB«nts/Not«s
a * ug/1
< Last Pag« >
Submitted By
: //Jl.
Aquatec Ir.c
-74-
-------
o
aquatec
CMyiftOMMtMTAL S0IVICSS
75 Citwn Mount** Dm*, So, Bwriwftim. VT SS403
TIL. HB/tM.1074
Babcock & Wilcox Company
RiD Division, Att: A/P
1562 Beeson Street
Alliance, OH 44601
Attention : Jean Czuczwa
Date :
ETR Number :
Proj ect No.:
No. Samples:
Arrived :
12/07/90
24022
90000
22
11/16/90
P.O. Nuaber: 537-OA247838
Page
In ac««r«lv«« nith
for IwMtwtinf Jolld UMfc, sy-S^A, or
All r«Kiitt ar* In i^/l
Lais No,/ Sa«3l« Description/
Method Ho. " Fmran*t*r
fw»
far t!M
not»d
of
124517 Soil-Spike 3, 1245-1310:(TCLP Ext)
6010 Cadmium, Total
6010 Chromium, Total
6010 Lead, Total
124517MS Soil-Spike 3,
6010
6010
6010
1245-1310:[MS] (TCLP Ext)
Cadmium, Total
Chromium, Total
Lead, Total
124517DP Soil-Spike 3, 1245-1310:[REP] TCLP Ext)
6010 Cadmium, Total
6010 Chromium, Total
6010 Lead, Total
124519 Soil-Spike 3, 1420-1433: (TCLP Fxt)
6010 Cadmium, Total
'6010 Chromium, Total
6010 Lead, Total
124521 Soil-Spike 3, 1642-1648:(TCLP Ext)
6010 Cadmium, Total
6010 Chromium, Total
6010 Lead, Total
Result
54000 a
aao a
73000 a
54000 a
1670 a
81000 a
55000 a
910 a
82000 a
46000 a
890 a
55000 a
52000 a
4400 a
132000 a
a = ug/l
< Cont. Next Page >
Comments/Notes
-75
-------
aquatec
INYHIOHMIHTAL MHWOW
71 CfMn Mtmmmm Drw«, So- •uri«t(ton. VT C84BJ
Til, «HliS§.tO?«
Babcock 6 Wilcox Company
R&D Division, Att: A/P
1562 eeson Street
Alliance, OH 44601
Attention : Jean Czuctva
Date :
ETR Number :
Project No. :
No. Samples:
Arrived :
P.O. Number:
12/07/90
24022
90000
22
11/16/90
537-OA247838
Page
Iterator* mlyM* Mr* pM>f«r**4 In •cecrdvw* nit* *»thod§ for An«ly*U of Uotor
Use NtttM* for Iv»lt«t1»j S«IU MMt«, W-144, «r Uaraterd
All rwuiU »r« <«t «g/l i*il
LabNo./ Sample Description/
Method *ff. Parameter
UMtoo, tM-MO/i/7?-0»,
of Usttr «nd W*stwu«t*f .
Result
124523
6010
6010
7421
3, 1230-1237: (TCLP Ext)
Cadmium, Total
Chromium, Total
L*ad, Total
124523MS Slag-Spike 3, 1230-1237 : [HS] (TCLP Ext)
6010 Cadmium. Total
6010 Chromium, Total
7421 Lead, Total
137 a
220 a
250 a
210 a
320 a
330 a
124523DP Slag-Spike 3, 1230-1237:[REP] (TCLP Ext)
6010 Cadmium, Total
6010 chromium, Total
7421 L«ad, Total
145 a
81 a
230 a
124525 Slag-Spike 3, 1418-1435:(TCLP Ext)
6010 Cadmium, Total
6010 Chromium, Total
7421 Lead, Total
60 a
28 a
210 a
124527 Slag-spike 3, 1640-1649:(TCLP Ext)
6010 Cadmium, Total
6010 Chromium, Total
7421 Lead, Total
107 a
112 a
250 a
Comments/Notes
i - ug/1
< Last Page >
submitted By J
Aquatec I n c
-76-
-------
o
aquatec
some**
MowMaM Ditv*. So. ••utingian. VT M403
TIL IB/*Si.l0?4
AftUlUrar* CA JL4R'E4frOlt Tn
Babcock and Wilcox
DMC 7 D«c«»b«r 1990
fw»«»N« 90000
ETTlNoe 24003 And 24022
16 Hov«mb«r 1990
T«t Mniwdi for EvmJmtun Sobd Wi
Kxorlaac* wi
•M.SW4440I
AJJrwuitt
^^^^11 1 III ^^^^^••111 IH ^^^^H
Cadmium
Chromium
L«Ad
aad WMM. B>A-«00/4/7MaD,
r StuxUrt VUUxxfc for tit* ^^^^M a* WM« t*d WMtmucr.
Lab Ho.
S*mpk Dcacripuoo
112690A: Method Blank for TCLP Extract samples 124376, 124376DP, 125161,
124378, 124380, 124382, 124382DP, 125162, 124384, 124386, 124517,
124517DP, 124517MS, 124519, 124521, 124523, 124523DP and 124523MS.
Res ults • are reported in ug/L.
Summed Br
Aquatec lo;
-77-
-------
aquatec
Spike Sample Recovery
Inorganic Data
ETR No. 24003
Sample ID: Soil-Spike 2, 1400-1412 (TM Ext)
Cd
Cr
Pb
Sample ID:
Parana tay
Cd
Cr
Pb
Spiked Staple
Result fuf/L)
53763.00
4147.90
145453.06
Slag-Spike 2, 1419
Spiked Saapl*
Result fug/Li
219.91
166.19
209.41
Saapl*
Results (uy/LV
55112.00
3161.84
146062.18
(TCLP Ext)
Sample
ReiulCi fuf/L)
169.64
73.88
155.24
Splk*
A4d««I fuf/ljl
NA
1000.0
N7\
Spike
Added fug/^
50.0
100.0
50.0
I ftlCOVMV
NA
98.6
NA
X Recovery
100.5
92.3
108.3
78
-------
»
ETR No. 2'
Sample ID: Soil-Spike 3. 1245-1310 (TCLP Ext)
Spiked Sample Sample spike
R««ulc fug/O R««ulti Cu«/L1
Cd
Cr
Pb
53518.
1665.
80592.
00
66
76
53857.
875.
72956.
00
01
19
NA
1000.0
NA
NA
79.1
NA
Sample ID: Slag-Spike 3, 1230-1237 (TCLP Ext)
Spiked Sample Sample Spike
tUault fu«/Ll
Cd
Cr
Pb
205.76
323.88
325.10
136.90
216.69
249.26
50.0
100.0
50.0
137.7
107.2
151.7
-71,
-------
Duplicate Sample Recovery
Inorganic Data
ETR No. 24003
Sample ID: Soil-Spike 2, 1400-1412 (TCLP Ext)
Duplic*t«
Sample ID: Slag-Spike 2, 1419 (TCLP Ext)
aquatet
Cd
Cr
Pb
55112.00
3161.84
146062.18
53971.00
1086.63
74810.21
n mam:
2.1
97.7
64.5
'uttitr
Cd
Cr
Pb
Sample
Raoule fu*/O
169.64
73.88
155.24
Duplicate
110.03
48.94
121.21
I R PD
42.6
40.6
24.6
-80-
-------
R«cov*ry
Inorganic
ET& No, 26022
Sample ID: Soil-Spike 3,1245-1310 (TCLP Ext)
Sample ID: Slag-Spike 3, 1230-1237 (TCLP Ext)
Sample Duplicate
Raiule fu/LI Ra«ilta ru/Ll
-il-
aquatec
•MM^|y
Cd
Cr
Pb
Sample
Hostile fuf/D
53857.00
875.01
72956.19
Duplicate
Rciule* fug/L)
54863.39
909.18
81766.37
1.9
3.8
11.4
^^^^MM^B
Cd
Cr
Pto
136.90
216.69
249.26
145.38
81.13
229.02
6.0
91.0
8.5
-------
aquatec
QC summary
ETR No. 24003 and 24022
Page 1 of 2
Gadaiua
Chromium
IPA
Standarj
IVQCS
IVQCS
IVQCS
IVQCS
IVQCS
IVQCS
IVQCS
Found
f 11/11
483.63
485.34
491.92
474.83
495.72
495.60
497.21
493.07
499.36
503.59
513.71
484.18
491.18
477.14
482.30
495.00
488.83
488.96
480.54
478.31
500.78
511.8o
525.72
515.87
480.46
508.08
494.23
497.37
509.24
514.91
499.33
478.58
475.31
489.01
477.24
True
£.Uf/l)
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
X R*covnrv
96.7
97.1
98.4
95.0
99.1
99.1
99.4
98.6
99.9
100.7
102.7
96.8
98.2
95.4
96.5
99.2
97.8
97.8
96.1
93.7
100.2
102.4
105.1
103.2
96.1
101.6
98.8
99.5
101.6
103.0
99 . 9
95.7
95.1
97.8
95.4
-------
QC Sunmry
ETR No. 24003 and 24022
Pag* 2 of 2
EPA
IVQCS
IVQCS
378-5
378-5
Found
Cuf/Jl
976.61
929.70
1020.58
1019.33
904.55
981.35
1005.24
975.77
983.23
907.34
1005.46
35.00
35.83
36.65
34.49
35.00
35.51
1000.0
1000.0
1000.0
1000.0
1000.0
1000.0
1000.0
1000.0
1000.0
1000.0
1000.0
34.0
34.0
34.0
34.0
34.0
34.0
97.7
93.0
102.1
101.9
90.
100
97.6
98.3
90.7
100.5
102.9
105.4
107.8
101.4
102.9
104.4
378-5
34.08
34.08
32.34
32.58
34.0
34.0
34.0
34.0
100.2
100.2
95.1
95.8
-83-
-------
Method Detection Limit Study
ETR 24003 and 24022
HDL
6010 Cadmium 12-05-90 2.55 0.839 9.1
6010 Chromium 12-05-90 2.89 0.816 10.6
7421 Lead 11-29-90 0.40 0.912 1.3
6010 Lead 12-05-90 22.13 0.854 77.8
«&L - 3 x
HDL- Mtthod d«t«ccion limit.
S|> - Standard deviation of the average noise level,
B • Slop* of cht calibration line.
90000E07DEC90
84
-------
o
aquatec
A JM*m6*r of tfM Jncftc^M tm^vnnmnM
M South Ptrfc Dnvt tekhttwr. Vtrmom «44*
m. lows-mo FAX
Babcock * Wilcox Company
R&D Division, Aft: A/P
1562 Beeson Street
Alliance, OH 44601
Attention i Jean Czuczwa
Date :
ETR Number:
Project No.:
No. Samples:
Arrived :
P.O. Number:*
Page
11/05/91
26202
91000
29
09/13/91
tn
tothedi for
Mr
NcttMdt for lv»lu»tir< UHd WMtt, SW-MA, or ttwterd H*th«dB for th« UaairMtlon of U«t*r and UH
*U rMult* or* In >t/l unloss otlwrvlM netod.
Lab No./ Sampl* Description/
Method NO. Parani«t«r Result
143696
Hopper 2001b/hr: (TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
6010 Lead, Total
143696MS F*«d Hopper 200lb/hr: [MS] (TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total-
6010 had, Total
143696DP Feed Hopper 2001b/hr: [REP] (TCLPExt)
Cadmium, Total
6010 Chromium, Total
6010 Lead, Total
143698 F*«4 Hopper 200lb/hr: (TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
6010 Lead, Total
143700 Feed Hopper 2 OOlb/hr: (TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
6010 Lead, Total
143702 Slag Tank 2001b/hr; (TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
7421 Lead, Total
33
0.46
78
31
0.67
66
34
0.46
70
34
0.50
88
32
0.46
65
0.11
0.02
0.19
< Cont. Next Page >
-85-
-------
o
aquatec
M MwnlMT at ift* IneAeap* IrwfrwMMMiaf
99 Sou* P*rt Dnv». ColdtMMr, Vtmiom 9544*
TEL a02/«S5-12IX> f AX *»«S"S24i
ANA L-Y XIC-A L -«R E POR T
Babcock 6 Wilcox Company
R&D Division, Att: A/P
1562 Beeson Street
Alliance, OH 44601
Attention : Jean Czuczwa
Dat* :
ETR Nunb«r:
Project No. :
No. Sanpl**:
Arrived :
P.O. Number:
11/05/91
26202
91000
29
09/13/91
Pag*
?MI nttka* far
Lab No./
M*thod No.
In tccortM^ct nltti n*tiwdk far *n«ly«t» of ttotw w , --
Solid UMt*t W-M*, or Stanctortf >»«th«J» far tlM iMBfnctlen of inter and UMf««ttr
All rttult* «r* in «t/l k*»t»»» «tlMtrMl«* r»t*d.
Saapl* Description/
param«t*r R«»ult
143704
143706
143708
143710
143712
143714
Slag Tank 2001b/hn (TCLPExt)
6010 Cadmium, Total
6010 Chroaiua, Total
7421 Lead, Total
Slag Tank 200lb/hr:(TCLPlXt)
6010 Cadmium, Total
6010 Chromium, Total
7421 L*ad, Total
F*«d Hopp*r lOOlb/hr:(TCLPExt)
6010 Cadmium, Total
6010 Chroodua, Total
6010 L«ad, Total
slag Tank lOOlb/hr:(TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
7421 Lead, Total
?««d Boppcr 3001b/hr:(TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
6010 Laad, Total
Slag Tank 300lb/hr:(TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
7421 Lead, Total
0.04
0.02
0.14
0.07
0.02
0.20
36
0.42
72
0.03
<0.01
0.06
40
0.42
78
0.07
<0.01
0.19
< Cont. Naxt Pag* >
-86-
-------
o
aquatec
M MMtter ot tfw /rtcrtcpp« £mrtroom«m*/ Oot/p
0 South P»rt Drtv*. Cokhnm Vrrmont 9544*
TIL,
ANALYTICAL A.EPO'RT-
Babcock 6 Wilcox Company
R&D Division, Att: A/P
1562 Beeson Street
Alliance, OH 44601
Attention
Jean Czuczwa
Data : 11/03/91
ETR Number : 26202
Project No. : 91000
No. Saapl««: 29
Arrived : 09/13/91
P.O. Nuab«r: •
Page
ttmterd miy*** »tr« pwforMd In •ccofd«nc« with Ntthodt for AiwtytU »f Uattr and UMtM, »A-600/4/79-020,
TMt H*thod» for IvalMtfn* tellrf UMta, W-M4, «r ttandtrd Hvtitodi for tfc* IwHiiraitien of Uitsr ind
AIL rwults ar« in n/l ml«u «ttMntlt« not«d.
Lab No./ Saapl* Description/
Mathod No. Parameter R«»ult
143716 Food Hopper Borax:(TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
6010 Lead, Total
143718 Slag Tank Borax:(TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
7421 Lead, Total
143720 Slag Tank Borax:(TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
7421 Lead, Total
30
0.13
54
0.27
0.02
0.43
0.27
0.01
0.35
< .Last Page >
Submitted By :
-87-
Aquatec Inc.
-------
aquatec
A erf tl*#
•W ;>
TEi
Babcock & Wilcox Co.
Date: 02 October 1991
Project No: 91000
ETRNo: 28202
Sample(s) Received on 13 September
I at 1
1991
«» «nt> for orf
fc* or few jj»» irf »*»
AH *»» <•
Cadaiam
Lab No. S*npie Description
Blank. TCLP extraction blank for samples labalad 143696, 143696DP, 143696MS,
143698, 143700, 143702, 143704, 143706, 143708, 143710, 143712.
143716, 143718 , and 143720.
143714,
/!.
-------
aquatec
S§ South fmk On**. CotehMMr, V««M>m 0544*
TIL 801- AM-', 203 FAX KKMMM14I
Babcock and Wile ox Company
Date: 05 November 1991
Project No: 91000
ETRNo: 28477
SMpfa(i) RMM OK 13 S«pttmb«r 1991
1** I el I
W.
Mtytu wm p«rfocn»««J m acxxxduuKS wtti Mttliodt tat AaiJytM of .
ftm MHto* tat Bvmh«oiij SaM WMM, SW-MA. at Su«tanJ ItatexH te tta EnMnanrisa of w»ur u*d Wi
Ptninctcf
C«dmlu»
Chromium
Lead
:Q.Ql
=0.01
:0.§§5
UbNo.
Staple Descriprioa
PBLK Prep blank for samples 143702MS, 143702DP, 143716MS, 143716DP, 143718MS
and 143718DP.
S«tniutt«l By:
-90-
-------
o
aquatec
ineliecp* tmttmnamtut Qnup
» Sen* Part Onm Cekhnmr. V««t*»«t 0944*
TEL KB/ftM-un
ANAJ-YTJCAL-stflEFOAT
Babcock 6 Wilcox Company
R&D Division, Att: A/p
1562 Beeson Street
Alliance, OH 44601
Attention : J«an Czuczwa
Data
ETR Number
Project No.
No. Samples
Arrived
P.O. Number
Paga
11/05/91
28477
91000
6
09/13/91
tyMs wtrt
for
Lab No./
H*thod NO.
In *cc0rdtnet »ftft Hortiod* for Araiytis of U*t*r and WMtn, IP*-600/4/79-020,
Solid UMt*. M-A44P of (tandtrtt »««thod» for th» I»«iin«tf«n of y«t«r tnd tf»«t«w«t«r.
•*•• tn ••/! i»lM« othorvtM no tod.
R«»ult
Sanpl« Description/
Paraa*t*r
143702MS Slag Tank 2001b/hr:[MS](TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
7421 L«adr Total
143702DP Slag Tank 2001b/hr:[REP](TCLPExt)
6010 Cadaiua, Total
6010 Chromium, Total
7421 L«ad, Total
143716MS F««d Hopp«r Borax:[MS](TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
6010 l*ad, Total
143716DP Feed Hopper Borax:[RZP](TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
6010 L«ad, Total
143718MS Slag Tank Borax: [MS] (TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
7421 L«ad, Total
143718DP Slag Tank Borax:[REP](TCLPExt)
6010 Cadmium, Total
6010 Chromium, Total
7421 Lead, Total
0.13
0.23
0.44
0.08
0.03
0.24
30
0.33
47
31
0.14
51
0.36
0.25
0.55
0.25
0.02
0.41
< Last Page >
Submitted By
Aquatec In s
-------
QC
EYt
aquatec
Cadmium IVQCS
Chromium
Lead
IVQCS
490.68
491.74
490.89
487.69
494.15
500.04
505.49
504.66
483.05
493.38
482.88
489.70
475.05
408.73
478.30
15.74
15.56
16.18
967.96
1030.30
1009.99
984.88
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
500.0
15.0
15.0
15.0
1000.0
1000.0
1000.0
1000.0
98,
96.
98.
97.5
90.0
100.0
101.1
100.9
96.6
96.5
96.6
97. t
95.0
97.7
9s.7
104.9
103.7
107.9
96.8
103.0
100.6
98.5
-91-
-------
QC Summary
ETR 26202
EFA ...... S C
Pound (UC/L1
I R«eov
-------
143702
143702
143702
143716
143716
143716
143718
143718
143718
143696
143696
143696
Cmdaims
Chtoaiua
Lead
Cadalua
threat am
Lead
Ca datum
ChroaiusR
Lead
C-a Anitas
Lend
QC Summary
ET1 NO. 28477/28202
Results in ug/L
Duplicate
109.4740 81.8600
15.0750 28.7660
189.3980 237.1300
29929.4000 31408.4390
132.3950 136.4310
54027.0160 51023.5780
267.9530
18.6640
428.5714
32656.9372
459.5020
77898.9380
253.1760
24.1630
413.7400
33795.2173
464.3000
70342.8830
ail
28.9
62.5
22.4
4.8
3.0
5.7
25.7
3.5
3.4
1.0
10.2
aquatec
Matrix
Spike
Sptkn
128.9970 49.19 39.7
234.2180 196.77 111.4
435.4300 492.42 50.0
30366.8320
331.8620
47450.1640
49.73 NC
198.93 100.3
497.31 NC
358.9100 49.47 NC
253.6400 197.86 118.8
551.3000 494.27 24.8
31437.8611
665.8240
65792.0230
49.98 NC
199.90 103.2
499.75 NC
NC - Sample result is greater than 4 times the splk« added therefore % recovery is
non-calculabi*.
-93-
-------
ACG-92-4191-07
October 23, 1991
ANALYSTS BY ICP-AES
DRY BASIS
Sample No. and Description..
M-48652
Soil, 100 Ib/hr Test, Composite
of 1025, 1115, 1245 hrs, 9/10/91
M-48653
Soil, 200 Ib/hr Test, Composite
of 1225, 1615, 1700, 1750 hrs,
M-486S4
Soil, 300 Ib/hr Test, Composite
of 1435, 1700, 1745 hrs, 9/10/91
M-48655
Soil with Borax, 200 Ib/hr Test,
Composite of 1030, 1250, 1350 hrs,
9/11/91
Cadmium,
Cd_
1,232
1223
1,281
1,248
1,255
1,292
1,366
1,268
1,251
Chromium,
1,541
1513
1,544
1,540
1566
1,567
1,622
1,577
1553
Lead,
ft
7,247
7,150
7,635
7,655
7836
7,509
7,894
8,208*
7,838
Acid Reagent Blank
(Aqua Regia -HF- Boric Acid)
<0.5
<0.5
<0.5
Note: Replicate values were determined from separate acid digestions.
• This value is probably too high - Pb calibration was difficult to maintain. ICP was
recalibrated 3 times during this run because 5ppm Pb standards were too low or too high.
See calibration data shown for 9/23/91. The lead level measured in the Cr Spiked
Sample was also lower than 8208ppm. See Spiked Sample Recovery data sheet in this
report.
-94-
-------
ACG-92-4191-07
October 23, 1991
ANALYSIS RY 1CP-ARS
Sample No . and PcsoiptJQQ
M-48656
Slag, 100 Ib/hr Test, Composite
of 1045, 1240, 1325 hrs,
9/10/91
M-48657
Slag, 200 Ib/hr Test, Composite
of 1245, 1615, 1730, 1820 hrs,
9/9/91
M-48658
Slag. 300 Ib/hr Test, Composite
of 1445, 1700, 1800 hrs, 9/10/91
M-48659
Slag with Borax, 200 Ib/hr Test,
Composite of 1215, 1300, 1408 hrs,
DRY RASIS
Cadmium,
Cd
116
111
187
186
197
178
180
279
289
Chromium,
Cr
1,489
1,421
1,500
1,484
1,481
1,440
1,403
1,219
1,197
Lead,
Pb
2,097
2,053
3,550
3,570
3,656
3,551
3,554
3,813
3,856
9/11/91
acnt Bla
<0.2
(Aqua Regia -HF- Boric Acid)
<0.2
Note: Replicate values were determined from separate acid digestions.
<0.2
-95-
-------
ACG-92-4191-07
October 23, 1991
1Y.ICP.AES
No.
M-48694
Filter & Combined Participates,
200 Ib/hr Test, 1610-1646 hrs,
9/9/91, 0.92 g Total particulates
M-48695
Filter & Combined Particulates,
2001b/hr Test, 1744-1820 hrs,
9/9/91, 0.69 g Total Particulates
0.1N HNO, Rinse for M-48695,
0.08g solids
IUURRQR
Filter & Combined Particulates
with Borax, 200 Ib/hr Test,
1238-1314 hrs, 9/11/91, 1.23g
Total Particulates
0.1N HNO, Rinse for M-48696,
O.llg solids
Acid Reagent Blank
(Aqua Regia-HF-Boric Acid)
M-48697
Filter Blank
0. IN
Acetone
Cadmium,
Cd..
17,720
25,625
6,159
13,103
Chromium,
«oom Cr
7,874
9,580
4,259
5,258
98,736
131.669
28,694
70,939
<0.5
<37
<0.2
<0.1
Sample Lost
<0.5
43
<0.2
<0.3
<0.5
< 37
<0.2
<0.1
-96-
-------
ACG-92-4191-07
October 23, 1991
;
CONSTITUENTS BY ICP-AES*
DRY BASIS
M-486S3
Soil Composite,
200 Ih/hr Test,
1225, 1615, 1700,
1750 hrs, 9/10/91
M-48655
Soil Composite
with Borax,
200 Ib/hr
Test, 1030,
1250, 1350 hrs,
9/11/91
M-48657
M-48659
Slag Composite, Slag Composite,
200 Ib/hr Test, with Borax,
1245, 1615, 1730 200 Ib/hr
1820 hrs,
Test, 1215,
1300, 1408 hrs,
9/11/91
SiO,,*
AIA.%
FeA.o/0
HO,,*
CaO,%
MgO,o/0
80,,%
PaOs,o/o
NaA%
KjO,%
O 1*1 n/
47.35
46.80
9.07
8.83
2.28
2.22
0.35
0.34
15.26
14.99
4.45
4.33
0.67
0.72
0.39
0.31
0.59
1.12
47.27
44.93
9.15
8.96
2.23
2.18
0.41
0.32
13.20
13.20
3.99
3.96
0.69
0.61
0.34
0.33
1.93
1.93
1.13
1.13
ORQ
60.87
59.26
13.25
12.88
2.83
2.84
0.67
0.65
16.87
16.81
4.74
4.64
0.30
0.36
0.42
0.40
0.74
1.30
59.54
10.29
2.77
0.54
17.51
4.77
0.27
0.41
1.95
1.89
1.20
1.18
1 81
Note: Replicate values were determined from separate acid digestions.
Elements are reported as oxides for convenience and arc not necessarily present in that form.
>T " ^ and K.20 were determined by flame photometry.
-97-
-------
ACG-92-4191-07
October 23, 1991
M-48653
Description; Soil Composite,
200 Ib/hr Test,
1225, 1615, 1700,
1750 hrs, 9/10/91
Carbonate, % CO2 15.44
-98-
-------
ACG-92-4191-07
October 23,1991
- % H7Q
(Before Compositing)
Soil. 100 1b/hf Test.
9/10/91
25.02
26.32
24.32
M-48653
Jb/hr.TcsL
24.94
25.42
25.73
1750 H« 25.12
Soil. 30Q Ib/ht
9/10/91
I43S Hrs 26.35
1700 H« 26.19
1745 Hrs 27.43
with 200 Test.
9/11/91
1030 Hrs 28.89
28.44
13SO Hrs 29.30
-99-
-------
ACG-92-4191-07
October 23, 1991
AS
M-48656
Slag Composite, 100 Ib/hr Test,
1045, 1240, 1325hrs, 9/10/91
Slag Composite, 200 Ib/hr Test, 85.47
1245, 1615, 1730, 1820, 9/9/91
M-48658
Slag Composite, 300 Ib/hr Test, 82.40
1445, 1700, 1800 hrs, 9/10/91
Slag Composite with Borax, 81.45
200 Ib/hr Test, 1215, 1300, 1408 hrs,
9/11/91
Values reported are average of 2 determinations within 10% of each other.
-------
ACG-92-4191-07
October 23,1991
SOIL BULK DENSITY*. POTINDS/FT3
DRY BASIS
Soil, 100 Ib/hr Test, 76.57
Partial Composite
Soil, 200 Ib/hr Test, 81.90
Partial Composite
M-48654
Soil, 300 Ib/hr Test, 81.53
Partial Composite
M-48655
Soil with Borax, 75.76
200 Ib/hr Test,
Partial Composite
Values reported arc average of 2 determinations within 10% of each other. Samples were dried at
ISO'F, and crushed with a jaw crusher (approximately 1/4"). Portions from 2 different hour tests
were used to fill the box for each sample.
-101-
-------
ACG-92-4191-07
October 23,1991
%
BYICP
M-4K6S7
Soil Composite, lOOlb/hr
Test, 1025, 1115, 1245 hrs,
9/10/91
Cd
107.34 %R
(1.565)
Pit
(7.417)
Soil Composite, 300 Ib/hr
Test, 1435, 1700, 1745 hrs,
9/9/91
M-4865S
Soil Composite with Borax,
200 Ib/hr Test, 1030, 1250,
1350 hrs, 9/1 1/91
(1.315)
(1,233)
(1,613)
103.43 %R
96.86 %1
(7,733)
M-48656
Slag Composite, 100 Ib/hr
Test, 1045,1240,1325 hrs,
9/10/91
M-48658
Slag Composite, 300 Ib/hr
Test, 1445,1700,1800 hrs,
9/10/91
92.03 %R
(167)
96.91 %R'
(3,425)
M-48659
Slag Composite with Borax,
200 Ib/hr Test, 1215, 1300,
1408 hrs, 9/11/91
099)
(1,242)
95.60 %R
Note: Values shown in parentheses are ppm of the 2 elements not spiked in each sample.
-102-
-------
ACG-92-4191-07
October 23, 1991
CALIBRATION VERIFICATION
Cadmium.
Initial
4.86
Continyjog
5.09
4.90
5.28
4.93
4.98
4.85
5.09
5.06
%R
97.2
%R
101.8
98.0
105.6
98.6
99.6
97.0
101.8
101.2
Chromium.... Sppm
Initial
4.97
%R
99.4
Continuing %B
5.13
5.00
5.19
4.90
4.81
4.84
5.13
5.04
102.6
100.0
103.8
(Recalibrated)
98.0
96.2
96.8
(Recalibrated)
102.6
100.8
Lead. Sppm
Initial
5.07
Continuing
5.11
5.16
5.41
5.03
4.73
4.56
5.28
5.54
%R
101.4
%R
102.2
103.2
108.2
100.6
94.6
91.2
105.6
110.8
CHECK STANDARD
Cadmium^ Q.S.ppm
Measure^ j%%
0.57 114.0
0.52 104.0
Chromium. Q.Spprn
0.56
0.51
112.0
102.0
Measured %R
0.42 84.0
0.48 96.0
-103-
-------
ACG-92-4191-07
October 23, 1991
CALIBRATION VERIFICATION
9/26/91
Ci4fflJMffli,
Initial
4.98
Continuing
4.83
4.87
%R
99.6
%R
96.6
97.4
, Chromium
Initial
4.95
Continuing
4.85
4.97
t 5pp.ro
%R
99.0
%R
97.0
99.4
LeMtJppiD
Initial
4.95
Continuing
5.25
5.21
x&
99.0
%R
105.0
104.2
CHECK STANDARDS
9/26/91
Cadmium.
Measured
JQrom
%R
Chromium.
Measured
j&Q&ni
%R
Lead. 50j
Measured
Wfl
J6R
49.96 99.9
49.44 98.9
50.69 101.4
Cadmium. Q.Sppm
Chromium. Q.Sppm'
Measured
%R
Measured
%R
-104-
* No peak found.
** These values were not used in reporting results.
Lead* Q.2ppm
Measured %R
0.53
0.46
Cadmium.
Measured
0.21
Cadmium.
19.59
19.50
106.0
92.0
JLZDom
%R
105.0
JStem
JR
98.0
97.5
0.63
0.32
Chromium.
Mssjirsd
0.20
Chromium
Measured
19.99
20.16
126.0
64.0
%R
100.0
11
100.0
100.8
0.53
0.52
LeaiL
Lad*.
Mea^ifed
19.60
19.65
106.0
104.0
Q.2ppm
*
2Qppm
1 M
98.0
98.3
-------
ACG-92-4191-07
October 23, 1991
CALIBRATION VERIFICATION
10/3/91
Cadmium. Sppm
Initial
4.99
%R
99.8
Chromium. Sopm
Initial %R
5.04 100.8
Lead. Sppm
Initial
5.06
101.2
Continuing
4.96
4.96
4.96
99.2
99.2
99.2
C_ontinyjng
4.99
4.82
4.92
99.8
96.4
98.4
Continuing
4.98
5.00
5.09
99.6
100.0
101.8
Cadmium. IQpum
Measured
%R
CHECK STANDARDS
10/3/91
Chromium. IQppm
Measured
Lead. IQppm
Measurai
%g
10.25
9.85
9.46
102.5
98.5
94.6
10.00
9.92
9.64
100.0
99.2
96.4
10.19
9.43
9.67
101.9
94.3
96.7
Cadmium, loom
Measured.
0.98
1.02
%R
98.0
102.0
ChromiumJppm
Measured
0.94
0.95
%R
94.0
95.0
Lead, loom
Measure^
0.95
0.96
%R
95.0
96.0
-105-
-------
ACG-92-4191-07
October 23, 1991
CALIBRATION VERIFICATION
10/4/91
Cadmium. Sppni
Initial %R
4.96 99.2
Chromium 5pprn
Lead. Sopm
Iniiial
5.09
%R
101.8
Initial
5.21
%R
104.2
Continuing
4."77 95.4
Continuing %R
5.02 100.4
Continuing
4.84 96.8
CHECK STANDARDS
10/4/91
Cadmium. .2Qpgnj
Measured %R
19.81 99.1
Chromium.
Measured %R
19.71 98.6
Lead. 20ppm
Measured.
19.23 96.2
.. O.Sm
Measured %R
0.50 100.0
Measured %R
0.52 104.0
Lead. O.Sppm*
Measured %R
0.70 140.0
Lead value was outside ± 10% range but samples contained much higher lead levels. Calibration was
within ± 10% at the higher levels.
-106-
-------
ACG-92-4191-07
October 23, 1991
CALIBRATION VERIFICATION
10/8/91 10/13/91
Boron. 5oom 5.
Initial
5.09
Continuing
5.13
5.07
5.12
5.17
%R
101.8
%R
102.6
101.4
102.4
103.4
Initial
5.04
Continuing
5.15
%R
100.8
%R
103.0
STANDARDS
10/8/91 10/13/91
Bo.ro.tL. Ippm Chromium Q.5ppm*
Measured %R %R
1.00 100.0 0.42 84.0
0.97 97.0
0.98 98.0
CJirojpiyini
%R
50.16 100.3
50.39 100.8
Approaching detection limit in this matrix. These values are for indication of acid reagent
blank levels.
-107-
-------
ACG-92-4191-07
October 23, 1991
CALIBRATION VERIFICATION
10/21/91
Cadmium. 5opm
Initial
4.61
%R
92.2
Chromium. 5ppm
Initial %R
4.93 98.6
Lead. SPPITI
4.79
%R
95.8
Continuing
4.63 92.6
Continuing %"R,
5.03 100.6
Continuing
4.71 94.2
CHECK
Cadmium. Q.
Measured %R
0.46 92.0
ChromiumQ-
Measured %R
0.50 100.0
Measured
0.64
128.0
Cadmium. Q.2ppm
%R
100.0
90.0
80.0
0.20
0.18
0.16
Chromium., Q,2pgiB
Measured %R
110.0
100.0
100.0
Lead. 0.2ppm
Measured %R
0.20
No peak found. The above low level values (0.2ppm) were used only to report < values for
Cadmium and Chromium in the filter blank and acid reagent blanks.
-108-
-------
ACG-92-4191-07
October 23, 1991
CALIBRATION VERIFICATION
10/22/91
Cadmium. Sppm
Initial
4.86
%R
97.2
5.08
Continuing
4.78
5.17
101.6
%R
95.6
103.4
Initial
5.20
%R
104.0
(Recalibrated)
5.26 105.2
Continuin
%R
Lead. Sm
Initial
4.77
95.4
4.94 98.8
Continuing JIB.
4.85
5.13
97.0
102.6
4.81
4.80
96.2
96.0
CHECK STANDARDS
10/22/91
Cadmium. O.Sppm
Measured %R
0.48 96.0
t Q.Sm
0.49
0.48
0.47
98.0
96.0
94.0
Measured %R
0.54 108.0
(Recalibrated)
0.53 106.0
0.51 102.0
0.52 104.0
Lead. Q.5m*
Measured
0.49
98.0
0.80 160.0
0.65 130.0
0.50 100.0
At low lead levels (0.5ppm) the lead intensities measured are close to background levels in
the matrix.
-109-
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ACG-92-4191-07
October 23,1991
CALIBRATION PROCEDURE FOR ICP
This instrument is calibrated using acid/matrix reagent blank (same matrix used in standards
preparation) as standard 1 and a matrix-matched standard (in this case 50ppm of each element)
as standard 2. An analytical curve is drawn by the instrument using the data obtained from
standards 1 and 2.
Instrument calibration is verified using a separate matrix-matched standard (or standards) in the
working range of the samples. The calibntion standard(s) are checked throughout the analysis
and recalibration (using standards 1 and 2) is performed when the calibration verification
standard falls outside (or sometimes near) the 90 to 110% range.
An independent check standard can also be used for calibration verification if it is in the working
range of the samples. An acid/matrix reagent blank which has been digested along with the
samples is also run as an unknown.
-110-
-------
Form VI
QC Report No. ACG-92-4191-07
DUPLICATES
Lab. Name
ARC - Analytical Chemistry
Date: September 21 1991 / October 3. 1991
Project No. 4191-07
Sample No. M-48652
Units: oom
Compound
I.
2,
3, Lead
Sampte(S)
1,232
1,541
7,24?
(D)
1,223
1,513
7,150
;
RDP I
0.733 I
1 , 83-4 !
1.347 I
N -Out of Control
RDP m [{S-D}]/[(S-i-D)/2)] x 100
NC - Non calculable RDP due to value(s)less than CRDL
-111-
-------
* Form VI
QC Report No. ACG-92-4I91-Q7
DUPLICATES
Lab. Name ARC - Analytical Chemistry
Date: September 23. IQQ1 /October 3. 1991
Project No. 4191-07
Sample No. M-48653
Units: t>pm
Compound
1 ,
2.
3.
(D)
1,248
1,540
7,655
*
2.609
0,259
0,262
• First 2 replicate samples were used to calculate RDP values.
N - out of Control
RDP= [{S-D}]/[(S+D)/2)]xlOO
NC - Non calculable RDP due to value(s) less than CRDL
-112-
-------
Form VI
QC Report No. AnO-92-4191-07
DUPLICATES
Lab. Name
ARC - Analytical Chemistry
Date: October 3. 1991
Project No. 4191-07
Sample No. M-48655
Units: ppm
Compound
1. Cadmium
2. Chromium
3. Lead
Control Limit
Sample(S)
1,268
1,577
Duplicate (D)
1,251
1,553
RDP
1.349
1.534
N - Out of Control
RDP= [(S-D}]/[(S+D)/2)] x 100
NC - Non calculable RDP due to value(s) less than CRDL
-113-
-------
Form VI
QC Report No. ACG-92-4191-07
DUPLICATES
Lab. Name ARC - Analytical Chemistry
Date: September 26. 1991 / October 3. 1991
Project No. 4191-07
Sample No. M-48657
Units: ppm
1
Compound
1. Cadmium
2, Chromium
3.
Control Limit
Sample(S)
187
1,500
3,550
Duplicate (D)
186
M84
3,570
|
.1
1
0,535 1
LOT4 1
i
0.562 1
• First 2 replicates were used to calculate RDP values.
N - out of Control
RDP= [{S-DM(S+D)/2)]xlOO
NC - Non calculable RDP due to value(s) less than CRDL
-114-
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Form VI
QC Report No. ACG-92-4191-07
DUPLICATES
Lab. Name ARC -'Aftlvticai Chemistry
Date: September 23. 1991 / October 3. 1991
Project No. 4191-07
Sample No. M-48654
Units: ppm
Compound
I.
2, Chromium
3,
Sampl«(S)
1,292
1,567
7,509
(D)
1,366
1,622
7,894
RDP !
!
3.
-------
Form VI
QC Report No. ACG-Q7-41Q1-07
DUPLICATES
Lab Name
ARC 'Analytical Chemistry
Date: September 26 1991 / October 3. 1991
Project No. 4191-07
Sample No. M-48656
Units:
JDPCL
Compound
1. Cadmium
2, Chromium
3,
Control Limit
Sample(S)
116
1,489
2,09?
Duplicate (D)
111
1,421
RDP \
4.386 j
4«6?i I
| 2,120 |
N - out of Control
RDP = [|S-D}]/[(S+D)/2)] x 100
NC - Non calculable RDP due tovalue(s) less than CRDL
-116-
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Form V
QC Report No. ACG-92-4191-07
DUPLICATES
Lab. Name ARC - Analytical Chemistry
Date: September 26. 1991 /October 3. 1991
Project No. 4191-07
Sample No. M-48658
Units:
Compound
1. Cadmium
2. Chromium
3. Lead
Control Limit
Sample(s)
178
1,440
3,551
Duplicate (D)
180
1,403
3,554
(
i
RDP I
1.117 1
2.607 [
0.084 ]
N -Out of Control
RDP= [{S-D}]/[(S+D)/2)J x 100
NC - Non calculable RDP due to value(s) less than CRDL
-117-
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Form V
QC Report No. ACG-92-4191-07
DUPLICATES
Lab. Name ARC • Analytical Chemistry
Date: September 26. 1991 /Octobers. 1991
Project No. 4191-07
Sample No. M-48659
U&S: _
pom
Compound
1.
2,
3. Lead
Sareple(s)
279
1,219
S :
(D) |
289 3.52! |
\
1 | LI:I j
N - Out of Control
RDP- [{S-D}3/[(S+D)/2)JxlOO
NC - Non calculable RDP due to value(s) less than CRDL
-118-
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Form IV
QC Report No._ ArG-Q7-41Q1-07
SPIKE SAMPLE RECOVERY
SOILS
Lab. Name ARC - Analytical Cherrjistry
Date: October 3. 1991
Project No. 4191-07
Units: nnm
Mo.
i
!
I
Compound
1 .
2, Chromium
3. Lead
Control Limit
% R
(SR)
6,57?
11,855
12,476
Sample
1,223
1,513
7,894
Spike
-------
Form IV
QC Report No. ACG-92-4191-07
SPIKE SAMPLE RECOVERY
SLAGS
Lab. Name ARC - Analytical Chemistry
Date: September 26 1991
Project No. 4191-07
Units: ppm
Sample No,
; M-48656
M'4St-58
M-4S659 f
Ccnrpound
L Cadmium
2, Chromium
3, Lead
Control Limit 1 Spiked Sample
% R fSR)
9,263
11,063
| '
Sample
(SR)
116
1,440
3,813
Spike
(SA)
9,945
9,930
9,995
.j
% R 1
92,01 1
96,->l |
95 60 1
%R= [(SSR-SR/SA)] x 100
N - out of control
NR- Not Required
-120-
-------
Form III
QC Report No Af.G-92-4191-07
BLANKS
Lab. Name ARC-Analytical Chemistry
Date: September 23. 1991
Project No. 4191-07
Units: ppm
. Cadmium
Aqua-Regia-HF-Boric Acid
initial Calibration
Continuing Calibration
<0.5
<0.5
Preparation Blank
I
} Compound
Blank Value
Blank Value
*
Blank Value j
2. Chromium
3. Lead
<0.5
<0.5
<0.5
<0.5
-121-
-------
Form III
QC Report No. Af!ri-92-4l9l-n7
BLANKS
Lab. Name ARC -Analytical Chemistry
Date: September 26. 1991
Project No. 4191-07
Units: ppm
Aqua-Regia-HF-Boric Acid
Initial Calibration
Continuing Calibration
Preparation Blank
Compound
1. Cadmium
2. Chromium
3. Lead
Blank Value
<0.2
<0.2
<0.2
Blank Value
<0.2
<0.2
<0.2
Blank Value
-122-
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Form III
QC Report No. Ar.G-Q7.-4lQl-n7
BLANKS
Lab. Name ARC - Analytical Chemistry
Date: October 4 1991
Project No. 4191-07
Units: ppm
Go;
;1 i.
Aqua-Regia-HF-Boric Acid
Initial Calibration
Continuing Calibration
Preparation Blank
Blank Value
<0.5
2. Chromium
3, r.ead
<0.5
<0.5
<0.5
<0.5
I
-123-
-------
Form III
QC Report No Ar.rT-92-4191-n7
BLANKS
Lab. Name ARC - Analytical Chemistry_
Date: O.tnher 4.1991
Project No. 4191-07
units:
ppm
Aqua-Regia-HF-Boric Acid
Initial Calibration
Compound
L
2,
3, Lead
<0,5
<0.5
<0,5
<0.S
-------
Form III
QC Report No. ACG-97-4191-07
BLANKS
Lab. Name ARC-Analytical Chemistry
Date: October 21. 1991
Project No. 4191-07
Units: oom
0. IN HNO, Rinse Blank
Initial Calibration
Continuing Calibration
Compound
1. Cadmium
2. Chromium
3. Lead
Blank Value
<0.2
<0.2
<0.2
Blank Value
<0.2
<0.2
<0.2
Blank Value \
\
- — — -<]
-125-
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Form III
QC Report No. Ar.fi-92-4191-07
BLANKS
Lab. Name ARC - Analytical Chemistry
Date: Qp.tnbpr 21. 1991
Project No. 4191-07
units: rmm
Acetone Rinse Blank
Comoound
1. Cadmium
2. Chromium
3. Lead
Blank Value
0.1
<0.3
0.1
Blank Value
<0.1
<0.3
0.1
Blank Value
-126-
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aquatec
Utmtmr ol M»« IneHeap* £nv/n>nm«nta/ Group
*8 South P*rt Dnv*. Cokhe*t«r. Vermont 0544*
TEL- 802.S5S-1203 FAX 102 6SM2U
Babcock 4 Wilcox Company
R&D Division, Att: A/P
1562 Beeson Street
Alliance, OH 44601
Attention
Jean Czuczwa
Date :
ETR Number :
Project No.:
No. Samples:
Arrived ::
P.O. Number:
Page
11/05/91
28477
91000
6
09/13/91
Standard mtlyiM wtr* ptrforMd In accordant* with N«thod» for Analytlt of Uattr and W«ttn, EPA-600/4/79-020,
TMI Methods for Eyaluatlng Solid UHT«, SW-K6, or St*nd«rd M*thod» for th« ExM
Submitted By
Aquatec inc.
-127-
------- |