vxEPA
United States
Environmental Protection
Agency
Office of Emergency and
Remedial Response
Washington, DC 20460
Office of
Research and Development
Cincinnati, OH 45268
Superfund
EPA/540/S-92/011
September 1992
Engineering Bulletin
SELECTION OF CONTROL TECHNOLOGIES
FOR REMEDIATION OF LEAD BATTERY
RECYCLING SITES
Purpose
Section 121(b) of the Comprehensive Environmental
Response, Compensation, and Liability Act, (CERCLA)
mandates the Environmental Protection Agency (EPA) to
select remedies that "utilize permanent solutions and
alternative treatment technologies or resource recovery
technologies to the maximum extent practicable" and to
prefer remedial actions in which treatment "permanently
and significantly reduces the volume, toxicity, or mobility
of hazardous substances, pollutants, and contaminants as
a principal element." The Engineering Bulletins are a
series of documents that summarize the latest information
available on selected treatment and site remediation
technologies and related issues. They provide summaries
and references for the latest information to help remedial
project managers, on-scene coordinators, contractors,
and other site cleanup managers understand the type of
data and site characteristics needed to evaluate a
technology for potential applicability to their Superfund or
other hazardous waste sites. Those documents that
describe individual site remediation technologies focus on
remedial investigation scoping needs. Addenda will be
issued periodically to update the original bulletins.
Introduction
The objective of this bulletin is to provide remedial
project managers (RPMs), potentially responsible parties
(PRPs), and their supporting contractors with information
to facilitate the selection of treatment alternatives and
cleanup services at lead battery recycling sites (LBRS).
This bulletin condenses and updates the information
presented in the EPA technical resource document (TRD)
entitled; "Selection of Control Technologies for
Remediation of Lead Battery Recycling Sites,"
EPA/540/2-91/014, July 1991 which is available from The
National Technical Information Service, Springfield, VA.
This bulletin consolidates useful information on LBRS,
such as the following:
Description of types of operations commonly
conducted, and wastes generated at LBRS;
Technologies implemented or selected for LBRS
remediation;
Case studies of treatability studies on LBRS wastes;
Past experience regarding the recyclability of
materials that are found at LBRS; and
Profiles of potentially applicable innovative treatment
technologies.
Batteries account for more than 80% of the lead
used in the United States, of which approximately 60% is
reclaimed during times of low lead prices and greater
percentages are reclaimed during times of high lead
prices. In general, 50% of the national lead requirements
are satisfied by recycled products. There are 29
Superfund lead battery recycling sites (LBRS). Twenty-
two sites are on the National Priority List (NPL), and 10 of
these sites have completed RODs. Removal actions are
underway or completed at seven other LBRS.
LBRS are likely to contain a variety of wastes (e.g.,
lead, plastic, hard rubber) that are potentially recyclable.
At LBRS, RPMs are typically confronted with metallic lead
and lead compounds as the principal contaminants of
concern. Other metals (e.g., cadmium, copper, arsenic,
antimony, and selenium) are often present at LBRS, but
-------
usually at much lower concentration than lead and often
below hazardous concentrations. Also sulfuric acid from
batteries may remain in liquid form in pits, ponds, lagoons,
storage tanks, or treatment vessels.
Background Information on Lead-Acid Batteries,
Battery Breaking and Secondary Lead Smelting
Operations
Lead-Acid Storage Battery
While all lead-acid storage batteries are not alike, a
description is provided below of a typical lead-acid
storage battery (i.e., a car battery) that is likely to have
been processed at a defunct LBRS that is now on the
Superfund cleanup list.
A lead-acid storage battery consists of two electrodes
dipped into partly diluted sulfuric acid. The electrodes
consist of metallic lead grids containing either lead dioxide
paste (cathode) or spongy lead (anode). The metallic
lead grids may contain various elemental additives
including antimony, arsenic, cadmium, copper, and tin.
An average automotive battery weighs 17.2 kg, and
contains 8.6-9.1 kg of lead (equally divided between
anode and cathode), 1.4 kg of polypropylene plastic, and
approximately 2 liters of 15-20% sulfuric acid. Although
most battery cases are now constructed of polypropylene,
they were previously composed primarily of hard rubber-
like material that was called ebonite.
Battery Breaking and Secondary Lead Smelting
Description
The lead recovery aspects of lead-acid battery
recycling operations consist of battery breaking,
component separation, lead smelting and refining, as
shown in Figure 1. Battery breaking is the first step in the
lead recycling process. The flow diagram in Figure 2
depicts the lead-acid battery breaking process. Most
breakers are either hammer mills or saw-type breakers.
The smelting process separates the metal from im-
purities in either blast, reverberatory, or rotary furnaces.
Refining is the final step in chemically purifying recycled
lead.
Lead Battery Recycling Site Characterization
Lead contaminated media at LBRS can be classified
into four main groups:
Soils, sediments, and sludges - includes soils and
paniculate matter intermixed with water or other
aqueous components.
Waste piles - by-products from battery recycling
operations.
Water - includes groundwater, surface water and
contaminated wash water or process waters from
soils, sediments, and sludges treatment processes.
Buildings, structures and equipment - includes all
process structures, buildings and equipment.
An example of a LBRS conceptual model for
potential pathways of exposure is presented in Figure 3.
Lead is the primary contaminant found in soils,
sediments, and sludges at LBRS. Concentrations ranging
up to 7% have been encountered. Lead (Pb), lead sulfate
(PbSO4), lead oxide (PbO), and lead dioxide (PbO2) are
the predominant lead species found at a LBRS. Sites with
carbonate soils generally contain lead carbonate (PbCO3),
hydrocerussite (Pb3(CO3)2(OH)2), or lead hillite (Pb4SO4
(C03)2(OH)2). Other heavy metals such as antimony,
arsenic, cadmium, and copper are sometimes present, but
normally in relatively low concentrations.
Soil cleanup goals vary depending on site specific
factors such as exposure routes and location of humans
and sensitive environmental receptors. In spite of this site
to site variability, two common cleanup goals do tend to
recur. One of these includes reduction of lead
concentrations in the soil, sediment, or sludge to the point
that the leachate yields less than 5 mg/L of lead when
subjected to an EPA-mandated leaching procedure (i.e.,
EP Toxicity or TCLP tests). Soils with TCLP leachates
above 5 mg/L lead are considered to be hazardous
waste, which means that the soils generally cannot be
landfilled until they have been treated to yield a leachate
less than 5 mg/L lead (Federal Register, 1990). A second
common cleanup goal is the reduction of the total lead
content in residential soil to a level of 500 to 1000 mg/kg.
In accordance with EPA Office of Solid Waste and
Emergency Response (OSWER) Directive #9355.4-02, an
Engineering Bulletin: Selection of Control Technologies for Remediation of Lead Battery Recycling Sites
-------
Market
Rubber/Ebonite
Plastic
Acid
Disposal
Market
Figure 1. Generalized Secondary Lead Smelting/Refining Process
Source: Exide Corporation, 1992
Batteries
Dkect dischari
to environmen
(primarily hammer mill
or saw-type breaker)
Acid
I
Add recycle
Plastic, rubber/ebonite
Flotation
Cdtectio'n facility| »| Treatment \-
Rubber/ebonite
Plastic
Fuel supplement
Fill and paving material
Oil drilling mud additive
Other
Disposal
Recycling *
Battery cases
Fuel
Other
j- Secondary toad smelters |
* Feasibility of reuse/recycling depends upon several
factors including: quantity, quality of materials,
economics, technical feasibility, and regulations.
Figure 2. Flow diagram of lead-acid battery breaking.
Engineering Bulletin: Selection of Control Technologies for Remediation of Lead Battery Recycling Sites
-------
Exposure
Route
Receptor
Human
Area
Residents
Site
Visitors
Biota
Terrestrial Aquatic
*
f uust r*"
Infiltration
Percolatio
. water
fi
1
-*
*
wing |
Ground-
water
_ ,
water and
-»
Dermal
Contact
Ingest bn
. Inhalation
Dermal
Contact
Ingest ion
Inhalation
Dermal
Contact
Inhalation
V
V
V
Dermal
Contact
Buildings, structures,
and equipment
Dermal
Contact
Figure 3. A lead battery recycling site conceptual model.
Interim soil cleanup level of 500 to 1,000 mg/kg total lead
was adopted for protection from direct contact at
residential settings. OSWER is in the process of revising
this directive to account for the contribution of various
media to total lead exposure and to produce a strong
scientific basis for choosing a soil lead cleanup level for a
site. OSWER believes that the best available approach is
to use the EPA uptake biokinetic model (USEPA, 1991 a).
Lead is generally not very mobile in the environment,
and tends to remain relatively close to its point of initial
deposition following its escape from the recycling process.
Soils strongly retain lead in their upper few centimeters.
The capacity of soil to adsorb lead increases with
increasing pH, cation exchange capacity, organic carbon
content, soil/water Eh (redox potential), and phosphate
levels. Lead exhibits a high degree of adsorption on clay-
rich soil. Lead compounds can also be adsorbed onto
hydrous oxides of iron and manganese and be
immobilized in double and triple salts. Metallic lead and
its compounds are heavier than water and tend to settle
out. Some of the compounds are slightly soluble while
Engineering Bulletin: Selection of Control Technologies for Remediation of Lead Battery Hecyciing bites
-------
others are insoluble in water. Throughout most of the
natural environment, the divalent form, Pb*2, is the most
stable ionized form.
Geophysical surveys can be used to determine the
vertical and lateral variations in both subsurface
stratigraphy and subsurface metal contamination. A
variety of survey techniques (e.g., ground penetrating
radar, electrical resistivity, electromagnetic induction,
magnetometry, and seismic profiling) can effectively detect
the locations and extent of buried waste deposits.
Borehole geophysics investigations can be conducted at
selected well locations in order to better characterize
subsurface stratigraphy. Field screening techniques such
as x-ray fluorescence (XRF) can be used to pinpoint
sampling locations at areas of greatest contamination
("hot spots"). To identify the level of risk presented by the
site and to evaluate remedial alternatives, soil samples are
typically analyzed in the laboratory for the USEPA Target
Analyte List (TAL) metals, TCLP toxicity, total cyanide,
total organic carbon, sulfate content, pH, acidity/alkalinity,
and cation exchange capacity.
Waste piles at LBRS are usually by-products from
recycling operations. These waste piles can be broken
down into several components: battery casings (made of
hard rubber-like composites or polypropylene), battery
internal components (e.g., polyvinyl chloride, paper),
matte (a metallic sulfide waste containing iron and lead),
slag, and contaminated debris. Waste samples are
analyzed for the parameters mentioned above.
Groundwater does not normally create a major
pathway for lead migration. However, since lead com-
pounds are soluble at low pHs, if battery breaking activi-
ties have occurred on-site, and the battery acid was
disposed on-site, elevated concentrations of lead and
other metals may occur in groundwater. Monitoring wells
are installed and sampled upgradient and downgradient
from a lead battery recycling site. To identify the level of
risk presented by the site and to evaluate remedial
alternatives, samples from the wells are analyzed for TAL
metals, total cyanide, total organic carbon, total
suspended solids, total dissolved solids, pH, alkalin-
ity/acidity, hardness, sulfate, chloride, specific conduc-
tance, temperature, and dissolved oxygen. The Office of
Emergency and Remedial Response (OERR) has
recommended an interim potable groundwater cleanup
level of 15 ppb for lead (USEPA, 1990a).
A variety of contaminated structures, buildings, and
equipment may be encountered at LBRS. Sampling
methods to determine the nature and extent of
contamination on buildings, structures, and equipment
surfaces have not yet been standardized. Surface-wipe
sampling is generally used.
Basic Approaches to the Control of Lead Battery
Recycling Sites
Remediation strategies for LBRS may incorporate
several distinct technology options assembled into a
treatment train to attain specific site goals. These
technologies include:
No action
Immobilization: preventing contaminant migration
through construction of physical barriers (e.g., caps,
slurry walls, liners) or utilizing chemical or thermal
processes (e.g., solidification/stabilization and
vitrification).
Separation/concentration: includes technologies
utilizing chemically or physically induced phase
separation processes to concentrate lead
contamination for further treatment, partial recycling,
or disposal while remediating a major portion of the
contaminated material.
Excavation and off-site disposal: removal of
contamination for disposal.
Treatment Technologies for Soils, Sediments, and
Sludges
No Action
Two out of 10 Record of Decisions (RODs) for LBRS
have selected no action as a remedial alternative, because
the results of the Remedial Investigation (Rl) showed that
the emergency removal processes (excavation and off-site
disposal) conducted at sites were effective in removing
contaminated soil from the site and the concentrations of
contaminants found in the groundwater were below any
applicable or relevant and appropriate requirements
(ARARs). No action involves environmental monitoring
and institutional restrictions such as site fencing, deed
restrictions, restrictions on groundwater usage, warning
against excavation and a public awareness program.
Engineering Bulletin: selection of Control Technologies tor Remediation of Lead Battery Recycling Sites
-------
Immobilization Options
Capping-
To date five out of 10 RODs for LBRS have selected
capping as an integral part of a treatment alternative.
Capping involves the installation of an impermeable barrier
over the contaminated soil to restrict access and reduce
infiltration of water into the soil. A variety of cap designs
and materials are available. Most designs are multi-
layered to conform with the performance standards in 40
CFR 264.310 which addresses RCRA landfill closure
requirements. However, single-layered designs are used
for special purposes at LBRS, for example, when treated
soil is backfilled into an excavated area. Low permeability
clays and synthetic membranes are commonly used.
They can be covered with top soil and vegetated to
protect them from weathering and erosion. Soil materials
are readily available, and synthetic materials are widely
manufactured and distributed.
The cost of a cap depends on the type and amount
of materials selected, the thickness of each layer, and the
region. In a recent RCRA Part B permit application for a
four acre hazardous waste landfill, the installed cost of a
multi-layered cap was estimated at SS/ft2, The design for
this cap included 3 ft of top soil, overlying a 1 ft sand
layer, overlying 1 ft of compacted clay, overlying a 30 mil
High Density Polyethylene (HOPE) liner, overlying 2 ft of
compacted clay (USEPA, 1985).
Table 1 summarizes the data needed to evaluate
capping as a remedial alternative for soils, sediments, and
sludges.
Solidification/Stabilization (S/S)-
To date, 5 out of 10 RODs for LBRS have selected ex
situ S/S as an integral part of a treatment alternative.
Solidification processes, either in situ or ex situ, produce
monolithic blocks of waste with high structural integrity.
The contaminants do not necessarily interact chemically
with the solidification reagents (typically cement/lime) but
are primarily mechanically locked within the solidified
matrix. Stabilization methods usually involve the addition
of materials such as fly ash or blast furnace slag which
limit the solubility or mobility of waste constituents -- even
though the physical handling characteristics of the waste
may not be changed or improved (USEPA, 1982). Ex situ
S/S is widely demonstrated and equipment is readily
available. However, long-term reliability of S/S is not yet
established.
Ex situ S/S involves mixing the excavated
contaminated soil with portland cement and/or lime along
with other binders such as fly ash or silicate reagents to
produce a strong, monolithic mass. Cement is generally
suitable for immobilizing metals (such as lead, antimony,
and cadmium) which are found at lead battery recycling
sites. Because the pH of the cement mixture is high
(approximately 12), most multivalent cations are converted
into insoluble hydroxides or carbonates. They are then
resistant to leaching.
Costs to use S/S technology are expected to be in
a range of $30-$170 per cu yd (USEPA, 1989a). Data
needs to evaluate S/S as a remedial alternative are
summarized in Table 1.
Three full-scale S/S operations have been
implemented at LBRS. Approximately 7,300 tons of soil
contaminated with lead (EP Tox >400 mg/L) were treated
in a mobile plant with portland cement, fly ash, and water
at a rate of 300 tons/day at Norco Battery Site in
California. EP Toxicity of the treated soil after 28 days
was less than 5 mg/L (USEPA, 1991b). Approximately
11,000 tons of soil (TCLP as high as 422 mg/L) were
treated by the proprietary MAECTITE process developed
by Maecorp, Inc. at the Lee's Farm in Wisconsin. TCLP
of the treated soil was less than 1 mg/L. About 20,000
cubic yards of lead-contaminated soil were recently
solidified at Cedartown Battery, Inc. in Georgia. Analytical
data on this site are currently being processed.
Numerous S/S treatability studies have been
completed at LBRS. A pilot-scale treatability test
conducted at the Gould Site in Oregon demonstrated that
a mix of approximately 14% portland cement Type Ml,
25% cement kiln dust, and 35% water successfully
stabilized soils and waste products crushed to 1 /8 in. size.
Bench-scale treatability studies conducted on soils from
three LBRS (C&R Battery Site in Virginia, Sapp Battery
Site in Florida, Gould Site in Oregon) demonstrated that
cement-based (i.e., cement or cement with additives)
blends decreased the teachability of lead and met the EP
Toxicity criterion of 5 mg/L.
Engmeenng Bulletin: Selection of Control Technologies for Remediation of Lead Battery Recycling Sites
-------
TABLE 1. DATA NEEDS FOR TREATMENT TECHNOLOGIES FOR SOILS, SEDIMENTS, AND SLUDGES
Technology
Data requirement
Capping
(USEPA, 1987a)
Solidification/stabilization
(USEPA, 1986a and Arniella et al., 1990)
Soil washing/acid leaching
(USEPA, 1989c and USEPA, 1990c)
Off-site land disposal
(USEPA, 1987b)
Extent of contamination
Depth to groundwater table
Climate
Waste volume
Metal concentrations
Moisture content
Bulk density
Grain-size distribution
Waste volume
Sulfate content
Organic content
Debris size and type
TCLP
Soil type and uniformity
Moisture content
Bulk density
Grain-size distribution
Clay content
Metal concentrations/species
pH
Cation exchange capacity
Organic matter content
Waste volume
Mineralogical characteristics
Debris size and type
TCLP
Soil characterization as dictated by the landfill
operator and the governing regulatory agency
Waste volume
TCLP
In situ treatment of contaminated soils is innovative.
Two specific in situ S/S techniques, under the Superfund
Innovative Technology Evaluation (SITE) Program, hold
promise for LBRS.
International Waste Technologies/Geo-Con, Inc.-
This in situ solidification/stabilization technology
immobilizes organic and inorganic compounds in wet or
dry soils, using additives to produce a cement-like mass.
The basic components of this technology are: a deep soil
mixing system (DSM) which delivers and mixes the
chemicals with the soil in situ; and a batch mixing plant to
supply the International Waste Technologies (IWT) propri-
etary treatment chemicals. The IWT technology can be
applied to soils, sediments, and sludges contaminated
with organic compounds and metals. The SITE Demon-
stration of this technology occurred at a PCB-
contaminated site in April, 1988 and the results are
summarized in an Applications Analysis Report (USEPA,
1990b).
S.M.W. Seiko, Inc.- The Soil-Cement Mixing Wall
(S.M.W.) technology developed by Seiko, Inc. involves the
in situ stabilization and solidification of contaminated soils.
Multi-axis, overlapping, hollow-stem augers are used to
inject solidification/stabilization agents and blend them
with contaminated soils in situ. The product is a
monolithic block down to the treatment depth. This
Engineering bulletin: selection of Control Technologies for Remediation of Lead Battery Recycling Sites
-------
technology is potentially applicable to soils contaminated
with metals and semi-volatile organic compounds. The
search for a demonstration site is currently underway.
Vitrification-
As with solidification, there are both ex situ and in situ
procedures for vitrification. In situ vitrification converts
contaminated soils into chemically inert, stable glass and
crystalline materials by a thermal treatment process.
Large electrodes are inserted into soil containing
significant levels of silicates. Because soil typically has low
conductivity, flaked graphite and glass frit are placed on
the soil surface between the electrodes to provide a
starter path for electric current. A high current passes
through the electrodes and graphite. The heat melts
contaminants, gradually working downward through the
soil. Volatile compounds are collected at the surface for
treatment. After the process ends and the soil has cooled,
the waste material remains fused in a chemically inert and
crystalline form that has very low leachability rates. This
process can be used to remove organics and/or
immobilize inorganics in contaminated soils or sludges.
It has not yet been applied at a Superfund site. However,
it has been field demonstrated on radioactive wastes at
the DOE's Hanford Nuclear Reservation by the Geosafe
Corporation. Geosafe has also contracted to conduct two
superfund site cleanups, one in Spokane, WA, and
another in Grand Ledge, Ml. Large-scale remediation of
this process has been suspended temporarily because of
the loss of offgas confinement and control during the
recent large-scale testing of its equipment that resulted in
fire.
Ex situ vitrification involves heating the excavated soil
by a thermal process to form chemically inert materials.
Two specific ex situ vitrification techniques under the SITE
Program have application to LBRS.
Retech, Inc. Plasma Reactor-This thermal treatment
technology uses heat from a plasma torch to create a
molten bath that detoxifies contaminants in soil. Organic
contaminants vaporize and react at very high
temperatures to form innocuous products. Solids melt
into the molten bath. Metals remain in this phase, which -
- when cooled - forms a non-leachable matrix. It is most
appropriate for soils and sludges contaminated with
metals and hard-to-destroy organic compounds. This
technology was demonstrated in August 1991 at a
Department of Energy research facility in Butte, Montana
and the final demonstration report will be completed in
August 1992.
Babcock and Wilcox Co. Cyclone Furnace
Process-This cyclone furnace technology is designed to
decontaminate wastes containing both organic and metal
contaminants. The cyclone furnace retains heavy metals
in a non-leachable slag and vaporizes organic materials
prior to incinerating them. The treated soils resemble
natural obsidian (volcanic glass), similar to the final
product of vitrification. This technology is applicable to
solids and soil contaminated with organic compounds and
metals. This technology was demonstrated in November
1991 at Babcock and Wilcox Co. research facility in
Alliance, Ohio.
Separation/Concentration Potions
Soil Washing and Acid Leaching-
Soil washing is a water-based process for
mechanically scrubbing soils ex situ to remove
undesirable contaminants. The process removes
contaminants from soils in one of two ways: by dissolving
or suspending them in the wash solution or by
concentrating them into a smaller volume of soil through
simple particle size separation techniques. Acid leaching
removes lead from soils by first converting the lead to a
soluble salt, and then precipitating a lead salt from
solution.
Implementation of this technology requires
excavating the lead-contaminated soil, washing the lead
on-site with a solution (such as nitric acid or EDTA), and
returning the treated soil to the site for disposal in the
excavation area. One of the limitations of soil washing as
a viable alternative concerns the physical nature of the
soil. Soils which are high in clay, silt, or fines have been
difficult to treat.
Figure 4 is a process flow diagram of an acid
leaching process developed by U.S. Bureau of Mines.
This process converts lead sulfate and lead dioxide to
lead carbonate, which is soluble in nitric acid. Lead is
recovered from the leaching solution by precipitating with
sulfuric acid (Schmidt, 1989). There is a potential market
for lead sulfate. The Bureau of Mines also investigated
converting the lead compounds to carbonates followed by
leaching with fluosilicic acid. Electrowinning recovers
metallic lead from solution while regenerating the acid for
Engineering Bulletin: Selection of Control Technologies for Remediation of Lead Battery Recycling Sites
-------
FEED
| ACID WASH
RINSE
CASINGS
OVERSIZE
(+4 INCH )
I CARBO ATION
. !
in
LJ
SOIL
RINSE »pu
IAPin
H2SO« 4 PRECin
RINSE
«-*-WASTE
RINSE
ER
TATION |
-- i ^ finnrtr
iTinu 1
MAKEUP
HN03
Figure 4. Bureau of Mines acid leaching process.
Source: Schmidt, 1989.
UME
GYPSUM
engineering awiean: oarecoon or uorarof lecnnoiogies tor Hemeaiation or Lead Battery Recycling Sites
-------
recycle. The clean soil can be returned to the site but
waste streams from either soil washing processes require
further treatment before final discharge.
Actual field experience of cleaning soil at LBRS is
limited. Two sites (Lee's Farm in Woodville, Wisconsin
and ILCO site in Leeds, Alabama) have unsuccessfully
attempted soil washing of contaminated soil. One ROD
(United Scrap Lead Co. Site in Ohio) out of 10 for LBRS
has selected acid leaching as an integral part of the
treatment alternative but full-scale treatment has not
occurred. The Bureau of Mines (BOM) conducted bench-
scale studies to evaluate the performance of acid leaching
solutions on lead in contaminated soil at battery recycling
sites. Table 2 shows some representative results from the
Bureau of Mines tests. The results indicated that nitric
acid solutions can achieve very high removal efficiencies
for soil (greater than 99%) and an EP Toxicity level less
than 1 mg/L (Schmidt, 1989). BOM estimates the cost of
full-scale operation to be $208 per cu yd of soil.
EPA completed a series of laboratory tests on soil
and casing samples from metal recycling sites. The soil
samples from these sites were subjected to bench-scale
washing cycles using water, EDTA, or a surfactant (Tide
detergent), respectively. Soil washing did not remove
significant amounts of lead from any of the soil fractions.
The lead was not concentrated in any particular soil
fraction but rather was distributed among all the fractions.
A comparison of lead concentrations in the wash waters
indicated that the EDTA wash performed better than the
surfactant and water washes (PEI Associates Inc., 1989).
While EDTA was reasonably effective in removing lead,
Bureau of Mines researchers observed that its effective-
ness seemed to vary with the species of lead present
(Schmidt, 1989). Additional bench-scale studies are
required to verify that site-specific cleanup goals can be
achieved employing these techniques. EPA researchers
are also in the early stages of investigating the use of
milder acids (e.g., acetic acid) than those acids used to
date (e.g., nitric, fluosilicic) for leaching of lead from soils
(USEPA, 1990d).
TABLE 2. REPRESENTATIVE RESULTS OF THE BUREAU OF MINES TREATABILITY
ON SELECTED SAMPLES OF BATTERY BREAKER SOIL WASTES
TESTS
Site/waste
United Scrap Lead soil
United Scrap Lead soil
Arcanum soil
Arcanum soil
C&R Battery Soil Sample B
Common
lead
species
Pb, PbSO4, PbOx
Pb, PbSO4, PbOx
Pb (6.6%), PbSO4
Pb (6.6%), PbSO4
Pb, PbS04>
PbCO3, PbO2
Average*
lead
total
(ppm)
8,000-18,000
8,000-18,000
71,000
71,000
17,000
Leaching
method
15% HNO3, 2-hr wash and 1%
HNO3, 24-hr soak
80 g/L F* 4-hr & 20 g/L F* 4-
hr, 2-stage wash, 1% HNO3, 24-
hr soak
80 g/L F*, 4-hr, 50°C & 20 g/L
F* 4-hr, 50°C, 2-stage leach
and 1%HNO3, 24-hr wash
15% HNO3, 2-hr, 50°C leach
and 1% HNO3, 50°C, 24-hr wash
15% HNO3, 2-hr and 2% HNO3,
24-hr wash and 1-hr water rinse
Total
lead
(ppm)
200
203
334
<250
29
EP
Toxicity
(mg/L)
<1.0
<1.0
0.26
<1.0
<0.1
"No initial EP Toxicity data available.
F* Ruosilicic acid
Source: Schmidt, 1989
10
Engineering Bulletin: Selection of Control Technologies tor Remediation or Leaa aanery hecyciing cwzes
-------
European vendor firms in the soil washing business
have been remediating for a number of years sites
contaminated with lead. Most of their experience has
been with relatively lower lead concentrations (typically
less than 500 ppm) from mine tailings and smelter waste
materials (bag house dust and slag). No European firms
have been found to date who have direct experience in
treating soils from lead battery recycling sites (or
equivalent) where the lead contamination typically could
be around 7,000 ppm total lead. However, in discussions
with certain of these vendors, they are of the opinion that
soil washing may have application although bench-scale
treatability tests would be needed to verify performance.
Soil Excavation and Off-Site Disposal
Excavation and removal of contaminated soil to a
RCRA landfill have been performed in the past at LBRS
but probably will not continue unless the materials are
treated prior to disposal due to land disposal restrictions
(LDRs). Excavation and removal are applicable to almost
all site conditions, although they may be cost-prohibitive
for sites with large volumes, greater depths or complex
hydrogeologic environments. Determining the feasibility
of off-site disposal requires knowledge of LDRs and other
regulations developed by state governments. Without
treatment, this technology may not meet RCRA LDRs.
The LDRs prohibit the land disposal of certain RCRA
hazardous wastes unless they meet specified treatment
standards. If lead-contaminated wastes (i.e., soils and
fragments of battery cases) fail the Toxicity Characteristic
Leaching Procedure (TCLP) test with lead levels equal to
or greater than 5.0 mg/L, then, if excavated, their
subsequent handling and disposal must comply with
RCRA hazardous waste regulations.
Cost estimates for this technology range from $287-
$488 per cu yd of soil.
Treatment Technologies for Waste Piles
Waste pile removal and off-site disposal have been
practiced in the past but probably will not continue due to
LDRs, unless the materials are treated prior to disposal.
Table 3 summarizes the data needs for treatment
technologies for waste piles.
Washing of Battery Casings
This technology, developed by the Bureau of Mines
(BOM), is similar to acid leaching of soil but somewhat
less complicated. Lead contamination is principally in the
form of PbSO4 in microcracks in the casing. Casing
materials are granulated to less than 3/8 inch to create
enough exposed surface area that the PbSO4 could then
be successfully removed by the leaching agent such as
nitric acid.
There has been no actual field experience to date in
the washing of battery casings at lead battery recycling
sites. BOM conducted bench-scale treatability studies that
showed good removal efficiencies (Table 4). The residual
battery casing materials have an EP Toxicity lead
concentration less than 5 mg/L (Schmidt, 1989).
Separation and Cleaning of Battery Casings
This alternative comprises excavation of the waste
piles, followed by on-site separation of battery casing
fragments. Separation is followed by recycling (possibly
off-site) of those components that have recycle value;
RCRA off-site disposal of hazardous non-recyclable
components; and on-site disposal of nonhazardous
components.
Canonie Environmental Services Corp. under
contract to NL Industries, Inc. has developed a proprietary
process for remediating lead battery and smelting wastes
at the Gould Site in Portland, Oregon (Canonie
Environmental, undated). The process separates the
waste materials into recyclable and nonrecyclable
products. The recyclable products consist of:
Materials with a lead content sufficiently high for
recycling, and
Cleaned materials such as plastic and ebonite that
will pass the EP Toxicity test for lead.
The materials that cannot be cleaned to pass the EP
Toxicity test for lead and do not contain sufficient
lead for recycling are considered "nonrecyclable".
The process is shown schematically in Figure 5. The
battery casing is crushed and washed in the first stage.
The fines are screened from the washed material, the
engineering uuiiean: oe/ecoon or Control technologies for Remediation of Lead Battery Recycling Sites
11
-------
TABLE 3. DATA NEEDS FOR TREATMENT TECHNOLOGIES
FOR WASTE PILES
Technology
Data requirement
Off-site landfill
(USEPA, 1987b)
Washing of battery casings
Separation of battery casings
Recycling
Waste pile characterization as dictated
by land disposal restrictions
Waste volume
TCLP
Casing type
Bulk density
Grain-size distribution
Metal concentrations
TCLP
Composition of battery casings
Metal concentrations
Waste volume
Other information required by recipient
TCLP
Potential buyer/user
Allowable lead content in ebonite/plastic for use
as fuels
Lead content for acceptance by smelter
TABLE 4. REPRESENTATIVE RESULTS OF THE BUREAU OF MINES TREATMENT TESTS ON
SELECTED CHIP SAMPLES OF BROKEN BATTERY CASING WASTES
Site/waste
United Scrap lead granulated
chips
Arcanum broken chips
C&R Battery casing chips
Gould buried casing chips
(broken)
Rhone-Poulenc casing chips
(broken)
Common
lead
specie*
PbSO4, Pb
PbSO4, Pb
PbSO4, Pb
PbCO3, PbSO4
PbC03
Average*
lead
total
(ppm)
3,000
3,000
175,000
193,000
65,000
Leaching
method
0.5% HNO3, 1-hr, 20° C wash
1% HNO3, tap water, 50°C, 24-hr,
agitated
1% HNO3 4-hr, wash and water
rinse
Ammonium carbonate carbonation,
1% HNO3, 20°C, 4-hr wash
Calcium carbonate carbonation,
0.5% HNO3, 20°C, 1-hr wash
Total
lead
(ppm)
86
210
277
145
516
EP
ToxteHy
(mgA)
<0.2
<3.5
0.15
0.52
3.68
No initial EP Toxicity data available.
Source: Schmidt, 1989
12
Engineering Bulletin: Selection of Control Technologies for Remediation of Lead Battery Recycling Sites
-------
WATER TO
RECYCLE OR
DISCHARGE
Figure 5. Battery waste treatment process.
Source: Canonie Environmental.
tngineenng Bulletin: selection or control Technologies for Remediation of Lead Battery Recycling Sites
13
-------
solids are separated from the water in a settling tank, and
the settled pulp is filtered from the solution. These
materials are the filter cake that will typically contain more
than 40% lead and less than 30% moisture. Following the
first wash, the screen oversize is fed to a gravity separa-
tion device. This system separates the plastic and ebonite
in the waste from furnace products, rocks, and trash
excavated with the waste. The ebonite and plastic
material passes to the second wash stage where the
residual amounts of lead contamination are removed.
Performance at the Gould Site-The Gould site
contains approximately 117,500 tons of waste. Canonie
claims that its separation and washing process there
could produce approximately 80,500 tons of recyclable
materials and 37,000 tons of material for stabilization and
subsequent on-site disposal. At other sites, the amount of
recyclable material may vary according to site history and
use (Canonie Environmental, undated).
Canonie Environmental conducted a marketing study
to identify the markets for the products from the above
process. The market suggested for the lead fines are
primary and secondary lead smelters. Plastic, if it can be
suitably cleaned, appears to have numerous potential
users. The most likely market for ebonite from the Gould
site appears to be as a fuel supplement for cement kilns
or power plants (Canonie Environmental, 1990).
Additional market research is planned to assess the effect
of the new RCRA boiler and industrial furnace regulations
regarding combustion of hazardous wastes. As noted
below, secondary lead smelters are potential users of hard
rubber-like battery casings, but none are sufficiently close
to the Gould site.
Innovative Processes for Waste Piles Treatment
The Horsehead Resource Development Co., Inc.
Flame Reactor Process~A patented, hydrocarbon-fueled,
flash smelting system that treats residues and wastes
containing metals. The reactor processes wastes with a
very hot reducing gas >2000°C produced from the
combustion of solid or gaseous hydrocarbon fuels in
oxygen-enriched air. In a compact, low cost reactor, the
feed materials react rapidly, allowing a high waste
throughput. The end products are a non-leachable slag
(glass-like when cooled) and a recyclable heavy metal-
enriched oxide, which may be marketable. This
technology has potential application to soils contaminated
with heavy metals. A SITE demonstration was performed
at the Monaca facility in Pennsylvania in March 1991. The
waste material was a secondary lead smelter blast furnace
slag from the National Smelting and Refining Site in
Atlanta, Georgia. Lead and other metals were removed
from the raw waste and concentrated in the bag house
dust which may be recycled for its lead content. The
process reduced the lead content of the slag from 5.4% to
0.6%. All samples of processed waste slag passed the
TCLP test for metals. For lead, the TCLP values fell from
approx. 5 mg/Lto <0.33 mg/L (USEPA, 1991c).
The Risk Reduction Engineering Laboratory
(RREL) Debris Washing System (DWS)-Developed by
RREL staff and IT Environmental Programs, Inc., this
technology will decontaminate debris found at Superfund
sites throughout the country. The DWS can clean various
types of debris (e.g., metallic, masonry, or other solids)
that are contaminated with hazardous chemicals such as
pesticides, PCBs, lead, and other metals. Site
demonstration was performed at three Superfund sites
(Carter Industrial Superfund Site in Detroit, MT, PCB-
Contaminated Site in Hopkinsville, KY, and Shaver's Farm
Site in Walker County, GA).
Bench-scale studies conducted on six pieces of
debris including plastic spiked with DDT, lindane, PCB and
lead sulfate, then washed using surfactant achieved an
overall percentage reduction of lead greater than 98%.
This technology has potential application to battery
casings and other metallic and masonry debris found at
LBRS.
As part of the emerging technology portion of the
SITE Program, the Center for Hazardous Materials
Research (CHMR) proposes to research, develop, and
evaluate the economics of using secondary lead smelters
for the recovery of lead from rubber battery casings.
Secondary lead smelting technology is a process which
may be able to remove the lead from the battery casings
and other waste materials. The net result will be the
detoxification of these materials while providing a usable
product (i.e., reclaimed lead). A test was conducted in
September 1991 with five truckloads of battery casing
material at Exide's Reading, PA smelter. The initial results
were promising, but the project report has not yet been
published.
14
Engineering Bulletin: Selection of Control Technologies for Remediation of Lead Battery Recycling Sites
-------
Treatment Technologies for Water
Treatments using precipitation/flocculation/
sedimentation and Ion exchange are often considered for
remediation of LBRS. Contaminated water from pits,
ponds, and lagoons is typically pumped and treated
together with groundwater.
Table 5 summarizes the data needs for treatment
technologies for water.
Precipitation/Flocculation/Sedimentation
The combination of precipitation/flocculation/
sedimentation is a well-established technology with
specific operating parameters for metals removal from
ground and surface waters. Typical removal of metals
employs precipitation with hydroxides, carbonates, or
sulfides. Generally lime, soda ash, or sodium sulfide is
added to water in a rapid-mixing tank along with
flocculating agents such as alum, lime, and various iron
salts. This mixture then flows to a flocculation chamber
that agglomerates particles, which are then separated
from the liquid phase in a sedimentation chamber.
Hydroxide precipitation with lime is the most common
choice. Metal sulfides exhibit significantly lower solubility
than their hydroxide counterparts, achieve more complete
precipitation, and provide stability over a broad pH range.
At a pH of 4.5, sulfide precipitation can achieve the EPA-
recommended standard for final cleanup level for lead in
groundwater usable for drinking water (I.e., 15 ^9/L).
Sulfide precipitation ~ often effective ~ can be
considerably more expensive than hydroxide precipitation,
due to higher chemical costs and increased process
complexity. The precipitated solids would then be
handled in a manner similar to contaminated soils. The
supernatant would be discharged to a nearby stream or to
a publicly owned treatment works (POTW).
Ion Exchange
Ion exchange is a process whereby the toxic ions
are removed from the aqueous phase in an exchange with
relatively harmless ions held by the ion exchange material.
Modern ion exchange resins consist of synthetic organic
materials containing ionic functional groups to which
exchangeable ions are attached. These synthetic resins
are structurally stable and exhibit a high exchange
capacity. They can be tailored to show selectivity towards
specific ions. The exchange reaction is reversible and
concentration-dependent; the exchange resins are
regenerable for reuse. All metallic elements - when
present as soluble species, either anionic or cationic --
can be removed by ion exchange.
TABLE 5. DATA NEEDS FOR TREATMENT TECHNOLOGIES
FOR WATER
Technology
Data requirement
Precipitation/flocculation/sedimentation
(USEPA, 1989b)
Ion exchange
(USEPA, 19895)
Pumping via wells
Total suspended solids
PH
Metal concentrations
Oil and grease
Specific gravity of suspended solids
Total suspended solids
Total dissolved solids
Inorganic cations and anions
Oil and grease
PH
Depth to water table
Groundwater gradients
Hydraulic conductivity
Specific yield estimate
Porosity
Thickness of aquifers
Storativity
. oefecoorr or ^ornroi lecnnoiogies TOT nemeaiaaon of Lead Battery Recycling Sites
15
-------
A practical upper concentration limit of toxic ions for
ion exchange is about 2,500 to 4,000 mg/L. A higher
concentration results in rapid exhaustion of the resin and
inordinately high regeneration costs. Suspended solids in
the feed stream should contain less than 50 mg/L to
prevent plugging the resins (USEPA, 1986b).
Innovative Processes for Water Treatment
The Bio-Recovery Systems, Inc. Biological
Sorption Process-Bio-Recovery Systems, Inc. in Las
Cruces, New Mexico is testing AlgaSORBR, a new
technology for the removal and recovery of heavy metal
ions from groundwater. This biological sorption process
is based on the affinity of algae cell walls for heavy metal
ions. This technology is being tested for the removal of
metal ions that are "hard" or contain high levels of
dissolved solids from groundwater or surface leachates.
This process is being developed under the SITE Emerging
Technologies Program.
Colorado School of Mines' Wetlands-Based
Treatment-This approach uses natural biological and
geochemical processes inherent in man-made wetlands to
accumulate and remove metals from contaminated water.
The treatment system incorporates principal ecosystem
components from wetlands, such as organic soils,
microbial fauna, algae, and vascular plants. Waters which
contain high metal concentrations and have low pH flow
through the aerobic and anaerobic zones of the wetland
ecosystem. The metals can be removed by filtration, ion
exchange, adsorption, absorption, and precipitation
through geochemical and microbial oxidation and
reduction.
Conclusion
EPA's recent publication of the document, Selection
of Control Technologies for the Remediation of Lead
Battery Recycling Sites, EPA/540/2-91/014, enables
EPA, State, and private sector remediation managers to
quickly identify past experience and information that can
be applied to site characterization and control technology
evaluation activities.
Regarding the remediation of soils, sediments, and
sludges, the feasibility of the previously popular remedy of
excavation and off-site disposal has been basically
eliminated unless a waiver can be obtained or the soil is
determined to pose a threat to groundwater, but is not
considered a RCRA hazardous waste. Cement-based S/S
has been implemented at full-scale on at least three sites
(Norco, CA; Lee's Farm.WI; Cedartown Battery, GA) and
is scheduled for implementation at several others. S/S of
soils can be expected to remain a popular option for lead
and other heavy metal contaminated soils, sediments, and
sludges due to (a) relative simplicity, (b) ready availability
of equipment and vendors, and (c) low cost.
Disadvantages include: (a) S/S can cause substantial
increases (e.g., 30%) in the volume of material, (b)
long-term immobilization of lead is not yet demonstrated,
and (c) organic contaminants present in the soil may
interfere with the S/S process.
Should S/S of soils, sediments, and sludges become
obsolete due to observed leaching failures, then the
chances of acceptance of other novel technologies such
as in situ and ex situ vitrification, soil washing, and acid
leaching may improve. In situ and ex situ vitrification may
provide improved permeation and leaching resistance, but
tend to be more complicated and expensive than
cement-based solidification. Soil washing and acid
leaching technologies are more complicated, costly, and
novel than solidification, but they have the potentially
significant advantage of actually removing the lead from
the soil, which should minimize the need for long-term
monitoring and would eliminate the potential of any
long-term leaching problems. The success or failure of
acid leaching technology at the United Scrap Lead Site in
Ohio is viewed as critical to the future acceptability of this
technology for LBRS remediation.
Recycling of waste piles to reduce the volume of
hazardous waste, and to recover lead, lead compounds,
plastic, and hard rubber is a challenge that has continued
to receive considerable attention. To date, large-scale
recycling of defunct LBRS waste materials is not known to
occur. A key site regarding recycling is the Gould site,
Portland, OR where efforts are underway in separating and
recycling of lead fines to a secondary smelter, plastic to
a plastics recycler, and hard rubber-like material as a fuel
supplement. Also important is the Tonolli site,
Nesquehoning, PA where a full-scale treatability study is
examining the feasibility of using hard rubber battery
scraps as a fuel supplement in a nearby secondary lead
smelter. Battery scraps from other defunct LBRS may be
tested as well. For sites where lead leaching from slag is
posing a health or environmental threat, a process (flame
reactor) for recovering lead from slag and simultaneously
converting the slag to a non-hazardous material (i.e.,
16
Engineering Bulletin: Selection of Control Technologies for Remediation of Lead Battery Recycling Sites
-------
TCLP leachate < 5 mg/L lead) is undergoing testing in
EPA's SITE Program. The flame reactor may also be
applicable to lead contaminated soils. Within another
several years, the use of acid leaching for cleaning and
recovery of lead from battery cases may also be
demonstrated at the United Scrap Lead site to be a viable
option.
The selection of control technology for LBRS
remediation is expected to remain an interesting and
Important remediation issue for the next several years.
Acknowledgement
This bulletin was prepared for the U.S. Environmental
Protection Agency, Office of Emergency and Remedial
Response (OERR) and the Office of Research and
Development (ORD) by Foster Wheeler Enviresponse, Inc.
(FWEI) under contract No.68-C9-0033. Mr. Michael D.
Royer served as the EPA Work Assignment Manager. Dr.
Ari Selvakumar was FWEI's Project Leader and primary
author. Mr. Roger Gaire co-authored this bulletin.
References
Arniella, E. F. and L J. Blythe. 1990. Solidifying Traps.
Chemical Engineering, pp. 92-102.
Canonie Environmental. Undated. Information Sheet on
Process for Remediating Lead Battery Sites.
Canonie Environmental. 1990. Marketing Studies Report
for Gould, Inc., Portland, Oregon.
Federal Register. 1990. 40 CFR Parts 148 et al. Land
Disposal Restrictions for Third Third Scheduled Wastes;
Rule. U.S. Environmental Protection Agency, Washington,
DC. pp.22567-22660.
PEI Associates, Inc. 1989. Lead Battery Site Treatability
Studies. Contract No.68-03-3413. Submitted to Risk
Reduction Engineering Laboratory, Edison, New Jersey.
Schmidt, B. William. 1989. Assessment of Treatment
Techniques at Superfund Battery Sites. International
Symposium on Hazardous Waste Treatment: Treatment
of Contaminated Soils, Cincinnati, Ohio.
USEPA. 1982. Guide to Disposal of Chemically Stabilized
and Solidified Waste. SW-872. U.S. Environmental
Protection Agency Office of Solid Waste and Emergency
Response, Washington, DC.
USEPA. 1985. Handbook, Remedial Action at Waste
Disposal Sites (Revised). EPA/625/6-85/006. U.S.
Environmental Protection Agency Office of Emergency
and Remedial Response, Washington, DC.
USEPA. 1986a. Handbook for Stabilization/Solidification
of Hazardous Wastes. EPA/540/2-86/001.
Hazardous Waste Engineering Research Laboratory,
Cincinnati, Ohio.
USEPA. 1986b. Mobile Treatment Technologies for
Superfund Wastes. EPA/540/2-86/003(f). U.S.
Environmental Protection Agency Office of Solid Waste
and Emergency Response, Washington, DC.
USEPA. 1987a. A Compendium of Technologies Used in
the Treatment of Hazardous Wastes.
EPA/625/8-87/014. Center for Environmental Research
Information, Office of Research and Development,
Cincinnati, Ohio.
USEPA. 1987b. Technology Briefs: Data Requirements
for Selecting Remedial Action Technology.
EPA/600/2-87/001. Hazardous Waste Engineering
Research Laboratory, Cincinnati, Ohio.
USEPA. 1989a. Stabilization/Solidification of CERCLA
and RCRA Wastes: Physical Tests, Chemical
Testing Procedures, Technology Screening, and Field
Activities. EPA/625/6-89/022. Center for Environmental
Research Information, Cincinnati, Ohio.
USEPA. 1989b. Guide for Conducting Treatability Studies
under CERCLA. Interim Final.
EPA/540/2-89/058. U.S. EPA Office of Solid Waste and
Emergency Response, Washington, DC.
USEPA. 1989c. Superfund Treatability Clearinghouse
Abstracts. EPA/540/2-89/001. U.S. Environmental
Protection Agency Office of Emergency and Remedial
Response, Washington, DC.
engineering uuuenn. oe/ecoon or uontroi lecnnoiogies Tor Hemediation of Lead Battery Recycling Sites
17
-------
USEPA. 1990a. Memorandum from Henry L Longest,
Director, Office of Emergency and Remedial Response to
Patrick M. Tobin, Director, Waste Management Division,
Region IV, Cleanup Level for Lead in Groundwater. U.S.
Environmental Protection Agency, Office of Emergency
and Remedial Response, Washington, DC.
USEPA. 1990b. International Waste Technologies/Geo-
Con In Situ Stabilization/Solidification, Applications
Analysis Report. EPA/540/A5-89/004. U.S.
Environmental Protection Agency, Office of Research and
Development, Cincinnati, Ohio.
USEPA. 1990c. Treatment Technology Bulletin: Soil
Washing Treatment. EPA/540/2-90/017. U. S.
Environmental Protection Agency Office of Emergency
and Remedial Response, Washington, DC.
USEPA. 1990d. Workshop on Innovative Technologies
for Treatment of Contaminated Sediments. Summary
Report. EPA/600/2-90/054. U.S. Environmental
Protection Agency Office of Research and Development,
Cincinnati, Ohio.
USEPA. 1991 a. Memorandum from Don R. Clay,
Assistant Administrator, Office of Solid Waste and
Emergency Response on Update on Soil Lead Cleanup
Guidance. U.S. Environmental Protection Agency, Office
of Solid Waste and Emergency Response, Washington,
DC.
USEPA. 1991b. Federal On-Scene Coordinators Report
on Norco Battery Site Removal Action. U. S.
Environmental Protection Agency, Region IX, California.
USEPA. 1991c. Demonstration Bulletin: Flame Reactor.
EPA/540/M5-91/005. U.S. Environmental Protection
Agency Office of Research and Development, Cincinnati,
Ohio.
18 Engineering Bulletin: Selection of Control Technologies for Remediation of Lead Battery Recycling Sites
U.S. Government Printing Office: 1992 648-080/60135
-------
-------
United States
Environmental Protection Agency
Center for Environmental Research Information
Cincinnati, OH 45268
Official Business
Penalty for Private Use
$300
Please make all necessary changes on the below label,
detach or copy, and return to the address in the upper
left-hand comer.
If you do not wish to receive these reports CHECK HERE D;
detach, or copy this cover, and return to the address in the
upper left-hand comer.
BULK RATE
POSTAGE & FEES PAID
EPA
PERMIT No. G-35
EPA/540/S-92/011
------- |