United States
Environmental Protection
Agency
Hazardous Waste Engineering
Research Laboratory
Cincinnati OH 45268
Research and Deveiopment
EPA/600/S2-87/099 Jan. 1988
<>ERA Project Summary
Technical Resource Document:
Treatment Technologies for
Corrosive-Containing Wastes,
Volume II
Lisa Wilk, Stephen Palmer, and Marc Breton
This Technical Resource Document
(TRD) for wastes containing corrosives
is one in a series of five documents
which evaluate waste management
alternatives to land disposal. In addition
to this TRD for corrosive wastes, the
other four TRDs in the series address
land disposal alternatives for the fol-
lowing waste categories: dioxins;
solvents; nonsolvent halogenated
organics; and metals/cyanides. The
purpose of these documents is to
provide a comprehensive source of
information that can be used by envir-
onmental regulatory agencies and
others in evaluating available waste
management options, which include
waste minimization and recycling as
well as treatment. Emphasis has been
placed on the collection and interpre-
tation of performance data for proven
technologies. However, all potentially
viable technologies are identified and
discussed. When possible, cost and
available capacity data are provided to
assist the user of the TRDs in assessing
the applicability of technologies to
specific waste streams.
This Project Summary was devel-
oped by EPA's Hazardous Waste Engi-
neering Research Laboratory, Cincin-
nati, OH, to announce key findings of
the research project that is fully doc-
umented in a separate report of the
same title (see Project Report ordering
information at back).
Background
Corrosive acids and alkalis are widely
used by all segments of American
industry and result in the generation of
approximately 40 percent of all RCRA-
regulated hazardous wastes.1 Improper
management of these wastes can result
in altered pH of surface waters to the
detriment of aquatic organisms. Land
disposal of these wastes can also lead
to the solubilization of toxic (e.g., heavy
metals) constituents of co-disposed
wastes, thereby enhancing the potential
for their transport into the environment.2
To combat the potential negative effects
associated with current disposal practi-
ces, the 1984 RCRA Amendments
directed EPA to ban corrosive wastes
from land disposal to the extent required
to protect human health and the
environment.
The land disposal ban excludes acidic
corrosive wastes (pH less than or equal
to 2.0) from land disposal units(excluding
underground injection), effective July 8,
1987. Treatment standards for corro-
sives which are currently managed
through underground injection will be
promulgated on August 8, 1988. Finally,
alkaline corrosive wastes (pH greater
than 12.5) will be banned from disposal
effective May 8, 1990. In addition,
treatment standards for hazardous con-
stituents which are commonly present in
corrosive wastes, such as heavy metals
and toxic organics, are also being pro-
mulgated under the 1984 RCRA Amend-
ments. Thus, prior to land disposal,
corrosive wastes will also have to meet
these standards as they are promulgated.
In fiscal year 1986, the U.S. EPA
Hazardous Waste Engineering Research
-------
Laboratory (HWERL) began developing a
series of technical resource documents
(TRDs) which evaluate waste manage-
ment alternatives to land disposal. These
documents are intended to serve a two-
fold purpose. First, they provide technical
support for current EPA efforts to identify
available alternative waste management
capacity and to evaluate the technical
feasibility of meeting proposed treatment
standards. Secondly, the documents
provide a single, comprehensive source
of technical data to assist waste gener-
ators and regulatory agencies in evaluat-
ing available waste management
options. To date, in addition to the
Corrosives Technical Resource Docu-
ment, three other TRDs have been
completed covering the following waste
categories: dioxins, solvents (halogen-
ated and non-halogenated), and non-
solvent halogenated organics.
Scope
This summary of the Corrosives Tech-
nical Resource Document provides envir-
onmental regulatory agencies and
hazardous waste generators with a
source of technical information describ-
ing corrosive waste management alter-
natives. These options include waste
minimization (i.e., source reduction,
recycling, waste exchange), and treat-
ment and disposal of waste streams.
Emphasis is placed on the collection and
interpretation of performance data for
neutralization and recovery technologies
which have demonstrated both technical
and economic feasibility for handling
corrosives.
Table 1 summarizes potentially appli-
cable corrosive waste management
alternatives for various waste character-
istics and management objectives. With
the exception of recycled or reused
wastes, all corrosive liquids and sludges
will require some form of neutralization
prior to ultimate disposal. Pretreatment
requirements are generally limited to
phase separation, equalization, cyanide
destruction, and chromium reduction.
Post-treatment (i.e, post-neutralization)
requirements vary with contaminant
types and concentrations and selection
of neutralization reagent. Contaminants
of particular concern in residual streams
include heavy metals and toxic organics
which exceed effluent limitations (e.g.,
NPDES, POTW) or land dipsosal treat-
ment standards.
Determination of the overall applica-
bility and availability of these technolo-
gies for managing corrosives required an
understanding of the nature of current
waste management practices. Analysis
of these practices served to identify
available methods which have proven to
be both technologically and economically
capable of treating corrosive wastes. To
a significant extent, waste management
alternatives which will permit industry
to meet EPA disposal requirements (e.g.,
neutralization, metals precipitation,
organic removal techniques) have
already been implemented. This occurred
in response to increased regulatory
requirements and the improved eco-
nomic viability of waste minimization and
treatment options. The latter resulted
from increased disposal costs and liabil-
ity, and advances in waste processing
technology.
Determining the applicability of alter-
native technologies also required an in-
depth understanding of the nature of
corrosive wastes. Data requirements
included the range and variability in
corrosive waste physical, chemical, and
flow (i.e., rate, periodicity) characteristics
which, in turn, required an understand-
ing of corrosive waste industrial origins.
Available data were summarized on a
national basis to assist EPA efforts in
evaluating the existence of available
alternative treatment capacity to manage
wastes which will be excluded from land
disposal. However, these data were
found to be limited. In particular, waste
characteristics from industries other
than the Chemical and Allied Products
Industries (SIC 28) need to be compiled
on a national basis.
Available data on corrosive waste
generation, characteristics and current
management practices are briefly sum-
marized below. This is followed by a
discussion of potential waste manage-
ment alternatives which have been
categorized as either neutralization (with
appropriate pretreatment and post-
treatment) or recycling processes.
Emphasis is placed on identifying pro-
cess design and operating parameters,
and waste characteristics which affect
overall process applicability. This discus-
sion concludes with a summary of
technical and economic factors which
should be considered in the selection of
an optimal waste management system.
Corrosive Waste Generation,
Characteristics, and
Management Practices
The most comprehensive source of
data regarding corrosive waste genera-
tion and management was a study1 based
on the results of the EPA's National
Survey of Hazardous Waste Generators
and Treatment, Storage and Disposal
Facilities(TSDFs) Regulated Under RCRA
in 1981.3 Highlights of the survey results
are as follows:1
• The total quantity of corrosive waste
(D002 and K062; corrosives and spent
pickle liquor from steel finishing
operations) generated in the United
Statesin 1981 was21.8to25.6billion
gallons. This represents approxi-
mately 40 percent of all hazardous
waste generation. However, it
includes mixtures of corrosive and
non-corrosive wastes which signifi-
cantly inflates the total estimate.
• The number of generators of D002
corrosive wastes was 4,705 which
represents over one-third of all RCRA
waste generators. These wastes were
handled at 513 TSDFs in 1981. In
addition, 64 TSDFs handled K062
corrosive wastes.
• The total quantity of corrosive waste
that was reportedly land disposed, and
thus affected by the proposed land
disposal ban, was 3.6 to 4.2 billion
gallons.
• Nearly 95 percent of land disposed
corrosives were liquid acidic wastes.
• Disposal by deep-well injection
accounted for 87 percent of land
disposed corrosives with another 6
percent disposed in surface impound-
ments and 5 percent in landfills.
Waste generation estimates provided
by the National Survey compare favor-
ably with more recent, but less compre-
hensive, projections.4'5 However, data
indicate that these estimates include
large quantities of corrosive waste
mixtures; i.e., corrosives mixed with
other wastes or nonhazardous mate-
rials.6 Thus, actual waste volume at the
point of production (i.e., excluding the
effects of mixing or treatment) may be
lower by 40 percent or more.1'6
The primary industrial applications for
acids and bases which result in gener-
ation of corrosive wastes are: (1) use as
chemical intermediates in the inorganic
and organic chemical manufacturing
industries; (2) use as a metal cleaning
agent in metal production and fabrication
industries; and (3) use in boiler blow-
down and stack gas treatment, primarily
in electricity generating facilities. Other
-------
Table 1. Waste Management AIternatives to Land Disposal
Waste Management
Objective
Applicable Waste TypefsJ
Potential Waste Management
Alternative
Waste minimization
Source reduction
Recycling
All
Concentrated inorganic
liquids (e.g.. plating,
etching solutions)
Raw material substitution Process redesign
Product reformulation Waste segregation
Crystallization
Ion exchange
Evaporation/distillation
Electrodialysis
Solvent extraction
Thermal decomposition
Dilute inorganic liquids
(e.g., plating rinses)
Concentrated organic
liquids (e.g., solvents
with acid/alkali)
Ion exchange
Electrodialysis
Reverse osmosis
Donnan dialysis/
coupled transport
Neutralization followed by recovery such as distillation, evaporation,
steam stripping, or use as a fuel.
Waste exchange
Pretreatment
Concentrated liquids
Dilute inorganic liquids
Liquid with solids
Liquid—two-phase
Liquid or sludge with
cyanide
Recycling
Mutual neutralization
Screening
Distillation
Centrifugation
Decanting
Extraction
Cyanide destruction
through chlorination
Reuse in process with
lower raw material
specifications
Sedimentation
Flotation
Equalization
Flotation
Distillation
Mutual neutralization
Filtration
Settling
Centrifugation
Equalization
Liquid or sludge with
hexavalent chromium
Chromium reduction
Sludge
Bulky solids
Vacuum filtration
Other dewatering
Shredders
Filter press
Hammermills
Centrifugation
Crushers
Neutralization
Acidic waste
Alkaline waste
All
Limestone
Sulfuric acid
Mutual neutralization
Lime
Hydrochloric acid
Caustic soda
Carbonic acid (COi)
Post-treatment
Metal-containing liquid
Trace organic-containing
liquids
Precipitation and
clarification
Adsorption
Dilute organic-containing
liquid
Concentrated organic
liquid
Inorganic sludges and
solids
Biological treatment
Air stripping
Distillation
Extraction
Incineration
Solidification
Chemical oxidation
Incineration
Steam stripping
Supercritical fluids
Use as a fuel
Encapsulation
Ozonation
Evaporation
Wet air oxidation
Landfill
Organic sludges and
solids
Incineration
Wet air oxidation
-------
significant corrosive waste sources
include refining processes in the petro-
leum industry and pulping liquor in the
paper industry. A summary of corrosive
waste quantity handled by various
industrial classification codes (SIC) is
provided in Table 2.1
The majority of corrosive wastes are
handled in onsite wastewater treatment
facilities which ultimately discharge
treated effluents to POTWs or to surface
waters under NPDES permits.1'6 How-
ever, approximately 16.5 percent of all
corrosives were reportedly land disposed
in 1981 in methods which would be
affected by the land disposal restric-
tions.1 A summary of these waste
management practices is provided in
Table 3. As shown, 87 percent of land
disposed corrosives are managed
through deep well injection.1 More
recent data suggest that deep well
injected waste volumes may have
decreased significantly (24 perecent)
since the National Survey data was
collected.8 However, other quantities
presented in Table 3 are expected to
adequately approximate current waste
management practices.
Waste charcteristics of land disposed
corrosives are less well defined. The vast
majority are acidic (82 percent), inorganic
(82 percent), and characterized as dilute
(94.3 percent, liquids only).1 Deep well
injection wastes have a high tendency
to contain toxic organics,6 whereas
landfilled wastes are likely (38 percent)
to contain heavy metals at concentra-
tions which exceed proposed land dis-
posal restrictions.9 Detailed characteri-
zation data for the Chemical and Allied
Products Industries, currently being
compiled by the EPA,6 will enable the
majority of deep well injected wastes to
be characterized. Approximately 60
percent of landfilled wastes are
accounted for by spent pickle liquor from
the iron and steel industry (K062) which
has also been adequately characterized.
However, data are limited for the
remainder of land disposed corrosives.
These data will be required for EPA to
assess the availability of alternative
waste management options when cor-
rosive wastes become prohibited from
land disposal.
Neutralization
Neutralization processes are the most
commonly applied methods for managing
corrosive wastes. Adjustment of waste
pH is typically required prior to subse-
quent treatment processes to limit
corrosion of processing equipment or to
enhance treatment; e.g., metals precip-
itation or biological degradation of toxic
organics.
Alkaline reagents commonly used to
neutralize strongly acidic waste streams
(greater than 5,000 mg/L of mineral acid
strength) include high calcium lime and
caustic soda.1 For the treatment of dilute
acidic waste streams (5,000 mg/L or
less), limestone treatment may also be
economically feasible.10 Mineral acids
such as sulfuric or hydrochloric are the
primary reagents used for the neutral-
ization of corrosive alkaline waste
streams.11 However, alkaline waste
streams which have flow rates of over
100,000 gpd or require greater than 200
tons of reagent per year, may also be
economically treated by liquid carbon
dioxide.12
Pretreatment requirements prior to
neutralization typically consist of gross
solids removal (i.e., filtration), flow
equalization, or treatment of individual
waste streams prior to combination with
other process wastes. These treatments
of segregated wastes result in economic
benefits from reduced reagent costs and
smaller equipment sizing. Common
pretreatment processes include cyanide
destruction, chromium reduction, metals
precipitation from highly chelated
wastes, and oil removal.
Post-treatment of neutralized wastes
which do not contain metals or organics
typically consists of liquid/solid separa-
tion (e.g., clarification) to precipitate
insoluble salts, followed by sludge
dewatering (e.g., filter press) and dispo-
sal in a secure landfill. Post-treatment
of corrosives with metals or toxic organ-
ics depends primarily on their
concentration.13'14
Neutralized waste streams containing
trace organics (less than 500 ppm) would
require additional post-treatment
through technologies such as carbon or
resin adsorption or air stripping.13 Dilute
organic waste streams (500 to 10,000
ppm) are most often economically treated
via biological degradation followed by
filtration and polishing; e.g., activated
carbon.14 Concentrated organic waste
streams usually undergo phase separa-
tion (e.g., dissolved air flotation) follow-
ing neutralization.14 The concentrated
organic phase can be recovered through
distillation, steam stripping, solvent
extraction, or thin film evaporation.13
Table 2. Corrosive Waste Quantity Handled by Industrial Classification (million gallons/
year)
SIC
Code
28
49
29
33
26
36
35
32
34
37
20
Industry Description
Chemicals and allied products
Electric, gas and sanitary services
Petroleum refining
Primary metals
Paper and allied products
Electric and electronic
machinery, equipment and
supplies
Machinery, except electrical
Stone, clay, glass, concrete
Fabricated metals
Transportation equipment
Food and kindred products
Other industries
Total:
Waste
High
18,337
2,305
1,150
1,143
1.126
581
417
190
183
136
27
50
25,645
Quantity Handled"
Low Percent
15.590
1,960
978
972
957
495
354
162
156
115
23
42
21.803
71 5
9.0
45
4.5
4.4
23
1.6
0.7
0.7
05
0.1
0.2
1000
'Includes O002 andK062 only.
Source: National Survey, Reference 1.
-------
Table 3. Management Practice Summary for Corrosive Wastes National Estimates (million gallons)
High Quantity Estimate' Low Quantity Estimate"
Handled0
Disposed0
Injection well
Landfill
Land treatment
Surface impoundment
Other
Treated0
Tanks
Surface impoundment
Incineration
Other
Stored0
Tanks
Containers
Surface impoundment
Waste piles
Other
Recycled"
Onsite:
Generator
TSDF
Offsite:
Generator
TSDF
Corrosive
Waste
D002
24.596
3,970
3,635
85
18
206
26
15.912
7,040
5,614
6
3.252
10.094
1.542
9
6,530
6
2.007
373
330
42
288
43
14
29
Spent
Pickle
Liquor
K062
1.048
236
28
131
56
20
218
139
39
40
265
211
47
7
354
34
6
28
320
170
150
Total
25,644
4,206
3,663
217
18
262
46
16.031
7,180
5.653
6
3,292
10.360
1,754
9
6,577
13
2.007
727
364
48
316
363
184
179
Corrosive
Waste
D002
20,912
3.375
3,090
73
15
175
22
13,528
5,986
4,773
5
2,764
8.582
1,311
8
5,552
5
1,706
327
280
35
245
36
11
25
Spent
Pickle
Liquor
K062
891
200
24
112
48
17
185
118
33
34
226
180
40
6
301
30
6
24
272
143
129
Total
21,803
3,576
3,114
185
15
223
39
13,714
6.104
4.806
5
2.799
8.809
1.491
8
5.592
11
1.706
618
310
41
269
308
154
154
°1.235 x base data.
"1.05 x base data.
cSource of base data: Reference 1.
"Source of base data: Reference 7.
The aqueous phase will be treated
through wastewater treatment methods
as previously discussed. Sludges con-
taining significant concentrations of toxic
organics (e.g., greater than 20 percent)
must be incinerated or otherwise treated
through processes which will destroy or
detoxify organic compounds; e.g., pyrol-
ysis, and wet air oxidation.13 Solidifica-
tion/encapsulation technologies have
not been adequately developed for
wastes with high organic content such
that land disposal treatment standards
can be achieved.13
Metals containing aqueous wastes
generally undergo precipitation followed
by sludge consolidation. Solidification or
encapsulation of the sludge product will
be required prior to disposal in a secure
landfill if the leachate exceeds EPtoxicity
standards for heavy metals. Unlike
fixation of organics, this technology is
demonstrated and widely available.13
A key consideration in the use of
neutralization technologies is selection
of the most appropriate reagent. Table
4 summarizes the most commonly used
reagents, applicable waste types, resid-
uals generated, and system costs. Neu-
tralization reagents and acid/alkali
waste combination are discussed in more
detail below.
Mutual Neutralization
Acid/alkali mixing (mutual neutraliza-
tion) is often the most economical
method of neutralization available,
particularly m cases where compatible
wastes are present in the same plant.1
The primary advantage of waste combi-
nation is reduced operating costs since
neutralizing reagent requirements are
minimized. The main disadvantage is that
mixing two waste streams, each with its
own variability in composition and flow,
may require more conservative system
design; i.e., larger equalization and
neutralization tanks and back-up neutral-
ization reagent systems. Additionally,
care must be exercised when combining
waste streams or accepting wastes from
another firm to prevent any hazardous
products or releases during the neutral-
ization reaction.
Limestone Neutralization
Limestone treatment is a well-
developed and established technology for
the neutralization of dilute acidic waste
streams. However, limestone (CaCO3) is
limited in its ability to achieve neutral-
ization endpoints over pH 6.0 or to
neutralize wastes with acid conentra-
-------
Table 4. Summary of Neutralization Technologies
Applicable Waste Stage of
Process Streams Development
Acid/ alkali mutual
neutralization
Limestone
Lime
Caustic soda
Suit uric acid
Hydrochloric acid
All acid/ alkali
compatible waste
streams except
cyanide.
Dilute acid waste
streams of less
than 5.000 mg/L
mineral acid
strength and
containing low
concentrations of
acid salts.
All acid wastes.
All acid wastes.
All alkaline wastes
except cyanide.
All acid wastes.
Well developed.
Well developed.
Well developed.
Well developed.
Well developed.
Well developed.
but rarely applied
due to high
reagent cost.
Performance
Generally slower
than comparable
technologies due
to dilute
concentrations of
reagents. May
evolve hazardous
constituents if
incompatible
wastes are mixed.
Requires stone
sizes of 0.074 mm
or less. Requires
45 minutes or
more of retention
time. Can only
neutralize acidic
wastes to pH 6.0.
Must be aerated to
remove evolved
CO*
Requires 15 to 30
minutes of
retention time.
Must be slurried
to a concentration
of 10 to 35%
solids prior to use.
Can under- (below
pH 7) or over-
(above pH 7)
neutralize.
Requires 3 to 15
minutes of
retention time. In
liquid form, easy
to handle and
apply. Can under-
or over- neutralize
including pH 13 or
'higher.
Requires 15 to 30
minutes of
retention time. In
liquid form, but
presents burn
hazard. Highly
reactive and
widely available.
Requires 5 to 20
minutes of
retention time.
Liquid form
presents burn and
fume hazard.
More reactive
than sulfuric.
Residuals
Generated
Variable.
dependent on
quantity of
insolubles and
products
contained in each
waste stream.
Will generate
voluminous sludge
product when
reacted with
sulfate-containing
wastes. Stones
over 200 mesh
will sulfonate. be
rendered inactive.
and add to sludge
product.
Will generate
voluminous sludge
similar to
limestone.
Reaction products
are generally
soluble, however.
sludges do not
dewater as readily
or as easily as
lime or limestone.
Will generate
large quantities of
gypsum sludge
when reacted with
calcium-based
alkaline wastes.
Reaction products
are generally
soluble.
Cost
Least expensive of
all neutralization
technologies.
Most cost-
effective in
treating
concentrated
wastes. May be
cost-effective in
treating dilute
acidic wastes.
More expensive
than crushed
limestone (200
mesh).
Most expensive of
all widely used
alkaline reagents
(five times the cost
of lime).
Least expensive of
all widely used
acidic reagents.
Approximately
twice as expensive
as sulfuric on a
neutralization
equivalent basis.
-------
Table 4.
Continued
Process
Carbonic acids.
liquid carbon
dioxide
Applicable Waste Stage of
Streams Development
All alkaline wastes Emerging
except cyanide. technology.
Performance
Retention time 1
to 1 Viminu1.es. In
liquid form, must
be vaporized prior
to use. Can only
neutralize alkaline
wastes to pH 8.3
end point.
Residuals
Generated
Will form calcium
carbonate
precipitate when
reacted with
calcium-based
alkaline wastes.
Cost
Approximately 3 to
4 times as
expensive as
sulfuric.
Therefore, limited
to applications
using more than
200 tons of
reagents per year
or with flow rate
greater than
1 00.000 gpd.
tions greater than 5,000 mg/L10 The
primary advantage of limestone neutral-
ization is that limestone is a low cost and
widely available reagent. It can be used
in an upflow expanded bed mode or as
a pretreatment in combination with lime.
In the latter case, the pH is raised to
approximately 3.0 to 6.0 with lime
addition completing the process of
neutralization.15 However, in the pres-
ence of concentrated acidic wastes,
limestone particles will become coated
with precipitate, rendering them inactive
and adding to already voluminous sludge
product.
Lime Neutralization
Lime slurry treatment of acidic waste
streams is analogous to that of limestone
in that both are calcium-based rea-
gents.18 Lime (CaO) is typically hydrated
(slaked) and slurried with water to a 10
to 35 percent solids concentration prior
to use.17 Slurried lime (Ca(OH)2) reacts
more rapidly than limestone, typically
requiring only 15 to 30 minutes retention
time versus 45 minutes or more for
limestone. The ability of lime slurry to
treat a wide variety of manufacturing
waste streams has been well demon-
strated in bench, pilot, and full-scale
systems. Lime slurry treatment is more
versatile than limestone since it can
effectively neutralize both dilute and
concentrated acidic waste streams to pH
endpoints ranging from 6.0 to 12.4.
However, when reacted with sulfate-
containing wastes (e.g., sulfuric acid),
lime (and limestone) will form a volumi-
nous calcium sulfate (gypsum) sludge
product.
Sodium Hydroxide
Neutralization
After lime, sodium hydroxide (NaOH)
is the second most widely used alkaline
reagent for the neutralization of both
dilute and concentrated acidic waste
streams. Its chief advantage over lime
slurry neutralization is that as a liquid
reagent, it is easier to store and handle,
will rapidly dissociate into solution, and
has minimal hold-up time.18 As a result,
retention times are typically 5 to 20
minutes19 with a corresponding reduc-
tion in feed system and tankage require-
ments. In addition, sodium hydroxide is
highly caustic (can neutralize to a 14.0
pH endpoint), and as a sodium-based
reagent, it generates reaction products
which are usually soluble.
The main disadvantage of sodium
hydroxide are burn dangers from splash-
ing and a 500 percent increase in reagent
costs on a neutralization equivalent basis
as compared to lime. Thus, in high
volume applications where reagent
expenditures constitute the bulk of
operating expenses, lime is generally the
reagent of choice. In low volume appli-
cations where low space requirements,
soluble end-products, and rapid reaction
rates are important factors in reagent
selection, caustic soda becomes
superior.
Mineral A cid Neutralization
Mineral acid treatment is the most
widely used and demonstrated technol-
ogy for the neutralization of corrosive
alkaline waste streams. Both sulfuric
(H2SCu) and hydrochloric(HCI) acids have
very high dissociation constants, so that
quantities required for neutralization are
relatively low in comparison to other
acids 1 Consequently, reactor volumes
and handling/storage facilities are
smaller. Sulfuric acid, being the most
widely available and lowest in cost on
a neutralization equivalent basis, is the
most prevalent acidic reagent.12 It is
typically used in combination with an
alkali reagent to control pH fluctuations
in both the acidic and alkaline ranges.
Hydrochloric acid is generally used in
situations requiring rapid reaction rates
and soluble reaction products.
The primary disadvantage in the use
of mineral acid reagents is the generation
of potentially hazardous sludge (sulfuric
acid), and acid mist, or toxic/hazardous
fumes (hydrochloric acid). The highly
corrosive nature of mineral acids pres-
ents a burn hazard to personnel, and
increases the likelihood of a possible
catastrophic release during bulk trans-
port or storage.
Carbonic Acid Neutralization
Carbonic acid (H2C03> treatment, using
liquid carbon dioxide as a neutralizing
agent, is a relatively new and emerging
technology. Currently, applications are
limited to waste streams with flow rates
greater than 100,000 gpd or facilities
using more than 200 tons of reagent per
year.12 Since liquid carbon dioxide is
vaporized prior to use and applied as
extremely fine (15 microns or less)
bubbles, capital requirements are min-
imal (e.g., sparger system) and reaction
times are typically only 1 to 11/2 minutes.
However, liquid CC>2 can only neutralize
to a pH 8.3 endpoint.12 In addition, it costs
two to three times as much as sulfuric
acid and will form an insoluble calcium
carbonate precipitate when reacted with
calcium-based alkaline waste streams.
Recovery/Reuse Technologies
As an alternative to conventional
neutralization treatment, recovery/
reuse technologies may be employed.
Certain recovery technologies have been
established as being cost-effective for
specific applications. Additional research
has shown the technical and potential
economical feasibility of a number of
-------
other emerging technologies. With the
implementation of the land disposal ban
and the resulting increases in costs for
sludge disposal, it is anticipated that
recovery/reuse will be cost-effective for
an increasing number of corrosive
wastes.
Crystallization and evaporation/distil-
lation involve the use of temperature
changes to effect a separation of con-
taminants and recovery of corrosive
solutions. Ion exchange methods are
based on the use of an anionic or cationic
selective resin to remove ionic contam-
inants (i.e., metal ions) from corrosive
wastes. Electrodialysis, reverse osmosis,
donnan dialysis, and coupled transport
processes involve the use of a membrane
to separate contaminants from corrosive
solutions. The driving force of the
membrane separation is an electric
current for electrodialysis, hydraulic
pressure (generated by a pump) for
reverse osmosis, and a concentration
gradient (between spent corrosive solu-
tion and a metal stripping solution) for
donnan dialysis and coupled transport.
Solvent extraction uses the differential
distribution of constituents between the
aqueous phase waste and an organic
solvent to separate constituents from a
mixed solution of metal salts and acid
wastes. Thermal decomposition involves
decomposing metal salts, present in
spent acid wastes, in a roaster and
collecting vaporized acid in a condenser.
In general, recovery/reuse process
selection will be limited to wastes
possessing specific chemical, physical,
and flow characteristics. A summary of
the overall performance, applicable
waste streams, residuals generation, and
status ot development for the corrosive
recovery/reuse technologies is provided
in Table 5. A brief description of these
processes and their current status is
presented below.
Evaporation/Distillation
Evaporation/distillation techniques
can be used to recover a variety of plating
and other process chemicals. They are
most commonly used in metal finishing
and electroplating industries to recovery
plating solutions, chromic acid and other
concentrated acids, and metal cyanides
by evaporating water from the dilute
rinse solution and concentrating the
corrosive solution for return to the
concentrated bath.1'20'21 Water recovered
from the distillation (condensation)
process is of high purity and can be
reused in process waters.
Evaporation systems used to recover
corrosive plating rinses are cost-
competitive with conventional neutrali-
zation and disposal technologies. Greater
cost savings are realized with larger
operations. However, the use of evapo-
ration/distillation systems to recovery
concentrated streams directly from the
spent bath solution is limited. Pilot-scale
evaporation/distillation systems for
recovery of nitric/hydrofluoric acid
pickling liquors have been tested at
facilities in Europe.22'23 However, cost-
effective systems for direct recovery of
spent solutions via evaporation/distilla-
tion have not been developed at the
commercial-scale for application in the
United States.
Crystallization
Crystallization is a recovery technique
whereby metal contaminants in a spent
corrosive solution are crystallized and
removed by settling or centrifugation. It
is a demonstrated and commercially
available technology for the recovery of
acid pickling liquors and caustic etching
solutions.24'25'2*27
The use of crystallization techniques
for the recovery of sulfuric acid pickling
liquors and caustic aluminum etching
solutions is limited by economics. This
is due to the small quantities of these
solutions used by individual manufactur-
ers, the costs for plant modifications, and
the varying demand for the crystal
product.1'28 Nitric-hydrofluoric acid pic-
kling liquors are used in larger quantities
by individual manufacturers in the steel
industry than sulfuric acid pickling
liquors. Therefore, crystallization tech-
niques would have wider application for
this waste type. Despite these limita-
tions, these processes are currently
being used in the metal finishing industry
in specialized applications.
Ion Exchange
Ion exchange has been used to recover
acids, bases, and process wastes from
the metal finishing, electroplating, and
fertilizer manufacturing industries by
removing metal contaminants and rec-
ycling the treated solution.1'29 Ion
exchange techniques involve the use of
an anionic or cationic selective resin to
remove ionic contaminants (i.e., metals)
from solution. Three types of ion
exchange configurations can be used:
cocurrent, countercurrent (reverse flow)
fixed bed, and countercurrent (reverse
flow) continuous.
Cocurrent ion exchange systems are
generally not employed for direct treat-
ment of corrosive wastes. Cocurrent
systems using weak exchangers have
inefficient exchange capacities in the
corrosive pH ranges. Thus, they are
generally used as polishing systems
following other treatment operations.
Corrosive systems using strong
exchangers are not cost effective
because of the high costs for column
regeneration. However, reciprocating
flow ion exchange (RFIE) systems have
been shown to be effective in the
treatment of corrosive wastes. These
may be more cost-effective for the
treatment of corrosives than conven-
tional neutralization, particularly when
enactment of land disposal restrictions
increase costs associated with land
disposal of residuals.
Chemical recovery systems using fixed
bed RFIE have been used to recover
chromic acid and metal salts, and to
deionize mixed-metal rinse solutions for
recovering process water and concen-
trating the metals for subsequent treat-
ment. °'31 Commercial units are available
from several vendors.
Acid purification systems using con-
tinuous RFIE have been used to remove
aluminum salts from sulfuric acid anod-
izing solutions, to remove metals from
nitric acid rack-stripping solutions, and
to remove metals from sulfuric and
hydrochloric acid pickling solutions.30
Acid purification systems are most cost-
effective for removing high concentra-
tions of contaminants relative to other
ion exchange systems.
Electrodialysis
Electrodialysis (ED) uses an electric
field and a semipermeable ion-selective
membrane to concentrate or separate
ionic species in a water solution.32'33 Its
primary application in the treatment of
corrosive wastes is recovery of corrosive
plating solutions, pickling solutions, and
etchants by removing contaminant metal
ions. Three types of configurations may
be used in the design of ED units:
concentrating-diluting, ion-substituting,
and electrolytic.
Currently, electrodialysis has a limited
area of application in the recovery/reuse
of corrosive wastes. Concentrating-
diluting and ion transfer ED units have
been successful in the recovery of
chromic acids from dilute solutions.34'35
Electrolytic ED units have demonstrated
the ability to recover concentrated acid
solutions by removing metal ion contam-
8
-------
Table 5. Summary of Recovery/ Reuse Technologies for Corrosive Wastes
Applicable Waste Stage of
Process Streams Development Performance
Evaporation/
distillation
Crystallization
Ion exchange
Electrodialysis
Metal plating
rinses; acid
pickling liquors
HiSOt pickling
liquors; HNOa/HF
pickling liquors;
caustic aluminum
etch solutions.
Plating rinses;
acid pickling
baths; aluminum
etching solutions;
HiSOt anodizing
solutions; rack-
stripping solutions
(HF/HNOsl.
Recovery of
chromic/ sulf uric
acid etching
solutions.
Recovery of
plating rinses
(particularly
chromic acid rinse
water).
Recovery ofHNOs/
HF pickling
liquors.
Well-established
for treating plating
rinses.
20 to 25 systems
currently in
operation (fewer
applications for
caustic recovery).
Several RFIE units
in operation for
treatment of
corrosives.
Units for direct
treatment of acid
bath only available
fromECO-TEC,
Ltd.
Units currently
being sold, but
limited area of
application.
5 in operation.
Several in
operation.
Marketed, none in
operation to date.
Plating solution
recovered for
reuse in plating
bath. Rinse water
can be reused.
97-98% recovery
f or HsSOt (80-85%
metal removal)
99% HN03 and
50% HF recovered.
80% recovery of
NaOH
Cocurrent systems
not technically
feasible for direct
treatment of
corrosives, can be
used in
conjunction with
neutralization
technologies to
lower overall
costs
RFIE units show
good results.
Conventional RFIE
performs best with
dilute solutions
APU performs best
with high metal
concentration (30
to 100g/L)
85% recovery of
etching solution.
45% copper
removal.
30% zinc removal
Works best when
copper
concentrations are
in the 2 to 4 oz/
gal usage.
3 M HF/HN03
recorded.
Residuals
Generated
Impurities will be
concentrated.
therefore.
crystallization/
filtration system
may be required
Ferrous sulf ate
heptahydeate
crystals lean be
traded or sold).
Metal fluoride
crystals (can
recover additional
HF by thermal
decomposition)
Aluminum
hydroxide crystals
(can be traded or
sold).
Cocurrent process
generates spent
regenerant, which
is also corrosive
Recovered metals
which can be
reused, treated.
disposed, or
marketed
Metals which can
be treated.
disposed, or
regenerated for
reuse
Chromic acid can
be returned to
plating bath, rinse
water can be
reused.
2 M KOH Soln
which can be
recycled back to
the pretreatment
step for this ED
application.
Cost
Can be cost-
effective for
recovering
corrosive plating
solutions from
rinse waters
Cost-effective if
treating large
quantities of
waste
RFIE and APU are
cost-effective.
Cost-effective for
specific
applications
(chromic/ sulf ate
acid etchantsl
Low capital
investment; cost-
effective for
specific
application
(chromic acid
rinses)
Cost-effective for
large quantity
generator.
-------
Table 5. (Continued)
Applicable Waste
Process Streams
Reverse osmosis Plating rinses.
Donnan dialysis/ Plating rinses;
coupled transport potentially
applicable to acid
baths.
Solvent extraction HN03 /HF pickling
liquors.
Thermal Acid wastes.
decomposition
Stage of
Development
Corrosive waste
membranes
marketed by four
companies. RD
module systems
applicable to
corrosives
available from two
companies.
Donnan analysis
only lab-scale
tested.
Coupled transport
lab and field
tested. Coupled
transport system
is currently being
marketed.
Commercial-scale
systems installed
for development
purposes in
Europe and Japan.
No commercial-
scale installations
in U.S.
Well-establshed
for recovering
spent pickle
liquors generated
by steel industry.
Pilot-scale stage
for organic
wastes.
Performance
90% conversion
achieved with
cyanide plating
rinses.
Data not available
for Donnan
analysis (further
testing required).
Coupled transport
has demonstrated
99% recovery of
chromate from
plating rinses.
Other plating
rinses should be
applicable, but not
fully tested.
95% recovery of
HNO3;70%
recovery of HF.
99% regeneration
efficiency for
pickling liquors.
Residuals
Generated
Recovered plating
solution returned
to plating bath
(after being
concentrated by
an evaporator).
Rinsewater
reused.
Data not available
for Donnan
analysis.
For chromate
plating rinse
applications.
sodium chromate
is generated; can
be used elsewhere
in plant or
subjected to ion
exchange to
recover chromic
acid for recycle to
plating solution.
Metal sludge (95%
iron can be
recovered by
thermal
decomposition).
98-99% purity iron
oxide which can
be reused, traded.
or marketed.
Cost
Cost-effective for
limited
applications.
Development of a
more chemically
resistant
membrane would
make it very cost-
effective for a
wider area of
application.
No cost data
available for
Donnan analysis.
Average capital
cost for plating
shop is $20,000.
Can be cost-
effective for
specific
applications.
Not available.
Expensive capital
investment. Only
cost-effective for
large quantity
waste acid
generators.
inants; e.g., removing copper ions from
spent chromic acid/sulfuric acid brass
etchants and bright dipping solutions.36
Another recently developed application
uses electrodialysis in conjunction with
neutralization to recover spent
hydrofluoric-nitric acid pickling
liquors.37'38
Current research in the application of
electrodialysis to the treatment of cor-
rosive wastes is directed at using the
electrolytic ED configuration. The U.S.
Bureau of Mines is currently investigat-
ing techniques for the removal of iron
from nitric-hydrofluoric acid pickling
liquors.39'40 In addition, Ionics, Inc. is
currently developing improved ED mem-
branes for use with corrosive wastes.
However, their research is currently
limited to bench-scale studies and
preliminary results have not yet been
released.41
Reverse Osmosis
RO involves passing the wastewater
through a semipermeable membrane at
a pressure greater than the osmotic
pressure caused by the dissolved mate-
rials in the solvent.42 Thus, the osmotic
flow, defined as the flow from a concen-
trated solution to a dilute solution, is
reversed due to the increase in pressure
applied to the system. The technology
has been applied in the metal finishing
industry to recover plating chemicals
from rinsewater, permitting reuse of both
plating chemicals arid rinsewaters.29'43
Reverse osmosis systems are currently
available for recovering corrosive waste-
water streams; e.g., plating rinses.
However, cost-effective use of RO sys-
tems for corrosive waste applications is
generally limited due to reduced mem-
brane lifetime and high costs for mem-
brane cleaning and replacement. How-
ever, future development of membranes
which are able to withstand corrosive
10
-------
and oxidizing solutions is expected.32
If membrane lifetimes are increased,
reverse osmosis would be a very cost-
effective alternative to conventional
treatment technologies. Excluding mem-
brane cleaning and replacement costs,
the only significant operating cost is the
electricity required for operation of the
pump. However, current systems are
limited in the degree of attainable
concentration in the recovered corrosive
solution. Thus, many applications may
also require the use of an evaporator in
conjunction with the RO unit. This
combined system is generally more cost-
effective than evaporation alone for
dilute solutions.
Donnan Dialysis and Coupled
Transport
Donnan dialysis and coupled transport
are similar processes in that both employ
a concentration gradient to drive ions
from a spent solution across a membrane
into a metal stripping solution. The major
difference between these processes is
the type of membrane and transport
mechanism employed. The coupled
transport membrane is highly selective
and, therefore, has more specific process
applications, whereas the donnan dial-
ysis membrane is applicable to a wider
variety of solution constituents. How-
ever, greater purity can be achieved
using the coupled transport membrane.
Donnan dialysis has not been tested
on a pilot-scale. Much of the research
that has been performed to date has
concentrated on membrane develop-
ment.44 However, preliminary research
performed by the Southwest Research
Institute has encouraged them to develop
a pilot-scale unit.45 Pilot-scale testing is
needed to determine if sufficient solution
concentrations can be achieved with the
process.
Bend Research Corporation has per-
formed most of the development work for
coupled transport technology and has a
patent pending on the process.46
Although the process is applicable to the
treatment of several metal-containing
solutions, the most developed application
is for the treatment of hexavalent chro-
mium in plating rinses. The process was
recently licensed to Concept Membrane,
Inc. for marketing and sales purposes.
However, commercial units are not
currently available for purchase.46
Both membrane technologies show
good potential as cost-effective alterna-
tives to conventional neutralization and
disposal practices. In addition, donnan
dialysis and coupled transport offer
potential economic advantages over
other membrane technologies, due to
lower energy requirements. The large
hydraulic pressures required for reverse
osmosis and the large electric current
flow required by electrodialysis are not
required for these technologies.44'46
Solvent Extract/on
Solvent extraction is a separation
technique utilizing the differential distri-
bution of constituents between the
aqueous phase and an organic solvent
phase to separate constituents from a
mixed solution. It is widely used as an
analytical chemistry technique and for
the recovery of metals in the field of
hydrometallurgy. Recently, research has
also shown applications for solvent
extraction in the recovery of spent nitric-
hydrofluoric acid pickling liquors gener-
ated by the steel industry. Commercial-
scale systems have been tested in both
Sweden and Japan but none have yet
been employed in the United States.47'48
Of the four solvent extraction pro-
cesses developed for acid waste recov-
ery, the Kawasaki (or Solex) process has
shown the most promising results.
Commercial-scale testing of the Kawa-
saki process has demonstrated 95 per-
cent recovery of nitric acid and 70
percent recovery of hydrofluoric acid.48
In addition, 95 percent of the iron in the
waste solution was recovered for
reuse.48 Kawasaki intends to eventually
market the process.48 However, although
the technology has been demonstrated
to be technically feasible, limited eco-
nomic data are available to assess its
economic viability.
Thermal Decomposition
Thermal decomposition is an effective
but capital intensive regeneration pro-
cess which has been used to recover both
free and bound acids from wastes. The
process involves precipitating and
decomposing metal salts in a roaster, and
collecting the vaporized acid in a con-
densor. Several steel manufacturers use
the thermal decomposition process for
the recovery of hydrochloric acid from
spent pickling liquors. Although there are
currently no other commercial-scale
applications, research has demonstrated
the technical feasibility of using thermal
decomposition to regenerate waste
sulfuric acid effluents from spent pickling
liquors and organic chemical industry
corrosive wastes.
The thermal decomposition process
has the advantage of being able to
recover bound, as well as free acid from
waste, which distinguishes it from the
previously mentioned recovery technol-
ogies. More than 99 percent of the
hydrochloric acid equivalents in waste
pickle liquor can be regenerated, and an
estimated 93 to 96 percent of sulfuric
acid equivalents can potentially be
regenerated by thermal decom-
position.28'49
However, capital costs for thermal
decomposition will be prohibitive for
small volume generators. Although the
total quantity of waste sulfuric acid
generated by the steel industry is greater
than the amount of hydrochloric acid
generated, the latter is generated by a
small number of large quantity genera-
tors. Combined with the higher purchase
price of hydrochloric acid, HCI regener-
ation systems may be more economically
viable than sulfuric acid regeneration
systems in the steel industry. However,
large quantities of waste sulfuric acid are
generated by individual organic chemical
manufacturing plants and, therefore,
acid regeneration may have a wider
application for this industry. With
increasing costs for disposal, and
increasing development of the technol-
ogy for other waste types, thermal
regeneration systems are likely to find
wider application in corrosive waste
treatment.
Selection of Optimal Waste
Management Alternative
Waste management options have been
summarized previously in Table 1. These
include source reduction, recycling, use
of a neutralization treatment system or
some combination of these waste han-
dling practices. Selection of the optimal
management alternative will ultimately
be a function of regulatory compliance,
economics, and availability of onsite and
offsite processing systems and equip-
ment. Economic considerations include
processing (including pretreatment and
post-treatment) and disposal costs, value
of recovered products, and potential
adverse effects on product quality or
process equipment resulting from waste
minimization or reuse of recovered
products. Additional consideration in
system selection must be given to factors
such as safety, public and employee
acceptance, liability, and degree of
11
-------
uncertainty in cost estimates and ability
to meet treatment objectives.
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39. Horter, G. L. U.S. Bureau of Mines,
Rolla, Missouri. Telephone conver-
sation with L. Wilk, GCA Technol-
ogy Division, Inc. August 29,1986.
40. Horter, G. L., J. B. Stephenson, and
W. M. Dressel. Permselective
Membrane Research for Stainless
Steel Pickle Liquors. In: Proceed-
ings of the International Sympo-
sium on Recycle and Secondary
Recovery of Metals; sponsored by
the metallurgical Society of AIME,
Warrendale, Pennsylvania; held in
FortLauderdale, Florida. December
1-4,1985.
41. Jain, S. M. Ionics, Inc. Telephone
conversation with J. Spielman,
GCA Technology Division, Inc.
August 12, 1986.
42. U.S. EPA. Sources and Treatment
of Wastewater in the Nonferrous
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EPA, Industrial Environmental
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02-2068. EPA/600/2-80/074.
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43. U.S. EPA, Office of Research and
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44. Hamil, H. F. Southwest Research
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Donnan Dialyzer for the Removal
of Toxic Metals from Electroplating
Rinse Waters. EPA/600/S2-85/
080. August 1985.
47. Rydberg, J., H. Reinhardt, B.
Lunden, and P. Haglund. Recovery
of Metals from Stainless Steel
Pickling Bath. In: Proceedings of
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48. Watanabe, T., M. Hoshimo, K.
Uchimo, and Y. Nakazato. A New
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36. Gary, S. Scientific Control, Inc.,
Chicago, Illinois. Telephone
conversation with L. Wilk, GCA
Technology Division, Inc. August
29, 1986.
37. Rodgers, B. Aquatech Systems,
Bethel, New Jersey. Telephone
conversation with J. Spielman,
GCA Technology Division, Inc.,
August 11, 1986.
45. Hamil, H. F. Southwest Research
Institute, San Antonio, Texas.
Telephone conversation with L.
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inc. September 24, 1986.
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13
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Lisa Wilk. Stephen Palmer, and Marc Breton are with Alliance Technologies
Corporation, Bedford, MA 01730.
Harry M. Freeman is the EPA Project Officer (see below).
The complete report, entitled "Technical Resource Document: Treatment
Technologies for Corrosive-Containing Wastes, Volume II," (Order No. PB
88-131 289/AS; Cost: $38.95) will be available only from:
National Technical Information Service
5285 Port Royal Road
Springfield, VA 22161
Telephone: 703-487-4650
The EPA Project Officer can be contacted at:
Hazardous Waste Engineering Research Laboratory
U.S. Environmental Protection Agency
Cincinnati, OH 45268
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