xvEPA
United States
Environmental Protection
Agency
Office of
Solid Waste
Washington, D C 20460
EPA/530-SW-88-0009-g
April 1988
Solid Waste
Best
Demonstrated
Available Technology
(BOAT) Background
Document for
Aniline Production
Treatability Group
(K103, K104)
Proposed
Volume 7
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"*-.,
;1
X FINAL
BEST DEMONSTRATED AVAILABLE TECHNOLOGY (BOAT)
BACKGROUND DOCUMENT FOR K103 AND K104
Volume 7
U. S. Environmental Protection Agency
Office of Solid Waste
401 M Street, S.W.
Washington, D.C. 20460
James R. Berlow, Chief
Treatment Technology Section
April 1988
U.S. Environmental Protection Agency
Keg'on 5, Library (PL-12J)
ff West Jackson Boulevard 12th Floor
<-h
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BOAT BACKGROUND DOCUMENT FOR K103 and K104
TABLE OF CONTENTS
VOLUME 7 Page
Executive Summary i
BOAT Treatment Standards for K103 and K104 vii
SECTION 1. Introduction 1-1
SECTION 2. Industries Affected and Waste
Characterization 2-1
SECTION 3. Demonstrated/Applicable Treatment
Technologies 3-1
SECTION 4. Selection of BOAT 4-1
SECTION 5. Determination of Regulated Constituents . . . 5-1
SECTION 6. Calculation of Treatment Standard 6-1
SECTION 7. Conclusions 7-1
APPENDIX A Statistical Analysis A-l
APPENDIX B Analysis of Variance Tests B-l
APPENDIX C Detection Limits for Constituents in the
Untreated and Treated Waste C-l
APPENDIX D Calculation of Treatment Standards D-l
APPENDIX E Analytical QA/QC E-l
APPENDIX F Thermal Conductivity Summary F-l
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EXECUTIVE SUMMARY
BDAT Treatment Standards for K103 and K104
Pursuant to the Hazardous and Solid Waste Amendments (HSWA)
enacted on November 8, 1984, and in accordance with the
procedures for establishing treatment standards under section
3004 (m) of the Resource Conservation and Recovery Act (RCRA),
the Environmental Protection Agency (EPA) is proposing treatment
standards for the listed wastes, K103 and K104, based on the
performance of treatment technologies determined by the Agency to
represent Best Demonstrated Available Technology (BDAT). This
background document provides the detailed analyses that support
this determination.
These BDAT treatment standards represent maximum acceptable
concentration levels for selected hazardous constituents in the
wastes or residuals from treatment and/or recycling. These
levels are established as a prerequisite for disposal of these
wastes in units designated as land disposal units according to 40
CFR 268 (Code of Federal Regulations). Wastes which, as
generated, contain the regulated constituents at concentrations
which do not exceed the treatment standards are not restricted
from land disposal units. The Agency has chosen to set levels
for these wastes rather than designating the use of a specific
treatment technology. The Agency believes that this allows the
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generators of these wastes a greater degree of flexibility in
selecting a technology or train of technologies that can achieve
these levels. These standards become effective as of August 8,
1988, as described in the schedule set forth in 40 CFR 268.10.
According to 40 CFR 261.32 (hazardous wastes from specific
sources) waste codes K103 and K104 are from the
nitrobenzene/aniline industry and are listed as follows:
K103: Process residues from aniline extraction from the
production of aniline.
K104: Combined wastewater streams generated from
nitrobenzene/aniline production.
Descriptions of the industry and specific processes
generating these wastes, as well as descriptions of the physical
and chemical waste characteristics, are provided in Section 2.0
of this document. The four digit Standard Industrial
Classification (SIC) code most often reported for the industry
generating this waste code is 2869 (nitrobenzene/aniline). The
Agency estimates that there are six facilities that may
potentially generate wastes identified as K103-K104.
The Agency has determined that K103/K104 collectively
represent one general treatability group with two subgroups -
wastewaters and nonwastewaters. For the purpose of the land
disposal restrictions rule, wastewaters are defined as wastes
containing less than 1% (weight basis) filterable solids and less
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than 1% (weight basis) total organic carbon (TOC). For K103 and
K104 wastes, this definition was amended to include wastewaters
with a TOC content up to 4% (weight basis). Wastes not meeting
this definition are classified as nonwastewaters.
These treatability subgroups represent classes of wastes
that have similar physical and chemical properties within each
subgroup. EPA believes that each waste within these subgroups
can be treated to the same concentrations when similar
technologies are applied. The Agency has examined the sources of
these two wastes from the nitrobenzene/aniline industry, the
specific similarities in waste composition, potential applicable
and demonstrated technologies, and attainable treatment
performance in order to support a simplified regulatory approach.
While the Agency has not, at this time, specifically identified
additional wastes which would fall into this treatability group
or two subgroups, this does not preclude the Agency from
extrapolating these standards to other wastes, in the future.
The K103 and K104 wastes, as generated, have a high water
content and are typically classified as wastewaters. Residues
from the treatment of these wastewaters (such as spent carbon and
the nitrobenzene solvent stream from the nitrobenzene
V
liquid/liquid extractor) are classified as nonwastewaters. The
K103/K104 nonwastewaters are generated primarily as a result of
the "derived-from rule" and the "mixture-rule" as outlined in 40
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CFR 261.3 (definition of hazardous waste).
The Agency has proposed BOAT treatment standards for the two
treatability subgroups of the K103 and K104 wastes - wastewaters
and nonwastewaters. In general, these treatment standards have
been proposed for a total of five (5) organic constituents. In
addition, a treatment standard has been proposed for one (1)
inorganic constituent in K104. The organic constituents that are
proposed for regulation in K103 and K104 wastes codes are as
follows: benzene, aniline, 2,4-dinitrophenol, nitrobenzene, and
phenol. Total cyanides were also proposed for regulation in
K104. Sulfide was not proposed for regulation in K103 because
the Agency requires additional analytical data on sulfide to
determine if it was effectively treated by the treatment system.
A detailed discussion of the selection of constituents to be
regulated is presented in Section 5.0 of this document.
BDAT treatment standards for wastewater K103 and K104 are
proposed based on performance data from a treatment train which
consisted of liquid/liquid extraction followed by steam stripping
and activated carbon adsorption. Testing was performed on
representative samples of K103 and K104. Liquid/liquid
extraction followed by steam stripping and activated carbon
v-
adsorption was determined to represent the best demonstrated
available technology (BDAT). This determination was based on a
statistical comparison of performance data. The Agency collected
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performance data for a treatment train consisting of
liquid/liquid extraction followed by steam stripping and carbon
adsorption. A statistical comparison was done with this
performance data from liquid/liquid extraction followed by steam
stripping and from liquid/liquid extraction alone. Based on this
analysis, the Agency has determined that the data for
liquid/liquid extraction followed by steam stripping and
activated carbon adsorption indicated the highest level of
performance.
BOAT treatment standards for K103 and K104 nonwastewaters
are proposed based on a transfer of treatment standards developed
for K048/K051 nonwastewaters (dissolved air flotation float and
API separator sludge from the petroleum industry). These
standards were developed based on the incineration of K048/K051
nonwastewaters. Treatment data were transferred on a constituent
basis from either the same constituent or from constituents
judged to be similar in physical and chemical properties. A
detailed discussion of the transfer of the data and methodology
is presented in Section 6.0 of this document.
The following tables list the specific BOAT treatment
standards for wastes identified as K103 and K104. The Agency is
setting standards based on analyses of total composition for both
wastewater and nonwastewater forms of K103 and K104. The units
for total composition analysis are in parts per million (mg/kg)
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on a weight by weight basis for nonwastewaters. For wastewaters
the units are expressed on a weight per unit volume basis (mg/1).
Testing procedures are specifically identified in the quality
assurance sections of this document.
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BOAT TREATMENT STANDARDS FOR K103/K104 WASTES
WASTEWATER
Regulated Constituents
Total Composition (mg/1)
K103 K104
Benzene
Aniline
2 , 4-Dinitrophenol
Nitrobenzene
Phenol
Total Cyanides (CN)
0.147
4.450
0.613
0.073
1.391
NR
0.147
4.450
0.613
0.073
1.391
2.683
NR = Not regulated since it is not presented at treatable levels.
NONWASTEWATER
(Nonwastewater forms of K103/K104 represent spent
carbon from the activated carbon adsorber. Treatment
standards were transferred from K019 for benzene,
aniline, 2,4-dinitrophenol, nitrobenzene, and phenol
and from K048/K051 for total cyanides).
Regulated Constituents
Total Composition (mq/kg)
K103 K10'
Benzene
Aniline
2 , 4-Dinitrophenol
Nitrobenzene
Phenol
Total Cyanides (CN)
5.96
5.44
5.44
5.44
5.44
NR
5.96
5.44
5.44
5.44
5.44
1.48
NR = Not regulated since it is not present at treatable levels.
VII
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1. INTRODUCTION
This section of the background document presents a summary
of the legal authority pursuant to which the BDAT treatment
standards were developed, a summary of EPA's promulgated
methodology for developing BOAT, and finally a discussion of the
petition process that should be followed to request a variance
from the BDAT treatment standards.
1.1 Legal Background
1.1.1 Requirements Under HSWA
The Hazardous and Solid Waste Amendments of 1984 (HSWA),
enacted on November 8, 1984, and which amended the Resource
Conservation and Recovery Act of 1976 (RCRA), impose substantial
new responsibilities on those who handle hazardous waste. In
particular, the amendments require the Agency to promulgate
regulations that restrict the land disposal of untreated
hazardous wastes. In its enactment of HSWA, Congress stated
explicitly that "reliance on land disposal should be minimized or
eliminated, and land disposal, particularly landfill and surface
impoundment, should be the least favored method for managing
hazardous wastes" (RCRA section 1002(b)(7), 42 U.S.C.
6901(b)(7)).
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One part of the amendments specifies dates on which
particular groups of untreated hazardous wastes will be
prohibited from land disposal unless "it has been demonstrated to
the Administrator, to a reasonable degree of certainty, that
there will be no migration of hazardous constituents from the
disposal unit or injection zone for as long as the wastes remain
hazardous" (RCRA section 3004(d)(1), (e)(1), (g)(5), 42 U.S.C.
6924 (d)(l), (e)(1), (g)(5)).
For the purpose of the restrictions, HSWA defines land
disposal "to include, but not be limited to, any placement of ...
hazardous waste in a landfill, surface impoundment, waste pile,
injection well, land treatment facility, salt dome formation,
salt bed formation, or underground mine or cave" (RCRA section
3004(k), 42 U.S.C. 6924(k)). Although HSWA defines land disposal
to include injection wells, such disposal of solvents, dioxins,
and certain other wastes, known as the California List wastes, is
covered on a separate schedule (RCRA section 3004(f)(2), 42
U.S.C. 6924 (f)(2)). This schedule requires that EPA develop
land disposal restrictions for deep well injection by
August 8, 1988.
The amendments also require the Agency to set "levels or
methods of treatment, if any, which substantially diminish the
toxicity of the waste or substantially reduce the likelihood of
migration of hazardous constituents from the waste so that
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short-term and long-term threats to human health and the
environment are minimized" (RCRA section 3004(m)(l), 42 U.S.C.
6924 (m)(l)). Wastes that meet treatment standards established
by EPA are not prohibited and may be land disposed. In setting
treatment standards for listed or characteristic wastes, EPA may
establish different standards for particular wastes within a
single waste code with differing treatability characteristics.
One such characteristic is the physical form of the waste. This
frequently leads to different standards for wastewaters and
nonwastewaters.
Alternatively, EPA can establish a treatment standard that
is applicable to more than one waste code when, in EPA's
judgment, all the waste can be treated to the same concentration.
In those instances where a generator can demonstrate that the
standard promulgated for the generator's waste cannot be
achieved, the Agency also can grant a variance from a treatment
standard by revising the treatment standard for that particular
waste through rulemaking procedures. (A further discussion of
treatment variances is provided in Section 1.3.)
The land disposal restrictions are effective when
promulgated unless the Administrator grants a national variance
and establishes a different date (not to exceed 2 years beyond
the statutory deadline) based on "the earliest date on which
adequate alternative treatment, recovery, or disposal capacity
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which protects human health and the environment will be
available" (RCRA section 3004(h)(2), 42 U.S.C. 6924 (h)(2)).
If EPA fails to set a treatment standard by the statutory
deadline for any hazardous waste in the First Third or Second
Third of the schedule (see section 1.1.2), the waste may not be
disposed in a landfill or surface impoundment unless the facility
is in compliance with the minimum technological requirements
specified in section 3004(o) of RCRA. In addition, prior to
disposal, the generator must certify to the Administrator that
the availability of treatment capacity has been investigated and
it has been determined that disposal in a landfill or surface
impoundment is the only practical alternative to treatment
currently available to the generator. This restriction on the
use of landfills and surface impoundments applies until EPA sets
a treatment standard for the waste or until May 8, 1990,
whichever is sooner. If the Agency fails to set a treatment
standard for any ranked hazardous waste by May 8, 1990, the waste
is automatically prohibited from land disposal unless the waste
is placed in a land disposal unit that is the subject of a
successful "no migration" demonstration (RCRA section 3004(g), 42
U.S.C. 6924(g)). "No migration" demonstrations are based on
case-specific petitions that show there will be no migration of
hazardous constituents from the unit for as long as the waste
remains hazardous.
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1.1.2 Schedule for Developing Restrictions
Under Section 3004(g) of RCRA, EPA was required to establish
a schedule for developing treatment standards for all wastes that
the Agency had listed as hazardous by November 8, 1984.
Section 3004(g) required that this schedule consider the
intrinsic hazards and volumes associated with each of these
wastes. The statute required EPA to set treatment standards
according to the following schedule:
(a) Solvents and dioxins standards must be promulgated by
November 8, 1986;
(b) The "California List" must be promulgated by July 8,
1987;
(c) At least one-third of all listed hazardous wastes must
be promulgated by August 8, 1988 (First Third);
(d) At least two-thirds of all listed hazardous wastes aust
be promulgated by June 8, 1989 (Second Third); and
(e) All remaining listed hazardous wastes and all hazardous
wastes identified as of November 8, 1984, by one or
more of the characteristics defined in 40 CFR Part 261
must be promulgated by May 8, 1990 (Third Third).
The statute specifically identified the solvent wastes as
those covered under waste codes F001, F002, F003, F004, and F005;
it identified the dioxin-containing hazardous wastes as those
covered under waste codes F020, F021, F022, and F023.
Wastes collectively known as the California List wastes,
defined under Section 3004(d) of HSWA, are liquid hazardous
wastes containing metals, free cyanides, PCBs, corrosives (i.e.,
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a pH less than or equal to 2.0), and any liquid or nonliquid
hazardous waste containing halogenated organic compounds (HOCs)
above 0.1 percent by weight. Rules for the California List were
proposed on December 11, 1986, and final rules for PCBs,
corrosives, and HOC-containing wastes were established
August 12, 1987. In that rule, EPA elected not to establish
standards for metals. Therefore, the statutory limits became
effective.
On May 28, 1986, EPA published a final rule (51 FR 19300)
that delineated the specific waste codes that would be addressed
by the First Third, Second Third, and Third Third. This schedule
is incorporated into 40 CFR 268.10, .11, and .12.
1.2 Summary of Promulgated BOAT Methodology
In a November 7, 1986, rulemaking, EPA promulgated a
technology-based approach to establishing treatment standards
under section 3004(m). Section 3004(m) also specifies that
treatment standards must "minimize" long- and short-term threats
to human health and the environment arising from land disposal of
hazardous wastes.
Congress indicated in the legislative history accompanying
the HSWA that "[t]he requisite levels of [sic] methods of
treatment established by the Agency should be the best that has
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been demonstrated to be achievable," noting that the intent is
"to require utilization of available technology" and not a
"process which contemplates technology-forcing standards" (Vol.
130 Cong. Rec. S9178 (daily ed., July 25, 1984)). EPA has
interpreted this legislative history as suggesting that Congress
considered the requirement under 3004(m) to be met by application
of the best demonstrated and achievable (i.e., available)
technology prior to land disposal of wastes or treatment
residuals. Accordingly, EPA's treatment standards are generally
based on the performance of the best demonstrated available
technology (BOAT) identified for treatment of the hazardous
constituents. This approach involves the identification of
potential treatment systems, the determination of whether they
are demonstrated and available, and the collection of treatment
data from well-designed and well-operated systems.
The treatment standards, according to the statute, can
represent levels or methods of treatment, if any, that
substantially diminish the toxicity of the waste or substantially
reduce the likelihood of migration of hazardous constituents.
Wherever possible, the Agency prefers to establish BDAT treatment
standards as "levels" of treatment (i.e., performance standards)
rather than adopting an approach that would require the use of
*•
specific treatment "methods." EPA believes that
concentration-based treatment levels offer the regulated
community greater flexibility to develop and implement compliance
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strategies as well as an incentive to develop innovative
technologies.
1.2.1 Waste Treatability Group
In developing the treatment standards, EPA first
characterizes the waste(s). As necessary, EPA may establish
treatability groups for wastes having similar physical and
chemical properties. That is, if EPA believes that wastes
represented by different waste codes could be treated to similar
concentrations using identical technologies, the Agency combines
the codes into one treatability group. EPA generally considers
wastes to be similar when they are both generated from the same
industry and from similar processing stages. In addition, EPA
may combine two or more separate wastes into the same
treatability group when data are available showing that the waste
characteristics affecting performance are similar or that one
waste would be expected to be less difficult to treat.
Once the treatability groups have been established, EPA
collects and analyzes data on identified technologies used to
treat the wastes in each treatability group. The technologies
evaluated must be demonstrated on the waste or a similar waste
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and must be available for use.
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1.2.2 Demonstrated and Available Treatment Technologies
Consistent with legislative history, EPA considers
demonstrated technologies to be those that are used to treat the
waste of interest or a similar waste with regard to parameters
that affect treatment selection (see November 7, 1986, 51 FR
40588). EPA also will consider as treatment those technologies
used to separate or otherwise process chemicals and other
materials. Some of these technologies clearly are applicable to
waste treatment, since the wastes are similar to raw materials
processed in industrial applications.
For most of the waste treatability groups for which EPA will
promulgate treatment standards, EPA will identify demonstrated
technologies either through review of literature related to
current waste treatment practices or on the basis of information
provided by specific facilities currently treating the waste or
similar wastes.
In cases where the Agency does not identify any facilities
treating wastes represented by a particular waste treatability
group, EPA may transfer a finding of demonstrated treatment. To
do this, EPA will compare the parameters affecting treatment
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selection for the waste treatability group of interest to other
wastes for which demonstrated technologies already have been
determined. The parameters affecting treatment selection and
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their use for this waste are described in Section 3.2 of this
document. If the parameters affecting treatment selection are
similar, then the Agency will consider the treatment technology
also to be demonstrated for the waste of interest. For example,
EPA considers rotary kiln incineration a demonstrated technology
for many waste codes containing hazardous organic constituents,
high total organic content, and high filterable solids content,
regardless of whether any facility is currently treating these
wastes. The basis for this determination is data found in
literature and data generated by EPA confirming the use of rotary
kiln incineration on wastes having the above characteristics.
If no commercial treatment or recovery operations are
identified for a waste or wastes with similar physical or
chemical characteristics that affect treatment selection, the
Agency will be unable to identify any demonstrated treatment
technologies for the waste, and, accordingly, the waste will be
prohibited from land disposal (unless handled in accordance with
the exemption and variance provisions of the rule). The Agency
is, however, committed to establishing treatment standards as
soon as new or improved treatment processes are demonstrated (and
available).
Operations only available at research facilities, pilot- and
bench- scale operations will not be considered in identifying
demonstrated treatment technologies for a waste because these
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technologies would not necessarily be "demonstrated."
Nevertheless, EPA may use data generated at research facilities
in assessing the performance of demonstrated technologies.
As discussed earlier, Congress intended that technologies
used to establish treatment standards under Section 3004(m) be
not only "demonstrated," but also available. To decide whether
demonstrated technologies may be considered "available," the
Agency determines whether they (1) are commercially available and
(2) substantially diminish the toxicity of the waste or
substantially reduce the likelihood of migration of hazardous
constituents from the waste.
EPA will only set treatment standards based on a technology
that meets the above criteria. Thus, the decision to classify a
technology as "unavailable" will have a direct impact on the
treatment standard. If the best technology is unavailable, the
treatment standard will be based on the next best treatment
technology determined to be available. To the extent that the
resulting treatment standards are less stringent, greater
concentrations of hazardous constituents in the treatment
residuals could be placed in land disposal units.
«•
There also may be circumstances in which EPA concludes that
for a given waste none of the demonstrated treatment technologies
are "available" for purposes of establishing the 3004(m)
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treatment performance standards. Subsequently, these wastes will
be prohibited from continued placement in or on the land unless
managed in accordance with applicable exemptions and variance
provisions. The Agency is, however, committed to establishing
new treatment standards as soon as new or improved treatment
processes become "available."
(1) Proprietary or Patented Processes. If the demonstrated
treatment technology is a proprietary or patented process that is
not generally available, EPA will not consider the technology in
its determination of the treatment standards. EPA will consider
proprietary or patented processes available if it determines that
the treatment method can be purchased or licensed from the
proprietor or is commercially available treatment. The services
of the commercial facility offering this technology often can be
purchased even if the technology itself cannot be purchased.
(2) Substantial Treatment. To be considered "available," a
demonstrated treatment technology must "substantially diminish
the toxicity" of the waste or "substantially reduce the
likelihood of migration of hazardous constituents" from the waste
in accordance with section 3004(m). By requiring that
substantial treatment be achieved in order to set a treatment
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standard, the statute ensures that all wastes are adequately
treated before being placed in or on the land and ensures that
the Agency does not require a treatment method that provides
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little or no environmental benefit. Treatment will always be
deemed substantial if it results in nondetectable levels of the
hazardous constituents of concern. If nondetectable levels are
not achieved, then a determination of substantial treatment will
be made on a case-by-case basis. This approach is necessary
because of the difficulty of establishing a meaningful guideline
that can be applied broadly to the many wastes and technologies
to be considered. EPA will consider the following factors in an
effort to evaluate whether a technology provides substantial
treatment on a case-by-case basis:
(a) Number and types of constituents treated;
(b) Performance (concentration of the constituents in the
treatment residuals); and
(c) Percent of constituents removed.
If none of the demonstrated treatment technologies achieve
substantial treatment of a waste, the Agency cannot establish
treatment standards for the constituents of concern in that
waste.
1.2.3 Collection of Performance Data
Performance data on the demonstrated available technologies
are evaluated by the Agency to determine whether the data are
representative of well-designed and well-operated treatment
systems. Only data from well-designed and well-operated systems
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are included in determining BOAT. The data evaluation includes
data already collected directly by EPA and/or data provided by
industry. In those instances where additional data are needed to
supplement existing information, EPA collects additional data
through a sampling and analysis program. The principal elements
of this data collection program are: (a) identification of
facilities for site visits, (b) engineering site visit,
(c) Sampling and Analysis Plan, (d) sampling visit, and (e)
Onsite Engineering Report.
(1) Identification of Facilities for Site Visits. To
identify facilities that generate and/or treat the waste of
concern, EPA uses a number of information sources. These include
Stanford Research Institute's Directory of Chemical Producers,
EPA's Hazardous Waste Data Management System (HWDMS), the 1986
Treatment, Storage, Disposal Facility (TSDF) National Screening
Survey, and EPA's Industry Studies Data Base. In addition, EPA
contacts trade associations to inform them that the Agency is
considering visits to facilities in their industry and to solicit
assistance in identifying facilities for EPA to consider in its
treatment sampling program.
After identifying facilities that treat the waste, EPA uses
this hierarchy to select sites for engineering visits:
(1) generators treating single wastes on site; (2) generators
treating multiple wastes together on site; (3) commercial
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treatment, storage, and disposal facilities (TSDFs); and (4) EPA
in-house treatment. This hierarchy is based on two concepts:
(1) to the extent possible, EPA should develop treatment
standards from data produced by treatment facilities handling
only a single waste, and (2) facilities that routinely treat a
specific waste have had the best opportunity to optimize design
parameters. Although excellent treatment can occur at many
facilities that are not high in this hierarchy, EPA has adopted
this approach to avoid, when possible, ambiguities related to the
mixing of wastes before and during treatment.
When possible, the Agency will evaluate treatment
technologies using commercially operated systems. If performance
data from properly designed and operated commercial treatment
methods for a particular waste or a waste judged to be similar
are not available, EPA may use data from research facilities
operations. Whenever research facility data are used, EPA will
explain why such data were used in the preamble and background
document and will request comments on the use of such data.
Although EPA's data bases provide information on treatment
for individual wastes, the data bases rarely provide data that
support the selection of one facility for sampling over another.
In cases where several treatment sites appear to fall into the
same level of the hierarchy, EPA selects sites for visits
strictly on the basis of which facility could most expeditiously
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be visited and later sampled if justified by the engineering
visit.
(2) Engineering Site Visit. Once a treatment facility has
been selected, an engineering site visit is made to confirm that
a candidate for sampling meets EPA's criteria for a well-designed
facility and to ensure that the necessary sampling points can be
accessed to determine operating parameters and treatment
effectiveness. During the visit, EPA also confirms that the
facility appears to be well operated, although the actual
operation of the treatment system during sampling is the basis
for EPA's decisions regarding proper operation of the treatment
unit. In general, the Agency considers a well-designed facility
to be one that contains the unit operations necessary to treat
the various hazardous constituents of the waste as well as to
control other nonhazardous materials in the waste that may affect
treatment performance.
In addition to ensuring that a system is reasonably well
designed, the engineering visit examines whether the facility has
a way to measure the operating parameters that affect performance
of the treatment system during the waste treatment period. For
example, EPA may choose not to sample a treatment system that
operates in a continuous mode, for which an important operating
parameter cannot be continuously recorded. In such systems,
instrumentation is important in determining whether the treatment
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system is operating at design values during the waste treatment
period.
(3) Sampling and Analysis Plan. If after the engineering
site visit the Agency decides to sample a particular plant, the
Agency will then develop a site-specific Sampling and Analysis
Plan (SAP) according to the Generic Quality Assurance Project
Plan for the Land Disposal Restriction Program ("BOAT"),
EPA/530-SW-87-011. In brief, the SAP discusses where the Agency
plans to sample, how the samples will be taken, the frequency of
sampling, the constituents to be analyzed and the method of
analysis, operational parameters to be obtained, and specific
laboratory quality control checks on the analytical results.
The Agency will generally produce a draft of the
site-specific Sampling and Analysis Plan within 2 to 3 weeks of
the engineering visit. The draft of the SAP is then sent to the
plant for review and comment. With few exceptions, the draft SAP
should be a confirmation of data collection activities discussed
with the plant personnel during the engineering site visit. EPA
encourages plant personnel to recommend any modifications to the
SAP that they believe will improve the quality of the data.
It is important to note that sampling of a plant by EPA does
not mean that the data will be used in the development of
treatment standards for BOAT. EPA's final decision on whether to
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use data from a sampled plant depends on the actual analysis of
the waste being treated and on the operating conditions at the
time of sampling. Although EPA would not plan to sample a
facility that was not ostensibly well-designed and well-operated,
there is no way to ensure that at the time of the sampling the
facility will not experience operating problems. Additionally,
EPA statistically compares its test data to suitable
industry-provided data, where available, in its determination of
what data to use in developing treatment standards. The
methodology for comparing data is presented later in this
section.
(Note: Facilities wishing to submit data for consideration
in the development of BOAT standards should, to the extent
possible, provide sampling information similar to that acquired
by EPA. Such facilities should review the Generic Quality
Assurance Project Plan for the Land Disposal Restriction Program
("BOAT"), which delineates all of the quality control and quality
assurance measures associated with sampling and analysis.
Quality assurance and quality control procedures are summarized
in Section 1.2.6 of this document.)
(4) Sampling Visit. The purpose of the sampling visit is
v
to collect samples that characterize the performance of the
treatment system and to document the operating conditions that
existed during the waste treatment period. At a minimum, the
1-18 Rev. 3
-------
Agency attempts to collect sufficient samples of the untreated
waste and solid and liquid treatment residuals so that
variability in the treatment process can be accounted for in the
development of the treatment standards. To the extent
practicable, and within safety constraints, EPA or its
contractors collect all samples and ensure that chain-of-custody
procedures are conducted so that the integrity of the data is
maintained.
In general, the samples collected during the sampling visit
will have already been specified in the SAP. In some instances,
however, EPA will not be able to collect all planned samples
because of changes in the facility operation or plant upsets; EPA
will explain any such deviations from the SAP in its follow-up
Onsite Engineering Report.
(5) Onsite Engineering Report. EPA summarizes all its data
collection activities and associated analytical results for
testing at a facility in a report referred to as the Onsite
Engineering Report (OER). This report characterizes the waste(s)
treated, the treated residual concentrations, the design and
operating data, and all analytical results including methods used
and accuracy results. This report also describes any deviations
from EPA's suggested analytical methods for hazardous wastes
(Test Methods for Evaluating Solid Waste, SW-846, Third Edition,
November 1986).
1-19 Rev. 3
-------
After the Onsite Engineering Report is completed, the report
is submitted to the plant for review. This review provides the
plant with a final opportunity to claim any information contained
in the report as confidential. Following the review and
incorporation of comments, as appropriate, the report is made
available to the public with the exception of any material
claimed as confidential by the plant.
1.2.4 Hazardous Constituents Considered and Selected for
Regulation
(1) Development of BOAT List. The list of hazardous
constituents within the waste codes that are targeted for
treatment is referred to by the Agency as the BOAT constituent
list. This list, provided as Table 1-1, is derived from the
constituents presented in 40 CFR Part 261, Appendix VII and
Appendix VIII, as well as several ignitable constituents used as
the basis of listing wastes as F003 and F005. These sources
provide a comprehensive list of hazardous constituents
specifically regulated under RCRA. The BOAT list consists of
those constituents that can be analyzed using methods published
in SW-846, Third Edition.
The initial BOAT constituent list was published in EPA's
Generic Quality Assurance Project Plan, March 1987
(EPA/53O-SW-87-011). Additional constituents will be added to
1-20 Rev. 3
-------
ISZlg
Table 1-1 BOAT Constituent List
BOAT
reference
no.
222.
1.
2.
3.
4.
5.
6.
223.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
224.
225.
226.
30.
227.
31.
214
32.
Parameter
Volatiles
Acetone
Acetonitri le
Acrolein
Acrylonitrile
Benzene
Bromodichloromethane
Bromomethane
n-Butyl alcohol
Carbon tetrachloride
Carbon disulfide
Chlorobenzene
2-Chloro-l,3-butad7ene
Chlorodibromomethane
Chloroethane
2-Chloroethyl vinyl ether
Chloroform
Chloromethane
3-Chloropropene
l,2-Dibromo-3-ch?oropropane
1,2-Dibromoethane
Dibromomethane
Trans-1 ,4-Dichloro-2-butene
Dichlorod if luoromethane
1 , 1-Dichloroethane
1 ,2-Oichloroethane
1 ,1-Dichloroethylene
Trans-1 ,2-Oichloroethene
1,2-Oichloropropane
Trans-1 ,3-Dichloropropene
cis-1 ,3-Oichloropropene
1,4-Dioxane
2-Ethoxyethanol
Ethyl acetate
Ethyl benzene
Ethyl cyanide
Ethyl ether
Ethyl methacrylate
Ethylene oxide
lodomethane
Cas no.
67-64-1
75-05-8
107-03-8
107-13-1
71-43-2
75-27-4
74-83-9
71-36-3
56-23-5
75-15-0
108-90-7
126-99-8
124-48-1
75-00-3
110-75-8
67-66-3
74-87-3
107-05-1
96-12-8
106-93-4
74-95-3
110-57-6
75-71-8
75-34-3
107-06-2
75-35-4
156-60-5
78-87-5
10061-02-6
10061-01-5
123-91-1
60-29-7
141-78-6
100-41-4
107-12-D
60-29-7
97-63-2
75-21-8
74-88-4
1-21 Rev. 3
-------
1521g
Table 1-1 (continued)
BOAT
reference
no.
33.
228.
34.
229.
35.
37.
38.
230.
39.
40.
41.
42.
43.
44.
45.
46.
47.
48.
49.
231.
50.
215.
216.
217.
51.
52.
53.
54.
55.
56.
57.
58.
59.
218.
60.
61.
62.
Parameter
Volatl les (continued)
Isobutyl alcohol
Methanol
Methyl ethyl ketone
Methyl isobutyl ketone
Methyl methacrylate
Methacrylonitri le
Methylene chloride
2-Nitropropane
Pyridme
1,1,1 , 2-Tetrachloroethane
1,1, 2 , 2-Tetrachloroethane
Tetrachloroethene
Toluene
Tnbromomethane
1,1, 1-Trichloroethane
1 , 1 ,2-Trichloroethane
Tnchloroethene
Trichloromonof luoromethane
1 ,2,3-Trichloropropane
l,l,2-Tnchloro-l,2,2-tnf luoro-
ethane
Vinyl chloride
1,2-Xylene
1,3-Xylene
1 ,4-Xylene
Semivolat i les
Acenaphthalene
Acenaphthene
Acetophenone
2-Acetylaminof luorene
4-Aminobiphenyl
Am 1 me
Anthracene
Aramite
Benz(a)anthracene
Benzal chloride
Benzenethiol
Deleted
Benzo(a)pyrene
Cas no.
78-83-1
67-56-1
78-93-3
108-10-1
80-62-6
126-98-7
75-09-2
79-46-9
110-86-1
630-20-6
79-34-6
127-18-4
108-88-3
75-25-2
71-55-6
79-00-5
79-01-6
75-69-4
96-18-4
76-13-1
75-01-4
97-47-6
108-38-3
106-44-5
208-96-8
83-32-9
96-86-2
53-96-3
92-67-1
62-53-3
120-12-7
140-57-8
56-55-3
98-87-3
108-98-5
50-32-8
1-22 Rev. 3
-------
1521g
Table 1-1 (continued)
BOAT
reference
63.
64
65.
66.
67.
68.
69.
70.
71.
72.
73.
74.
75.
76.
77.
78.
79.
80.
81.
82.
232.
83
84
85.
86. '
87
88.
89.
90.
91.
92.
93.
94
95
96
97.
98
99
100.
101.
Parameter
Semivolatiles (continued)
Benzo ( b ) f 1 uorant hene
Benzo(ghi jperylene
Benzo(k)f luoranthene
p-Benzoquinone
B i s ( 2-ch loroethoxy ) methane
Bis(2-chloroethyl)ether
Bis(2-chloroisopropyl)ether
B1s(2-ethylhexyl)phthalate
4-Bromophenyl phenyl ether
Butyl benzyl phthalate
2-sec-Butyl-4,6-dimtrophenol
p-Chloroam 1 me
Chlorobenzi late
p-Chloro-m-cresol
2-Chloronaphthalene
2-Chlorophenol
3-Chloropropionitn le
Chrysene
ortho-Cresol
para-Cresol
Cyclohexanone
D i benz ( a, h) anthracene
Dibenzo(a,e)pyrene
Oibenzo(a, i )pyrene
m-Dichlorobenzene
o-Dichlorobenzene
p-Oichlorobenzene
3,3'-Dichlorobenzidine
2,4-Oichlorophenol
2,6-Oichlorophenol
Diethyl phthalate
3,3'-Dimethoxybenzidine
p-Oi me thy lam inoazobenzene
3,3'-Dimethylbenzidine
2,4-Dimethylphenol
Dimethyl phthalate
Oi-n-butyl phthalate
1 ,4-Dinitrobenzene
4,6-Dinitro-o-cresol
2,4-Dinitrophenol
CAS no.
205-99-2
191-24-2
207-08-9
106-51-4
111-91-1
111-44-4
39638-32-9
117-81-7
101-55-3
85-68-7
88-85-7
106-47-8
510-15-6
59-50-7
91-58-7
95-57-8
542-76-7
218-01-9
95-48-7
106-44-5
108-94-1
53-70-3
192-65-4
189-55-9
541-73-1
95-50-1
106-46-7
91-94-1
120-83-2
87-65-0
84-66-2
119-90-4
60-11-7
119-93-7
105-67-9
131-ll-*3
84-74-2
100-25-4
534-52-1
51-28-5
1-23
Rev. 3
-------
1521g
Table 1-1 (continued)
BOAT
reference
no.
102.
103.
104.
105.
106.
219.
107.
108.
109.
110.
111.
112.
113.
114.
115.
116.
117.
118.
119.
120.
36.
121.
122.
123.
124.
125.
126.
127.
128.
129.
130.
131.
132.
133.
134.
135.
136.
137.
138.
Parameter
Semivolati les (continued)
2,4-Oinitrotoluene
2,6-Dimtrotoluene
Di-n-octyl phthalate
Di-n-propylnitrosamme
Diphenylamine
Dipnenylmtrosamine
1,2-Oiphenylhydrazine
Fluoranthene
Fluorene
Hexach lorobenzene
Hexach lorobutad i ene
Hexachlorocyclopentadlene
Hexachloroethane
Hexach lorophene
Hexach loropropene
Indeno(l,2,3-cd)pyrene
Isosafrole
Methapyrilene
3-Methylcholanthrene
4,4'-Methylenebis
(2-chloroamline)
Methyl methanesulfonate
Naphthalene
1,4-Naphthoquinone
1-Naphthylamine
2-Naphthylamine
p-Nitroaniline
Nitrobenzene
4-Nitrophenol
N-Nitrosodi-n-butylamine
N-Nitrosodiethylamine
N-Nitrosodimethylamine
N-Nitrosomethylethylamine
N-Nitrosomorpholine
N-Nitrosopipendine
n-Nitrosopyrrolidme
5-Nitro-o-toluidine
Pentach lorobenzene
Pentach loroethane
Pentach loron 1 1 robenzene
CAS no.
121-14-2
606-20-2
117-84-0
621-64-7
122-39-4
86-30-6
122-66-7
206-44-0
86-73-7
118-74-1
87-68-3
77-47-4
67-72-1
70-30-4
1888-71-7
193-39-5
120-58-1
91-80-5
56-49-5
101-14-4
66-27-3
91-20-3
130-15-4
134-32-7
91-59-8
100-01-6
98-95-3
100-02-7
924-16-3
55-18-5
62-75-9
10595-95-6
59-89-2
100-75-4
930-55-7
99-65-8
608-93-5
76-01-7
82-68-8
1-24 Rev. 3
-------
1521g
Table 1-1 (continued)
BOAT
reference
no.
139.
140.
141.
142
220.
143.
144.
145.
146.
147.
148.
149.
150.
151.
152.
153.
154.
155.
156.
157.
158.
159.
221.
160.
161.
162.
163.
164.
165.
166.
167.
168
169.
170.
171
Parameter
Semivolatiles (continued)
Pentachlorophenol
Phenacetin
Phenanthrene
Phenol
Phthalic anhydride
2-Picoline
Pronamide
Pyrene
Resorcinol
Safrole
1 , 2 , 4 , 5-Tetrachlorobenzene
2,3,4, 6-Tetrach loropheno 1
1 ,2,4-Trichlorobenzene
2,4,5-Tnchlorophenol
2, 4, 6-Trich loropheno 1
Tr i s ( 2 , 3-d i bromopropy 1 )
phosphate
Metals
Antimony
Arsenic
Barium
Beryll ium
Cadmium
Chromium (total)
Chromium (hexavalent)
Copper
Lead
Mercury
Nickel
Selenium
Silver
Thallium
Vanadium
Zinc
Inorganics
Cyanide
Fluoride
Sulf ide
CAS no.
87-86-5
62-44-2
85-01-8
108-95-2
85-44-9
109-06-8
23950-58-5
129-00-0
108-46-3
94-59-7
95-94-3
58-90-2
120-82-1
95-95-4
88-06-2
126-72-7
7440-36-0
7440-38-2
7440-39-3
7440-41-7
7440-43-9
7440-47-32
-
7440-50-8
7439-92-1
7439-97-6
7440-02-0
7782-49-2
7440-22-4
7440-28-0
7440-62-2
7440-6&-6
57-12-5
16964-48-8
8496-25-8
1-25
Rev. 3
-------
1521g
Table 1-1 (continued)
BOAT
reference
no.
172.
173.
174.
175.
176.
177.
178.
179.
180.
181.
182.
183.
184.
185.
186.
187.
188.
189.
190.
191.
192.
193.
194.
195.
196.
197.
198.
199.
200.
201.
202.
Parameter
Orqanochlorine pesticides
Aldrin
alpha-BHC
beta-BHC
delta-BHC
ganma-BHC
Chlordane
ODD
DDE
DDT
Dieldrin
Endosulfan I
Endosulfan II
Endrin
Endrin aldehyde
Heptachlor
Heptachlor epoxide
Isodnn
Kepone
Methoxyclor
Toxaphene
Phenoxvacet ic acid herbicides
2,4-Dichlorophenoxyacetic acid
Silvex
2,4,5-T
Orqanoohosphorous insecticides
Disulfoton
Famphur
Methyl parathion
Parathion
Phorate
PCBs
Aroclor 1016
Aroclor 1221
Aroclor 1232
CAS no.
309-00-2
319-84-6
319-85-7
319-86-8
58-89-9
57-74-9
72-54-8
72-55-9
50-29-3
60-57-1
939-98-8
33213-6-5
7-2-20-8
7421-93-4
76-44-8
1024-57-3
465-73-6
143-50-0
72-43-5
8001-35-2
94-75-7
93-72-1
93-76-5
298-04-4
52-85-7
298-00-0
56-38-2
298-02-2
V
12674-11-2
11104-28-2
11141-16-5
1-26
Rev. 3
-------
1521g
Table 1-1 (continued)
BOAT
reference Parameter CAS no.
PCBs (continued)
203. Aroclor 1242 53469-21-9
204. Aroclor 1248 12672-29-6
205. Aroclor 1254 11097-69-1
206. Aroclor 1260 11096-82-5
Dioxins and furans
207. Hexachlorodibenzo-p-dioxins
208. Hexachlorodibenzofurans
209. Pentachlorodibenzo-p-dioxins
210. Pentachlorodibenzofurans
211. Tetrachlorodibenzo-p-dioxins
212. Tetrachlorodibenzofurans
213. 2,3,7,8-Tetrachlorodibenzo-p-dioxin 1746-01-6
1-27 Rev. 3
-------
the BDAT constituent list as additional key constituents are
identified for specific waste codes or as new analytical methods
are developed for hazardous constituents. For example, since the
list was published in March 1987, eighteen additional
constituents (hexavalent chromium, xylene (all three isomers),
benzal chloride, phthalic anhydride, ethylene oxide, acetone,
n-butyl alcohol, 2-ethoxyethanol, ethyl acetate, ethyl benzene,
ethyl ether, methanol, methyl isobutyl ketone, 2-nitropropane,
1,1,2-trichloro-1,2,2-trifluoroethane, and cyclohexanone) have
been added to the list.
Chemicals are listed in Appendix VIII if they are shown in
scientific studies to have toxic, carcinogenic, mutagenic, or
teratogenic effects on humans or other life-forms, and they
include such substances as those identified by the Agency's
Carcinogen Assessment Group as being carcinogenic. Including a
constituent in Appendix VIII means that the constituent can be
cited as a basis for listing toxic wastes.
Although Appendix VII, Appendix VIII, and the F003 and F005
ignitables provide a comprehensive list of RCRA-regulated
hazardous constituents, not all of the constituents can be
analyzed in a complex waste matrix. Therefore, constituents that
V
could not be readily analyzed in an unknown waste matrix were not
included on the initial BDAT list. As mentioned above, however,
the BDAT constituent list is a continuously growing list that
1-28 Rev. 3
-------
does not preclude the addition of new constituents when
analytical methods are developed.
There are 5 major reasons that constituents were not
included on the BOAT constituent list:
(a) Constituents are unstable. Based on their chemical
structure, some constituents will either decompose in
water or will ionize. For example, maleic anhydride
will form maleic acid when it comes in contact with
water and copper cyanide will ionize to form copper and
cyanide ions. However, EPA may choose to regulate the
decomposition or ionization products.
(b) EPA-approved or verified analytical methods are not
available. Many constituents, such as
1,3,5-trinitrobenzene, are not measured adequately or
even detected using any of EPA's analytical methods
published in SW-846 Third Edition.
(c) The constituent is a member of a chemical group
designated in Appendix VIII as not otherwise specified
(N.O.S.). Constituents listed as N.O.S., such as
chlorinated phenols, are a generic group of some types
of chemicals for which a single analytical procedure is
not available. The individual members of each such
group need to be listed to determine whether the
constituents can be analyzed. For each N.O.S. group,
all those constituents that can be readily analyzed are
included in the BDAT constituents list.
(d) Available analytical procedures are not appropriate for
a complex waste matrix. Some compounds, such as
auramine, can be analyzed as a pure constituent.
However, in the presence of other constituents, the
recommended analytical method does not positively
identify the constituent. The use of high pressure
liquid chromotography (HPLC) presupposes a high
expectation of finding the specific constituents of
interest. In using this procedure to screen samples,
protocols would have to be developed on a case-specific
basis to verify the identity of constituents present in
the samples. Therefore, HPLC is not an appropriate
analytical procedure for complex samples containing
1-29 Rev. 3
-------
unkown constituents.
(e) Standards for analytical instrument calibration are not
commercially available. For several constituents, such
as benz(c)acridine, commercially available standards of
a "reasonably" pure grade are not available. The
unavailability of a standard was determined by a review
of catalogs from specialty chemical manufacturers.
Two constituents (fluoride and sulfide) are not specifically
included in Appendices VII and VIII; however, these compounds are
included on the BDAT list as indicator constituents for compounds
from Appendices VII and VIII such as hydrogen fluoride and
hydrogen sulfide, which ionize in water.
The BDAT constituent list presented in Table 1-1 is divided
into the following nine groups:
o Volatile organics
o Semivolatile organics
o Metals
o Other inorganics
o Organochlorine pesticides
o Phenoxyacetic acid herbicides
o Organophosphorous insecticides
o PCBs
o Dioxins and furans
The constituents were placed in these categories based on their
chemical properties. The constituents in each group are expected
to behave similarily during treatment and are also analyzed, with
the exception of the metals and inorganics, by using the same
V
analytical methods.
1-30 Rev. 3
-------
(2) Constituent Selection Analysis. The constituents that
the Agency selects for regulation in each treatability group are,
in general, those found in the untreated wastes at treatable
concentrations. For certain waste codes, the target list for the
untreated waste may have been shortened (relative to analyses
performed to test treatment technologies) because of the extreme
unlikelihood of the constituent being present.
In selecting constituents for regulation, the first step is
to summarize all the constituents that were found in the
untreated waste at treatable concentrations. This process
involves the use of the statistical analysis of variance (ANOVA)
test, described in Section 1.2.6, to determine if constituent
reductions were significant. The Agency interprets a significant
reduction in concentration as evidence that the technology
actually "treats" the waste.
There are some instances where EPA may regulate constituents
that are not found in the untreated waste but are detected in the
treated residual. This is generally the case where presence of
the constituents in the untreated waste interferes with the
quantification of the constituent of concern. In such instances,
the detection levels of the constituent are relatively high,
V
resulting in a finding of "not detected" when, in fact, the
constituent is present in the waste.
1-31 Rev. 3
-------
After determining which of the constituents in the untreated
waste are present at treatable concentrations, EPA develops a
list of potential constituents for regulation. The Agency then
reviews this list to determine if any of these constituents can
be excluded from regulation because they would be controlled by
regulation of other constituents in the list.
EPA performs this indicator analysis for two reasons: (1) it
reduces the analytical cost burdens on the treater and (2) it
facilitates implementation of the compliance and enforcement
program. EPA's rationale for selection of regulated constituents
for this waste code is presented in Section 5 of this background
document.
(3) Calculation of Standards. The final step in the
calculation of the BDAT treatment standard is the multiplication
of the average treatment value by a factor referred to by the
Agency as the variability factor. This calculation takes into
account that even well-designed and well-operated treatment
systems will experience some fluctuations in performance. EPA
expects that fluctuations will result from inherent mechanical
limitations in treatment control systems, collection of treated
samples, and analysis of these samples. All of the above
fluctuations can be expected to occur at well-designed and
well-operated treatment facilities. Therefore, setting treatment
standards utilizing a variability factor should be viewed not as
1-32 Rev. 3
-------
a relaxing of 3004(m) requirements, but rather as a function of
the normal variability of the treatment processes. A treatment
facility will have to be designed to meet the mean achievable
treatment performance level to ensure that the performance levels
remain within the limits of the treatment standard.
The Agency calculates a variability factor for each
constituent of concern within a waste treatability group using
the statistical calculation presented in Appendix A. The
equation for calculating the variability factor is the same as
that used by EPA for the development of numerous regulations in
the Effluent Guidelines Program under the Clean Water Act. The
variability factor establishes the instantaneous maximum based on
the 99th percentile value.
There is an additional step in the calculation of the
treatment standards in those instances where the ANOVA analysis
shows that more than one technology achieves a level of
performance that represents BOAT. In such instances, the BOAT
treatment standard is calculated by first averaging the mean
performance value for each technology for each constituent of
concern and then multiplying that value by the highest
variability factor among the technologies considered. This
procedure ensures that all the BOAT technologies used as the
basis for the standards will achieve full compliance.
1-33 Rev. 3
-------
1.2.5 Compliance with Performance Standards
All the treatment standards reflect performance achieved by
the Best Demonstrated Available Technology (BDAT). As such,
compliance with these standards only requires that the treatment
level be achieved prior to land disposal. It does not require
the use of any particular treatment technology. While dilution
of the waste as a means to comply with the standard is
prohibited, wastes that are generated in such a way as to
naturally meet the standard can be land disposed without
treatment. With the exception of treatment standards that
prohibit land disposal, all treatment standards proposed are
expressed as a concentration level.
EPA has used both total constituent concentration and TCLP
analyses of the treated waste as a measure of technology
performance. EPA's rationale for when each of these analytical
tests is used is explained in the following discussion.
For all organic constituents, EPA is basing the treatment
standards on the total constituent concentration found in the
treated waste. EPA based its decision on the fact that
technologies exist to destroy the various organics compounds.
V
Accordingly, the best measure of performance would be the extent
to which the various organic compounds have been destroyed or the
total amount of constituent remaining after treatment. (NOTE:
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EPA's land disposal restrictions for solvent waste codes
F001-F005 (51 FR 40572) uses the TCLP value as a measure of
performance. At the time that EPA promulgated the treatment
standards for F001-F005, useful data were not available on total
constituent concentrations in treated residuals and, as a result,
the TCLP data were considered to be the best measure of
performance.)
For all metal constituents, EPA is using both total
constituent concentration and/or the TCLP as the basis for
treatment standards. The total constituent concentration is
being used when the technology basis includes a metal recovery
operation. The underlying principle of metal recovery is the
reduction of the amount of metal in a waste by separating the
metal for recovery; therefore, total constituent concentration in
the treated residual is an important measure of performance for
this technology. Additionally, EPA also believes that it is
important that any remaining metal in a treated residual waste
not be in a state that is easily leachable; accordingly, EPA is
also using the TCLP as a measure of performance. It is important
to note that for wastes for which treatment standards are based
on a metal recovery process, the facility has to comply with both
the total constituent concentration and the TCLP prior to land
V
disposal.
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In cases where treatment standards for metals are not based
on recovery techniques but rather on stabilization, EPA is using
only the TCLP as a measure of performance. The Agency's
rationale is that stabilization is not meant to reduce the
concentration of metal in a waste but only to chemically minimize
the ability of the metal to leach.
1.2.6 Identification of BOAT
(1) Screening of Treatment Data. This section explains how
the Agency determines which of the treatment technologies
represent treatment by BOAT. The first activity is to screen the
treatment performance data from each of the demonstrated and
available technologies according to the following criteria:
(a) Design and operating data associated with the treatment
data must reflect a well-designed, well-operated system
for each treatment data point. (The specific design
and operating parameters for each demonstrated
technology for this waste code are discussed in Section
3.2 of this document.)
(b) Sufficient QA/QC data must be available to determine
the true values of the data from the treated waste.
This screening criterion involves adjustment of treated
data to take into account that the type value may be
different from the measured value. This discrepancy
generally is caused by other constituents in the waste
that can mask results or otherwise interfere with the
analysis of the constituent of concern.
V
(c) The measure of performance must be consistent with
EPA's approach to evaluating treatment by type of
constituents (e.g., total concentration data for
organics, and total concentration and TCLP for metals
in the leachate from the residual).
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In the absence of data needed to perform the screening
analysis, EPA will make decisions on a case-by-case basis of
whether to include the data. The factors included in this
case-by-case analysis will be the actual treatment levels
achieved, the availability of the treatment data and their
completeness (with respect to the above criteria), and EPA's
assessment of whether the untreated waste represents the waste
code of concern. EPA's application of these screening criteria
for this waste code are provided in Section 4 of this background
document.
(2) Comparison of Treatment Data. In cases in which EPA
has treatment data from more than one technology following the
screening activity, EPA uses the statistical method known as
analysis of variance (ANOVA) to determine if one technology
performs significantly better. This statistical method
(summarized in Appendix A) provides a measure of the differences
between two data sets. If EPA finds that one technology performs
significantly better (i.e., the data sets are not homogeneous),
BOAT treatment standards are the level of performance achieved by
the best technology multiplied by the corresponding variability
factor for each regulated constituent.
V
If the differences in the data sets are not statistically
significant, the data sets are said to be homogeneous.
Specifically, EPA uses the analysis of variance to determine
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whether BDAT represents a level of performance achieved by only
one technology or represents a level of performance achieved by
more than one (or all) of the technologies. If the Agency finds
that the levels of performance for one or more technologies are
not statistically different, EPA averages the performance values
achieved by each technology and then multiplies this value by the
largest variability factor associated with any of the
acceptable technologies. A detailed discussion of the treatment
selection method and an example of how EPA chooses BDAT from
multiple treatment systems is provided in Appendix A.
(3) Quality Assurance/Quality Control. This section
presents the principal quality assurance/quality control (QA/QC)
procedures employed in screening and adjusting the data to be
used in the calculation of treatment standards. Additional QA/QC
procedures used in collecting and screening data for the BDAT
program are presented in EPA's Generic Quality Assurance Project
Plan for Land Disposal Restrictions Program ("BOAT")
(EPA/530-SW-87-001, March 1987).
To calculate the treatment standards for the Land Disposal
Restriction Rules, it is first necessary to determine the
recovery value for each constituent (the amount of constituent
recovered after spiking, which is the addition of a known amount
of the constituent, minus the initial concentration in the
samples divided by the amount added) for a spike of the treated
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residual. Once the recovery value is determined, the following
procedures are used to select the appropriate percent recovery
value to adjust the analytical data:
(a) If duplicate spike recovery values are available for
the constituent of interest, the data are adjusted by
the lowest available percent recovery value (i.e., the
value that will yield the most conservative estimate of
treatment achieved). However, if a spike recovery
value of less than 20 percent is reported for a
specific constituent, the data are not used to set
treatment standards because the Agency does not have
sufficient confidence in the reported value to set a
national standard.
(b) If data are not available for a specific constituent
but are available for an isomer, then the spike
recovery data are transferred from the isomer and the
data are adjusted using the percent recovery selected
according to the procedure described in (a) above.
(c) If data are not available for a specific constituent
but are available for a similar class of constituents
(e.g., volatile organics, acid-extractable
semivolatiles), then spike recovery data available for
this class of constituents are transferred. All spike
recovery values greater than or equal to 20 percent for
a spiked sample are averaged and the constituent
concentration is adjusted by the average recovery
value. If spiked recovery data are available for more
than one sample, the average is calculated for each
sample and the data are adjusted by the lowest average
value.
(d) If matrix spike recovery data are not available for a
set of data to be used to calculate treatment
standards, then matrix spike recovery data are
transferred from a waste that the Agency believes is a
similar matrix (e.g., if the data are for an ash from
incineration, then data from other incinerator ashes
could be used). While EPA recognizes that transfer of
matrix spike recovery data from a similar waste is not
an exact analysis, this is considered the best approach
for adjusting the data to account for the fact that
most analyses do not result in extraction of 100
percent of the constituent. In assessing the recovery
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data to be transferred, the procedures outlined in (a),
(b), and (c) above are followed.
The analytical procedures employed to generate the data used
to calculate the treatment standards are listed in Appendix E of
this document. In cases where alternatives or equivalent
procedures and/or equipment are allowed in EPA's SW-846, Third
Edition (November 1986) methods, the specific procedures and
equipment used are also documented in this Appendix. In
addition, any deviations from the SW-846, Third Edition, methods
used to analyze the specific waste matrices are documented. It
is important to note that the Agency will use the methods and
procedures delineated in Appendix E to enforce the treatment
standards presented in Section 6 of this document. Accordingly,
facilities should use these procedures in assessing the
performance of their treatment systems.
1.2.7 BOAT Treatment Standards for "Derived-From" and "Mixed"
Wastes
(1) Wastes from Treatment Trains Generating Multiple
Residues. In a number of instances, the proposed BDAT consists
of a series of operations each of which generates a waste
residue. For example, the proposed BDATvfor a certain waste code
is based on solvent extraction, steam stripping, and activated
carbon adsorption. Each of these treatment steps generates a
waste requiring treatment — a solvent-containing stream from
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solvent extraction, a stripper overhead, and spent activated
carbon. Treatment of these wastes may generate further residues;
for instance, spent activated carbon (if not regenerated) could
be incinerated, generating an ash and possibly a scrubber water
waste. Ultimately, additional wastes are generated that may
require land disposal. With respect to these wastes, the Agency
wishes to emphasize the following points:
(a) All of the residues from treating the original listed
wastes are likewise considered to be the listed waste
by virtue of the derived-from rule contained in 40 CFR
Part 261.3(c)(2). (This point is discussed more fully
in (2) below.) Consequently, all of the wastes
generated in the course of treatment would be
prohibited from land disposal unless they satisfy the
treatment standard or meet one of the exceptions to the
prohibition.
(b) The Agency's proposed treatment standards generally
contain a concentration level for wastewaters and a
concentration level for nonwastewaters. The treatment
standards apply to all of the wastes generated in
treating the original prohibited waste. Thus, all
solids generated from treating these wastes would have
to meet the treatment standard for nonwastewaters. All
derived-from wastes meeting the Agency definition of
wastewater (less than 1 percent TOG and less than 1
percent total filterable solids) would have to meet the
treatment standard for wastewaters. EPA wishes to make
clear that this approach is not meant to allow partial
treatment in order to comply with the applicable
standard.
(c) The Agency has not performed tests, in all cases, on
every waste that can result from every part of the
treatment train. However, the Agency's treatment
standards are based on treatment of the most
concentrated form of the waste. Consequently, the
Agency believes that the less concentrated wastes
generated in the course of treatment will also be able
to be treated to meet this value.
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(2) Mixtures and Other Derived-From Residues. There is a
further question as to the applicability of the BOAT treatment
standards to residues generated not from treating the waste (as
discussed above), but from other types of management. Examples
are contaminated soil or leachate that is derived from managing
the waste. In these cases, the mixture is still deemed to be the
listed waste, either because of the derived-from rule (40 CFR
Part 261.3(c)(2)(i)) or the mixture rule (40 CFR Part
261.3(a)(2)(iii) and (iv) or because the listed waste is
contained in the matrix (see, for example, 40 CFR Part
261.33(d)). The prohibition for the particular listed waste
consequently applies to this type of waste.
The Agency believes that the majority of these types of
residues can meet the treatment standards for the underlying
listed wastes (with the possible exception of contaminated soil
and debris for which the Agency is currently investigating
whether it is appropriate to establish a separate treatability
subcategorization). For the most part, these residues will be
less concentrated than the original listed waste. The Agency's
treatment standards also make a generous allowance for process
variability by assuming that all treatability values used to
establish the standard are lognormally distributed. The waste
also might be amenable to a relatively nonvariable form of
treatment technology such as incineration. Finally, and perhaps
most important, the rules contain a treatability variance that
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allows a petitioner to demonstrate that its waste cannot be
treated to the level specified in the rule (40 CFR Part
268.44(a). This provision provides a safety valve that allows
persons with unusual waste matrices to demonstrate the
appropriateness of a different standard. The Agency, to date,
has not received any petitions under this provision (for example,
for residues contaminated with a prohibited solvent waste),
indicating, in the Agency's view, that the existing standards are
generally achievable.
(3) Residues from Managing Listed Wastes or that Contain
Listed Wastes. The Agency has been asked if and when residues
from managing hazardous wastes, such as leachate and contaminated
ground water, become subject to the land disposal prohibitions.
Although the Agency believes this question to be settled by
existing rules and interpretative statements, to avoid any
possible confusion the Agency will address the question again.
Residues from managing First Third wastes, listed California
List wastes, and spent solvent and dioxin wastes are all
considered to be subject to the prohibitions for the underlying
hazardous waste. Residues from managing California List wastes
likewise are subject to the California List prohibitions when the
residues themselves exhibit a characteristic of hazardous waste.
This determination stems directly from the derived-from rule in
40 CFR Part 261.3(c)(2) or in some cases from the fact that the
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waste is mixed with or otherwise contains the listed waste. The
underlying principle stated in all of these provisions is that
listed wastes remain listed until delisted.
The Agency's historic practice in processing delisting
petitions addressing mixing residuals has been to consider them
to be the listed waste and to require that delisting petitioners
address all constituents for which the derived-from waste (or
other mixed waste) was listed. The language in 40 CFR Part
260.22(b) states that mixtures or derived-from residues can be
delisted provided a delisting petitioner makes a demonstration
identical to that which a delisting petitioner would make for the
underlying waste. These residues consequently are treated as the
underlying listed waste for delisting purposes. The statute
likewise takes this position, indicating that soil and debris
that are contaminated with listed spent solvents or dioxin wastes
are subject to the prohibition for these wastes even though these
wastes are not the originally generated waste, but rather are a
residual from management (RCRA section 3004(e)(3)). It is EPA's
view that all such residues are covered by the existing
prohibitions and treatment standards for the listed hazardous
waste that these residues contain and from which they are
derived.
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1.2.8 Transfer of Treatment Standards
EPA is proposing some treatment standards that are not based
on testing of the treatment technology of the specific waste
subject to the treatment standard. Instead, the Agency has
determined that the constituents present in the subject waste can
be treated to the same performance levels as those observed in
other wastes for which EPA has previously developed treatment
data. EPA believes that transferring treatment performance for
use in establishing treatment standards for untested wastes is
valid technically in cases where the untested wastes are
generated from similar industries, similar processing steps, or
have similar waste characteristics affecting performance and
treatment selection. Transfer of treatment standards to similar
wastes or wastes from similar processing steps requires little
formal analysis. However, in the case where only the industry is
similar, EPA more closely examines the waste characteristics
prior to concluding that the untested waste constituents can be
treated to levels associated with tested wastes.
EPA undertakes a two-step analysis when determining whether
wastes generated by different processes within a single industry
can be treated to the same level of performance. First, EPA
reviews the available waste characteristic data to identify those
parameters that are expected to affect treatment selection. EPA
has identified some of the most important constituents and other
1-45 Rev. 3
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parameters needed to select the treatment technology appropriate
for a given waste. A detailed discussion of each analysis,
including how each parameter was selected for each waste, can be
found in the background document for each waste.
Second, when an individual analysis suggests that an
untested waste can be treated with the same technology as a waste
for which treatment performance data are already available, EPA
analyzes a more detailed list of constituents that represent some
of the most important waste characteristics that the Agency
believes will affect the performance of the technology. By
examining and comparing these characteristics, the Agency
determines whether the untested wastes will achieve the same
level of treatment as the tested waste. Where the Agency
determines that the untested waste is easier to treat than the
tested waste, the treatment standards can be transferred. A
detailed discussion of this transfer process for each waste can
be found in later sections of this document.
1.3 Variance from the BOAT Treatment Standard
The Agency recognizes that there may exist unique wastes
that cannot be treated to the level specified as the treatment
standard. In such a case, a generator or owner/operator may
submit a petition to the Administrator requesting a variance from
the treatment standard. A particular waste may be significantly
1-46 Rev. 3
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different from the wastes considered in establishing treatability
groups because the waste contains a more complex matrix that
makes it more difficult to treat. For example, complex mixtures
may be formed when a restricted waste is mixed with other waste
streams by spills or other forms of inadvertent mixing. As a
result, the treatability of the restricted waste may be altered
such that it cannot meet the applicable treatment standard.
Variance petitions must demonstrate that the treatment
standard established for a given waste cannot be met. This
demonstration can be made by showing that attempts to treat the
waste by available technologies were not successful or by
performing appropriate analyses of the waste, including waste
characteristics affecting performance, which demonstrate that the
waste cannot be treated to the specified levels. Variances will
not be granted based solely on a showing that adequate BOAT
treatment capacity is unavailable. (Such demonstrations can be
made according to the provisions in Part 268.5 of RCRA for
case-by-case extensions of the effective date.) The Agency will
consider granting generic petitions provided that representative
data are submitted to support a variance for each facility
covered by the petition.
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Petitioners should submit at least one copy to:
The Administrator
U.S. Environmental Protection Agency
401 M Street, S.W.
Washington, DC 20460
An additional copy marked "Treatability Variance" should be
submitted to:
Chief, Waste Treatment Branch
Office of Solid Waste (WH-565)
U.S. Environmental Protection Agency
401 M Street, S.W.
Washington, DC 20460
Petitions containing confidential information should be sent
with only the inner envelope marked "Treatability Variance" and
"Confidential Business Information" and with the contents marked
in accordance with the requirements of 40 CFR Part 2 (41 FR
36902, September 1, 1976, amended by 43 FR 4000).
The petition should contain the following information:
(1) The petitioner's name and address.
(2) A statement of the petitioner's interest in the
proposed action.
(3) The name, address, and EPA identification number of the
facility generating the waste, and the name and
telephone number of the plant contact.
(4) The process(es) and feed materials generating the waste
and an assessment of whether such process(es) or feed
materials may produce a waste that is not covered by
the demonstration.
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(5) A description of the waste sufficient for comparison
with the waste considered by the Agency in developing
BDAT, and an estimate of the average and maximum
monthly and annual quantities of waste covered by the
demonstration. (Note: The petitioner should consult
the appropriate BDAT background document for
determining the characteristics of the wastes
considered in developing treatment standards.)
(6) If the waste has been treated, a description of the
system used for treating the waste, including the
process design and operating conditions. The petition
should include the reasons the treatment standards are
not achievable and/or why the petitioner believes the
standards are based on inappropriate technology for
treating the waste. (Note: The petitioner should refer
to the BDAT background document as guidance for
determining the design and operating parameters that
the Agency used in developing treatment standards.)
(7) A description of the alternative treatment systems
examined by the petitioner (if any); a description of
the treatment system deemed appropriate by the
petitioner for the waste in question; and, as
appropriate, the concentrations in the treatment
residual or extract of the treatment residual (i.e.,
using the TCLP where appropriate for stabilized metals)
that can be achieved by applying such treatment to the
waste.
(8) A description of those parameters affecting treatment
selection and waste characteristics that affect
performance, including results of all analyses. (See
Section 3.0 for a discussion of waste characteristics
affecting performance that the Agency has identified
for the technology representing BDAT.)
(9) The dates of the sampling and testing.
(10) A description of the methodologies and equipment used
to obtain representative samplevs.
(11) A description of the sample handling and preparation
techniques, including techniques used for extraction,
containerization, and preservation of the samples.
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(12) A description of analytical procedures used including
QA/QC methods.
After receiving a petition for a variance, the Administrator
may request any additional information or waste samples that may
be required to evaluate and process the petition. Additionally,
all petitioners must certify that the information provided to the
Agency is accurate under 40 CFR Part 268.4(b).
In determining whether a variance will be granted, the
Agency will first look at the design and operation of the
treatment system being used. If EPA determines that the
technology and operation are consistent with BOAT, the Agency
will evaluate the waste to determine if the waste matrix and/or
physical parameters are such that the BDAT treatment standards
reflect treatment of this waste. Essentially, this latter
analysis will concern the parameters affecting treatment
selection and waste characteristics affecting performance
parameters.
In cases where BDAT is based on more than one technology,
the petitioner will need to demonstrate that the treatment
standard cannot be met using any of the technologies, or that
none of the technologies are appropriate vfor treatment of the
waste. After the Agency has made a determination on the
petition, the Agency's findings will be published in the Federal
Register, followed by a 30-day period for public comment.
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After review of the public comments, EPA will publish its final
determination in the Federal Register as an amendment to the
treatment standards in 40 CFR Part 268, Subpart D.
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2. INDUSTRY AFFECTED AND WASTE CHARACTERIZATION
The previous section provided the background for the
Agency's study of K103 and K104 wastes. The purpose of this
section is to describe the industry that will be affected by land
disposal restrictions on waste codes K103 and K104, and to
characterize these wastes. This section includes a description
of the industry affected, the production processes employed in
this industry, and a discussion of how K103 and K104 wastes are
generated by these processes. The section concludes with a
characterization of the K103 and K104 waste streams, and a
determination of the waste treatability group for these wastes.
The full list of hazardous waste codes from specific sources
is given in 40 CFR 261.32 (see discussion in Section 1 of this
document). Within this list, two specific hazardous waste codes
are generated by the aniline/nitrobenzene industry:
K103: Process residues from aniline extraction from the
production of aniline (basis for listing:
aniline, nitrobenzene, phenylenediamine).
K104: Combined wastewater streams generated from
nitrobenzene/aniline production (basis for
listing: aniline, benzene, diphenylamine,
nitrobenzene, phenylenediamine).
The Agency has determined that these waste codes (K103 and
K104) represent a separate waste treatability group. This was
established because industry processes are similar; therefore,
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the wastes are expected to have similar physical and chemical
characteristics (see Section 1 for a discussion of waste
treatability groups). In addition, these wastes are frequently
mixed in industry prior to treatment. As a result, the Agency
has examined the sources of the wastes, applicable treatment
technologies, and treatment performance attainable in order to
support a single regulatory approach for the two wastes.
2.1 Industry Affected and Process Description
The four digit standard industrial classification (SIC) code
reported for the aniline/nitrobenzene industry is 2869. The
Agency estimates that six facilities in the United States are
actively involved in aniline production which could generate
K103. Four of these facilities are actively co-producing aniline
and nitrobenzene, and could generate K104 waste.
Information from trade associations provide a geographic
distribution of the number of these facilities across the United
States. Tables 2-1 and 2-2 present the location of those
facilities which may generate waste codes K103 and K104 in each
state and in each EPA region. As can be seen in Tables 2-1 and
2-2, these facilities are concentrated in the central and eastern
V
states (EPA Regions III through VI). Figure 2-1 illustrates this
data plotted on a map of the United States.
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Table 2-1 Facilities Producing K103 and K104
State (EPA Region)
Louisiana (VI)
Mississippi (IV)
North Carolina (IV)
Ohio (V)
Texas (VI)
West Virginia (III)
Total
Number of Facilities
1
1
1
1
1
1
6
Reference; SRI Chemical Economics Handbook, 1985
Table 2-2 Facilities Producing K103 and K104
EPA Recrion
III
IV
V
VI
Number of Facil
1
2
1
2
Total 6
ities
Reference; SRI Chemical Economics Handbook, 1985.
Nitrobenzene is manufactured by either liquid or vapor phase
nitration of benzene. The liquid phase nitration process is
reported to be the more prevalent of the two processes used to
manufacture nitrobenzene. In liquid phase nitration, benzene is
nitrated in a reactor with an aqueous mixture of sulfuric acid
and nitric acid (see Figure 2-2). Crude .nitrobenzene is formed,
and is separated from the reactants and by-products by a series
of purification steps.
2-3
Rev. 3
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to
A - ANILINE
PRODUCER
N - NITROBENZENE
PRODUCER
FIGURE 2-1 FACILITIES PRODUCING K103 AND K104 BY STATE AND EPA REGION
-------
LIQUID/
LI8UID
EXTRACTION
TO FURTHER
WASTEtlATER
TREATMENT
SOURCE: DELISTING PETITION FOR WASTE STREAM K104 - COMBINED
WASTEWATER STREAMS GENERATED FROM NITROBENZENE/ANILINE
PRODUCTION. PETITION NO. 0312.
FIGURE 2-2
GENERATION OF K103 AND K104 FROM NITROBENZENE/ANILINE
PRODUCTION (LIQUID PHASE NITRATION OF BENZENE AND LIQUID PHASE
REDUCTION OF NITROBENZENE)
2-5
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In the initial nitrobenzene purification step, the product
stream from the reactor enters a separator where it is cooled and
allowed to settle and to separate by gravity into an organic and
an aqueous phase. The aqueous phase, consisting mainly of
untreated sulfuric and nitric acid, goes to the denitrator where
fresh benzene is added to remove trace amounts of nitric acid.
The benzene and trace amounts of nitrobenzene, formed in the
denitrator, are returned to the nitrobenzene reactor. The acid
phase from the denitrator is sent to the waste acid stripper for
acid recovery by volatilization. The recovered acid from the
waste acid stripper is recycled through an acid concentrator to
the reactor.
The organic phase from the separator, consisting mainly of
nitrobenzene, is washed with water in a prewasher and with
caustic soda in a washer to remove traces of acid. The washwater
streams from the prewasher and washer are both sent to a
wastewater extractor where nitrobenzene is recovered from the
washwater (or wastewater). In the final purification step, the
nitrobenzene stream from the washer is distilled in the
nitrobenzene topping column to produce a high purity nitrobenzene
product.
Aniline is produced by reducing nitrobenzene with hydrogen
in the presence of a catalyst. The three alternative reduction
processes currently in use are as follows: catalytic vapor
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phase, catalytic liquid phase, and dissolving metal (or Bechamp)
process. Most of the aniline in the United States is reported to
be produced by the catalytic vapor phase and catalytic liquid
phase processes.
In the catalytic liquid phase process, nitrobenzene is
reduced by hydrogen to form aniline in the presence of a nickel
catalyst in a reactor (see Figure 2-2). The crude aniline from
the reactor is separated from water and other by-products in a
two-stage gravity decantation process consisting of a crude
aniline separator and a separator. The water phases from both
separators are combined and sent to the aniline liquid/liquid
extractor which recovers aniline from the residual wastewater
stream. The aniline stream from the crude aniline separator is
distilled in a rectification column to produce a high purity
aniline product.
The listed wastes K103 and K104 are generated in the
manufacture of aniline and aniline/nitrobenzene, respectively.
The generation of these wastes is discussed further in Sections
2.1.1 and 2.1.2.
2.1.1 Generation of K103 Waste
V
The listed waste K103 is generated in the production of
aniline in both the crude aniline separator and in the
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aniline/water separator after the rectifier column. In the crude
aniline separator (see Figure 2-2), the product stream from the
aniline reactor is cooled and allowed to settle and separate by
gravity into an organic and an aqueous phase. The aqueous phase,
which is the listed waste K103, is pumped to the aniline
liquid/liquid extractor.
The bottoms stream from the rectifier column that purifies
the crude aniline enters a purge recovery column which separates
water and aniline by distillation. The aniline-containing stream
from the purge recovery columns enters a separator where it is
cooled and allowed to settle and separate by gravity into an
organic and an aqueous phase. The organic phase, consisting
mainly of aniline, is recycled to the aniline reactor. The
aqueous phase, which is the listed waste K103, is combined with
the aqueous phase from the crude aniline separator and pumped to
the aniline liquid/liquid extractor. The bottoms from the purge
recovery column are stored in the tars tank and eventually
incinerated.
2.1.2 Generation of K104 Waste
The listed waste K104 is generated in the production of
V
nitrobenzene at both the prewasher and the washer (see
Figure 2-2). In the prewasher, water is used to remove acid from
the nitrobenzene stream coming from the separator by exploiting
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the relatively high solubility of the acids in water. An organic
phase, consisting mainly of nitrobenzene, is separated from the
aqueous phase in the prewasher and is sent to the washer. The
aqueous phase from the prewasher, which is the listed waste K104,
is sent to the nitrobenzene liquid/liquid extractor.
In the washer, caustic soda is used to neutralize remaining
traces of acid in the nitrobenzene stream from the prewasher. As
before, organic and aqueous phases are formed by settling and
gravity separation. Nitrobenzene is removed with the organic
phase from the washer and enters the nitrobenzene topping column.
The aqueous phase from the washer, which is the listed waste
K104, is combined with the aqueous phase from the prewasher and
enters the nitrobenzene liquid/liquid extractor. Other
wastewater streams from the co-production of nitrobenzene and
aniline are also considered to be K104, if they are not mixed
with the wastewater streams from the prewasher and washer. These
streams include the overhead stream from the waste acid stripper
and the wastewater stream from the aniline liquid/liquid
extractor.
2.2. Waste Characterization
This section includes all waste characterization data
available to the Agency for the K103 and K104 waste treatability
group. An estimate of the major constituents which comprise each
2-9 Rev. 3
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waste and their approximate concentrations is presented in
Table 2-3. The percent concentration of each major constituent
in the waste was determined from best estimates based on chemical
analyses. Table 2-3 shows that the major constituent of both
K103 and K104 is water (at >94.7% and >98.7%, respectively). The
primary organic BOAT constituent in K103 is aniline, with benzene
and sulfide being the other primary BDAT constituents present
(<1.0%). The primary organic BDAT constituent in K104 is
nitrobenzene, with benzene and cyanides being the other primary
BDAT constituents present (<1.0%).
The ranges of BDAT constituents present in each waste and
all other available data concerning waste characterization
parameters obtained from the Onsite Engineering report for E. I.
duPont de Nemours, Beaumont, Texas, are presented by waste code
in Table 2-4. This table lists the levels of BDAT organics
(volatile and semivolatile), metals, and inorganics present in
K103 and K104 wastes. Other parameters analyzed in the wastes
include: total dissolved solids, total suspended solids, total
organic carbon, and chemical oxygen demand. Tables 2-3 and 2-4
together provide a thorough characterization of K103 and K104
wastes.
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Table 2-3 Major Constituent Composition for K103 and K104 Wastes*
Constituent
Water
Aniline
BOAT Constituents
(Other than Aniline)
Total
K103 Waste
Concentration (Wt. Percent)
>94.7
4.3
100.0%
Constituent
Water
Nitrobenzene
BOAT Constituents
(Other than Nitrobenzene)
Total
K104 Waste
Concentration (Wt. Percent)
>98.7
0.3
100.0
* Percent concentrations presented here were determined from best
estimates based on chemical analyses.
Reference: Onsite Engineering Report for E. I. duPont de Nemours,
Beaumont, Texas. Pages 6 and 8.
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Rev. 3
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TABLE 2-4
BOAT CONSTITUENT ANALYSIS AND OTHER DATA
Untreated Waste Conentration Range, pcm*
BOAT ORGAN ICS K103 K104
Volatile
4. Benzene 32-81 4.5 - 320
Semivolatile
56. Aniline 33.000 - 53,000 <150 - <300
101. 2,4-Dinitrophenol <7,500 - <15,000 750 - <1,500
126. Nitrobenzene 1,900 - 2,800** 2,200 - 3,900
142. Phenol 1,500 - <3,000 <150 - <300
BOAT Metals
155. Arsenic 0.01 - 21 <0.01
156. Barium <.001 .0015 - .017
159. Chromium <.007 <-007 - .432
160. Copper <.006 <.006 - .012
161. Lead <-005 - 6 <.020
163. Nickel <.011 <.011 - .238
168. Zinc 3 - 21 <.038 - .079
BOAT Inorganics
169. Total Cyanides <0.010 - 0.075 3.06 - 6.28
171. Sulfide 62 - 89 <1.0
Other Parameters
Total Dissolved Solds + 10,200 - 27,200
Total Suspended Solids 8-24 21-172
Total Organic Carbon 33,500 - 36,300 1,420 - 2,990
Chemical Oxygen Demand 97,800 - 111,000 5,290 - 48,200
* - Values obtained from Onsite Engineering Report of Treatment Technology Performance for E. I. du Pont
de Nemours, Inc., Beaumont, Texas. Tables 6-6 and 6-8.
+ - Total dissolved solids could not be analyzed since the sample flashed before an analysis could be
completed. This was due to the amount of organics contained in the sample.
** - Value represents the treated waste from the aniline liquid/liquid extractor. Nitrobenzene was
used as a solvent in the aniline liquid/liquid extractor.
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2.3 Determination of Waste Treatability Group
Fundamental to waste treatment is the concept that the type
of treatment technology used and the level of treatment achieved
depend on the physical and chemical characteristics of the waste.
In cases where EPA believes that wastes represented by different
codes can be treated to similar concentrations using the same
technologies, the Agency combines the codes into one treatability
group. In particular, the two listed wastes (K103 and K104) from
the production of aniline and nitrobenzene were combined into a
single waste treatability group.
These two wastes are produced in the aniline/nitrobenzene
industry and are frequently treated together in the industry
using a single waste treatment technology. Also, the two wastes
have similar physical and chemical characteristics including:
high water content, high BDAT organic levels (benzene and aniline
or nitrobenzene), relatively low levels of BDAT metals and
inorganics, and low filterable solids content. For these
reasons, the Agency believes that the K103 and K104 wastes
represent a separate waste treatability group.
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3. APPLICABLE/DEMONSTRATED TREATMENT TECHNOLOGIES
The purpose of this section is to describe applicable
treatment technologies for treatment of K103 and K104 wastes that
the Agency has identified as applicable and to describe which of
the applicable technologies the Agency has determined to be
demonstrated. Included in this section are discussions of those
applicable treatment technologies that have been demonstrated on
a commercial basis. The technologies which were considered to be
applicable are those which treat organic compounds by
concentration reduction. Also, this section describes the
performance data available for these technologies.
The previous section described the industry that will be
affected by the land disposal restrictions on K103 and K104
wastes, and presented a characterization of these wastes.
Analysis of the K103 wastewaters indicates that they primarily
consist of water (94.7 percent) and aniline (4.3 percent). The
K104 wastewater primarily consists of water (98.7 percent),
nitrobenzene (0.3 percent) and small amounts of cyanides. The
Agency has identified these treatment technologies which may be
applicable to K103 and K104 because the technologies are designed
to reduce the concentration of organic cojmpounds present in the
untreated waste. The selection of the treatment technologies
applicable for treating organic compounds and cyanides in K103
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and K104 wastewaters is based on information obtained from
engineering site visits and available literature sources.
3.1 Applicable Treatment Technologies
For K103 and K104 wastewaters, the Agency has identified the
following treatment technologies as being applicable:
liquid/liquid (or solvent) extraction which separates the organic
components from the aqueous components by exploiting the relative
differential or selective solubility of the organic constituents
in a particular solvent; steam stripping, which removes organics
from the liquid phase through volatilization; activated carbon
adsorption which uses carbon granules to selectively remove
organic contaminants by adsorption; and biological treatment
which involves the use of microorganisms to degrade organic
compounds.
The use of activated carbon adsorption in treating the
wastewaters generates a spent carbon which is nonwastewater. The
Agency has identified rotary kiln incineration as being an
applicable treatment technology for this nonwastewater form of
K103 and K104.
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3.2 Demonstrated Treatment Technologies
i. Nonwastewaters
The demonstrated technology that the Agency has identified
for treatment of K103 and K104 nonwastewaters is rotary kiln
incineration. This technology has not been commercially
demonstrated for the treatment of K103 and K104 nonwastewaters,
but it has been demonstrated for wastes similar to K103 and K104
nonwastewaters. However, the Agency does not have performance
data for this treatment technology.
ii. Wastewaters
The Agency has determined that all of the applicable
technologies for wastewaters are demonstrated. The demonstrated
treatment technologies listed above for K103 and K104 generally
are combined to form treatment systems or treatment trains which
are more effective than single technologies alone in removing and
recovering organics from wastewater. The three treatment
technology systems which are demonstrated or are currently in
commercial use are as follows:
liguid/liquid extraction followed by steam stripping
and activated carbon adsorption,
steam stripping followed by activated carbon
adsorption, and
steam stripping followed by biological treatment.
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A more detailed discussion of the treatment technology
system for which the Agency has collected performance data is
presented in Sections 3.2.1 through 3.2.3.
3.2.1 Solvent Extraction
Solvent extraction is a treatment technology used to remove
a constituent from a waste by mixing the waste with a solvent
that is immiscible with the waste and in which the waste
constituent of concern is preferentially soluble. Solvent
extraction is commonly called liquid extraction or liquid-liquid
extraction. EPA also uses this term to refer to extraction of
BDAT list organics from a solid waste. When BOAT list metals are
extracted using acids, EPA uses the term acid leaching.
(1) Applicability and Use of Solvent Extraction
Theoretically, solvent extraction has broad applicability in
that it can be used for wastes that have high or low
concentrations of a range of waste characteristics including
total organic carbon, filterable solids, viscosity, and BDAT list
metals content. The key to its use is whether the BDAT
constituents can be extracted from the waste matrix containing
the constituents of concern. For a waste matrix with high
filterable solids this would mean that the solids could be land
disposed following solvent extraction. For a predominately
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liquid waste matrix with low filterable solids, the extracted
liquid (referred to as the raffinate) could be reused. Solvent
extraction can seldom be used without additional treatment
(e.g., incineration) of the extract; however, some industries may
be able to recycle the solvent stream contaminated with the BOAT
constituents back to the process.
(2) Underlying Principles of Operation
For solvent extraction to occur, the BOAT constituents of
concern in the waste stream must be preferentially soluble in the
solvent and the solvent must be essentially immiscible with the
waste stream. In theory, the degree of separation that can be
achieved is provided by the selectivity value; this value is the
ratio of the equilibrium concentration of the constituent in the
solvent to the equilibrium concentration of the constituent in
the waste.
The solvent and waste stream are mixed to allow mass
transfer of the constituent(s) from the waste stream to the
solvent. The solvent and waste stream are then allowed to
separate under quiescent conditions. The solvent solution,
containing the extracted contaminant is called the extract. The
V
extracted waste stream with the contaminants removed is called
the raffinate. The simplest extraction system comprises three
components: (1) the solute, or the contaminant to be extracted;
3-5 Rev. 3
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(2) the solvent; and (3) the nonsolute portion of the waste
stream. For simple extractions, solute passes from the waste
stream to the solvent phase. A density difference exists between
the solvent and waste stream phases. The extract can be either
the heavy phase or the light phase.
(3) Physical Description of a Solvent Extraction Process
The simplest method of extraction is a single stage system.
The solvent and waste stream are brought together; clean effluent
and solvent are recovered without further extraction. The clean
effluent is referred to as the raffinate, and the solvent
containing the constituents that were removed from the waste
stream are known as the extract. The amount of solute extracted
is fixed by equilibrium relations and the quantity of solvent
used. Single stage extraction is the least effective extraction
system.
Another method of extraction is simple multistage contact
extraction. In this system, the total quantity of solvent to be
used is divided into several portions. The waste stream is
contacted with each of these portions of fresh solvent in a
series of successive steps or stages. Raffinate from the first
v
extraction stage is contacted with fresh solvent in a second
stage, and so on.
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In countercurrent, multistage contact, fresh solvent and the
waste stream enter at opposite ends of a series of extraction
stages. Extract and raffinate layers pass continuously and
countercurrently from stage to stage through the system.
In order to achieve a reasonable approximation of phase
equilibrium, solvent extraction requires the intimate contacting
of the phases. Several types of extraction systems are used for
contact and separation; two of these, mixer-settler systems and
column contactors, are discussed below.
i. Mixer-Settler Systems
Mixer-settler systems are comprised of a mixing chamber for
phase dispersion, followed by a settling chamber for phase
separation. The vessels may be either vertical or horizontal.
Dispersion in the mixing chamber occurs by pump circulation,
nonmechanical in-line mixing, air agitation, or mechanical
stirring. In a two-stage mixer-settler system the dispersed
phase separates in a horizontal settler. The extract from the
second settler is recycled to the first settler (see Figure 3-1).
Extract properties such as density or specific constituent
concentration may be monitored to determine when the extract must
be sent to solvent recovery and fresh or regenerated solvent
V
added to the system. Mixer-settler systems can handle solids or
highly viscous liquids. Design scaleup is reliable, and
mixer-settlers can handle difficult dispersion systems. Intense
3-7 Rev. 3
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WASTE,
OJ
00
MIXER
A
RECYCLED SOLVENT FROM
RECOVERY/ FRESH SOLVENT
MAKEUP
RAFFINATE
A
MIXER
(_ _ RAFFINATE
y SOLVENT
RECYCLED
SOLVENT
V
EXTRACT
_ RAFFINATE "\
SOLVENT J
EXTRACT TO RECOVERY
FIGURE 3-1
TWO-STAGE MIXER-SETTLER
EXTRACION SYSTEM
(D
-------
agitation to provide high rates of mass transfer can produce
solvent-feed dispersions that are difficult to separate into
distinct phases.
ii. Column Contactors
Packed and sieve-tray are two different types of column
contactors that do not require mechanical agitation. Figure 3-2
presents schematics of the two types of extraction columns.
A packed extractor contains packing materials, such as
saddles, rings, or structured packings of gauze or mesh. Mass
transfer of the solute to the extract is promoted because of
breakup and distortion of the dispersed phase as it contacts the
packing.
The sieve-tray extractor is similar to a sieve-tray column
used in distillation. Tray perforations result in the formation
of liquid droplets to aid the mass transfer process. The
improved transfer is accomplished by the fact that the droplets
allow for more intimate contact between extract and raffinate.
(4) Waste Characteristics Affecting Performance
In determining whether solvent extraction is likely to
achieve the same level of performance on an untested waste as a
previously tested waste, the Agency will focus on the waste
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SOLVENT-LIQUID
INTERFACE
SOLVENT
WASTE
RAFFINATE
RAFFINATE
SOLVENT
. PACKING
SUPPORT/
REDISTRIBUTER
PACKING
SUPPORT
jjr--^^r —
---•=]
_ ^^ , ____
EXTRACT
SOLVENT-LIQUID
' INTERFACE
DOMNCOHER
WASTE
EXTRACT
A. PACKED
EXTRACTOR
B.SIEVE TRAY
EXTRACTOR
FIGURE 3-2
EXTRACTION COLUMNS WITH
NONMECHANICAL AGITATION
(D
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characteristics that provide an estimate of the selectivity value
previously described. EPA believes that the selectivity value
can best be estimated by analytically measuring the partitioning
coefficients of the waste constituents of concern and the
solubility of the waste matrix in the extraction solvent.
Accordingly, EPA will use partitioning coefficients and
solubility of the waste matrix as surrogates for the selectivity
value in making decisions regarding transfer of treatment
standards.
For the liquid/liquid extraction system, the WCAPs are the
relative solubilities which is a measure of the partitioning
coefficient, of the various waste constituents in water and in
nitrobenzene. The primary organic constituents of K103 and K104
(benzene, aniline, nitrobenzene, phenol, and 2,4-dinitrophenol),
along with cyanides, are all soluble in nitrobenzene at 40°C.
Phenol and cyanides are soluble in water at 40°C, while benzene,
aniline, and nitrobenzene are relatively insoluble in water
(0.137 g/100 g H2Osaturated solution at 54.5°C). It should also
be noted that the density of nitrobenzene relative to water is
1.205 at 4°C.
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(5) Design and Operating Parameters
EPA's analysis of whether a solvent extraction system is
well designed will focus on whether the BDAT list constituents
are likely to be effectively separated from the waste. The
particular design and operating parameters to be evaluated are:
(1) the selection of a solvent, (2) equilibrium data, (3)
temperature and pH, (4) mixing, and (5) settling time.
(1) The selection of a solvent. In assessing the design of
a solvent extraction system, the most important aspect to
evaluate is the solvent used and the basis on which the
particular solvent was selected. Solvent selection is important
because, as indicated previously, different waste constituents of
concern will have different solubilities in various solvents, and
it is the extent to which the waste constituents
are preferentially soluble in the selected solvent that
determines the effectiveness of this technology. In addition to
this information, EPA would also want to review any empirical
extraction data used to design the system.
(2) Equilibrium Data. For solvent extraction systems that
are operated in a continuous mode, the extraction process will
generally be conducted using a series of equilibrium stages as
discussed previously. The number of equilibrium stages and the
associated flow rates of the waste and solvent will be based on
3-12 Rev. 3
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empirical equilibrium data. EPA will evaluate these data as part
of assessing the design of the system.
(3) Temperature and pH. Temperature and pH changes can
affect equilibrium conditions and, consequently, the performance
of the extraction system. Thus, EPA would attempt to monitor and
record these values on a continuous basis.
(4) Mixing. For mixer-settler type extraction processes,
mixing determines the amount of contact between the two
immiscible phases and, accordingly, the degree of mass transfer
of the constituents to be extracted. EPA would thus want to know
the type of mixers used and the basis for determining that this
system would provide sufficient mixing.
(5) Settling Time. For batch systems, adequate settling
time must be allowed to ensure that separation of the phases has
been completed. Accordingly, in assessing the design of a
system, EPA would want to know settling time allowed and the
basis for selection.
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3.2.2 Steam Stripping
Steam stripping is a technology which can separate more
volatile materials from less volatile materials by a process of
vaporization and condensation. As such, it is a type of
distillation process.
(1) Applicability and Use of Technology
Steam stripping is applicable to wastewaters that contain BOAT
organics that are sufficiently volatile such that they can be
removed by the application of steam. Waste parameters affecting
treatment selection are filterable solids, total organic carbon
(TOC), and the presence of BDAT organics that are either not
volatile or only minimally volatile.
(2) Underlying Principles of Operation
The basic principle of operation for steam stripping is the
volatilization of hazardous constituents through the application
of heat. The constituents that are volatilized are then
condensed and either reused or further treated by liquid
injection incineration.
An integral part of the theory of steam stripping is the
principle of vapor-liquid equilibrium. When a liquid mixture of
two or more components is heated, a vapor phase is created above
3-14 Rev. 3
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the liquid phase. The vapor phase will be more concentrated in
the constituents having the higher vapor pressure. If the vapor
phase above the liquid phase is cooled to yield a condensate, a
partial separation of the components results. The degree of
separation would depend on the relative differences in the vapor
pressures of the constituents; the larger the difference in the
vapor pressure, the easier the separation can be accomplished.
If the difference between the vapor pressure is extremely
large, a single separation cycle or single equilibrium stage of
vaporization and condensation may achieve a significant
separation of the constituents. If the difference between the
vapor pressures are small, then multiple equilibrium stages are
needed to achieve effective separation. In practice, the
multiple equilibrium stages are obtained by stacking trays or
placing packing into a column. The vapor phase from a tray rises
to the tray above it and the liquid phase falls to the tray below
it. Essentially, each tray represents one equilibrium stage. In
a packed steam stripping column, the individual equilibrium
stages are not discernible, but the number of equivalent trays
can be calculated from mathematical relationships.
The vapor liquid equilibrium is expressed as relative
volatility or the ratio of the vapor to liquid concentration for
a constituent divided by the ratio of the vapor to liquid
concentration of the other constituent. The relative volatility
3-15 Rev. 3
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is a direct measure of the ease of separation. If the numerical
value is 1, then separation is impossible because the
constituents have the same concentrations in the vapor and liquid
phases. Separation becomes easier as the value of the relative
volatility becomes increasingly greater than unity.
(3) Physical Description of the Process
A steam stripping unit consists of a boiler, a stripping
section, a condenser, and a collection tank as shown by Figure
3-3. The boiler provides the heat required to vaporize the
liquid fraction of the waste. The stripping section is composed
of a set of trays or packing in a vertical column. The feed
enters at the top.
The stripping process uses multiple equilibrium stages, with
the initial waste mixture entering the uppermost equilibrium
stage. The boiler is located below the lowermost equilibrium
stage so that vapor generated moves upward in the column coming
into contact with the falling liquid. As the vapor comes into
contact with the liquid at each stage, the more volatile
components are removed or "stripped" from the liquid by the vapor
phase. The concentration of the emerging vapor is slightly
V
enriched (as it is in equilibrium with the incoming liquid), and
the liquid exiting the bottom of the boiler ("bottoms") is
considerably enriched in the lower vapor pressure constituent(s).
3-16 Rev. 3
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HASTE
INFLUENT
TREATED
EFFLUENT
VENT OF
NON-CONDENSED VAPORS
A
CONDENSER
RECIEVER
RECOVERED
SOLVENT FOR
REUSE OR
TREATMENT
FIGURE 3-3
STEAM STRIPPING
3-17
Rev. 3
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The process of stripping is very effective for wastewaters where
the relative volatilities are large between the organics of
concern and wastewater. Steam stripping is used to strip the
organic volatiles from wastewater. The water effluent from the
bottom of the stripper is reduced in organic content, but in some
circumstances may require additional treatment, such as carbon
adsorption or biological treatment. The steam and organic vapors
leaving the top of the column are condensed. Organics in the
condensate that form a separate phase in water usually can be
separated and recovered or disposed of in a liquid injection
incinerator. After separation the aqueous condensate is usually
recycled to the stripper.
(4) Waste Characteristics Affecting Performance
In determining whether steam stripping is likely to achieve
the same level of performance on an untested waste as a
previously tested waste, EPA will focus on the following
characteristics: boiling point, total dissolved solids, total
dissolved volatile solids, and oil and grease. EPA recognizes
these characteristics have some limitations in assessing transfer
of performance; nevertheless, the Agency believes that they
provide the best possible indicator of the preferred waste
characteristic analysis, i.e., relative volatility. Below is a
discussion of relative volatility, as well as, EPA's rationale
for evaluating the above described waste characteristics in
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determining transfer of treatment performance.
As discussed earlier, the term relative volatility ( oC )
refers to the ease with which a substance present in a solid or
liquid waste will vaporize from that waste upon application of
heat from an external source. Hence, it bears a relationship to
the equilibrium vapor pressure of the substance.
For an ideal binary mixture, the relative volatility ( o( ) is
expressed as:
fi Iiffi
K. -Y.X.
where K. and K. are equilibrium concentrations for components i
and j respectively, Y is the mole fraction of the component in
the vapor and X is the mole fraction of the component in the
liquid.
The term "ideal" refers to whether the vapor pressures of the
two components can be linearly related to their respective
compositions in the liquid phase; this,, is known as Raoult's
law. In general, binary solutions at low pressures follow
this law and are, therefore, "ideal"; most mixtures do not.
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For non- ideal binary mixtures, the relative volatility (
-------
point alone would not account for any non-ideal behavior of the
solution. Accordingly, EPA will examine the concentrations of
oil and grease, total dissolved solids, and total dissolved
volatile solids. All of these characteristics affect the partial
pressures of the individual organic constituents of concern as
well as the solubility. Accordingly, these characteristics will
affect relative volatility of a constituent and, hence, the
ability of the constituent to be treated using steam stripping.
The WCAPs for the steam stripper are the vapor pressures of
the various constituents in the waste. The higher the vapor
pressure, the more easily stripped. At 40°C, benzene has a vapor
pressure of 182.7 mm Hg, aniline has a vapor pressure of 2.90 mm
Hg, and phenol has a vapor pressure of 2.02 mm Hg. Nitrobenzene
has a vapor pressure of 1 mm Hg at 44.4°C, and 2,4-dinitrophenol
has a vapor pressure of 1 mm Hg at 49.3°C. The cyanides present
are primarily solid salts, and hence have low vapor pressures or
decompose upon heating. There are no known azeotropes among the
constituents of these wastes, and there is no known
polymerization potential upon heating these wastes.
(5) Design and Operating Parameters
*>
EPA's analysis of whether a steam stripping system is well
designed will focus on the degree of separation the system is
designed to achieve and the controls installed to maintain the
3-21 Rev. 3
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proper operating conditions. The specific parameters are
presented below.
(1) Treated and Untreated Concentrations. In determining
whether to sample a particular steam stripper as a candidate for
BOAT, EPA will pay close attention to the treated design
concentration of the unit to ensure that it is consistent with
best demonstrated practice. This evaluation is important in that
a treatment system will usually not perform its design. The
various untreated waste characteristics that affect performance
are important to know, because operation of the system with
untreated waste concentrations in excess of initial design
conditions can easily result in poor performance of the treatment
unit. In evaluating the performance of a steam stripper, EPA
would want data on the untreated waste characteristics to ensure
that they conformed with design specifications.
(2) Vapor-Liquid Equilibrium Data. The vapor liquid
equilibrium data are determined in laboratory tests unless
already available. The use of these data are required for
several reasons. First, they are used to calculate the number of
theoretical stages required to achieve the desire separation.
Using the theoretical number of stages, the actual number of
V
stages can then be determined through the use of empirical tray
efficiency data supplied by an equipment manufacturer.
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Secondly, the vapor liquid equilibrium data are used to
determine the liquid and vapor flow rates that ensure sufficient
contact between the liquid and vapor streams. These rates are,
in turn, used to determine the column diameter.
(3) Column Temperature and Pressure. These parameters are
integrally related to the vapor liquid equilibrium conditions.
Column temperature design include performing a heat balance
around the steam stripping unit, accounting for the heat removed
in the condenser, heat input in the feed, heat input from steam
injectors and heat loss from the column. Column pressure
influences the boiling point of the liquid. For example, the
column temperature required to achieve the desired separation can
be reduced by operating the system under vacuum. During
treatment, it is important to continuously monitor these
parameters to ensure that the system is operated at design
conditions.
(4) Column Internals. Column internals are designed to
accommodate the physical and chemical properties of the
wastewater to be stripped. Two types of internals may be used in
steam stripping: trays or packing. Tray types include bubble
cap, sieve, valve and turbo-grid. Trays have several advantages
over packing. Trays are less susceptible to blockage by solids,
they have a lower capital cost for large diameter columns
(greater than or equal to 3 feet), and they accommodate a wider
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range of liquid and vapor flow rates. Compared to trays, packing
has the advantages of having a lower pressure drop per
theoretical stage, being more resistant to corrosive materials,
having a lower capital cost for small diameter column (less than
3 feet), and finally being less susceptible to foaming because of
a more uniform flow distribution.
3.2.3 Carbon Adsorption
Adsorption with activated carbon is an important separation
method for removing organics and some other dissolved materials
from liquids. It occurs when the surface of the activated carbon
attracts the ions or molecules of the organic or dissolved solid
to form a layer on the carbon surface and accumulate in its
pores.
(1) Applicability and Use of Technology
Activated carbon treatment is used to remove dissolved
organic pollutants from aqueous streams. To a lesser extent it
also is used to remove dissolved heavy metal and other inorganic
contaminants. Inorganics are usually not very adsorbable, but
there are some exceptions (e.g., molybdates, gold chloride,
mercuric chloride, silver salts and iodine). The most effective
metals removal occurs with metal/inorganic complexes, or metal
organic complexes.
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Activated carbon treatment is not selective in the organic
contaminants it will remove. Hence, all organics will compete
for system capacity, including organics that are not necessary to
remove. In some systems (downflow granular activated carbon
beds), suspended solids over 50 mg/1 cannot be tolerated and must
be removed prior to activated carbon treatment. Activated carbon
is frequently applied as a final polishing mechanism following
other treatment technologies (e.g., biological treatment).
These waste component separations most commonly occur in
industries manufacturing organic chemicals, inorganic chemicals,
dyes and pigments, insecticides, refineries, textiles,
explosives, food, tobacco, leather, primary metals, fabricated
metals, Pharmaceuticals, and plastics.
(2) Underlying Principles of Operation
Activated carbon treatment is an application of the
principle of adsorption. Adsorption is the mass transfer of a
molecule from a liquid or gas into a solid surface.
Activated carbon is manufactured in such a way as to produce
extremely porous carbon particles, whose internal surface area is
V
very large (500 to 1400 square meters per gram of carbon). This
porous structure, through chemical and physical forces, attracts
and holds (adsorbs) organic molecules as well as certain
3-25 Rev. 3
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inorganic molecules. It is not unusual for activated carbon to
adsorb from aqueous solution 0.15 grams of an organic contaminant
per gram of carbon, though 0.10 gram/gram is probably a more
realistic general estimate. The principal factor that affects
carbon adsorption is the chemical affinity between the carbon and
the organic compound. Other characteristics such as solubility,
temperature, pH, type of activated carbon used and presence of
other organics also influence the effectiveness of carbon
adsorption.
The effectiveness of adsorption generally improves with
increasing contact time. Exceptions to this rule include
chemical compounds that are not preferentially adsorbed onto the
carbon surface. These compounds can be adsorbed from adsorption
sites in favor of compounds that have a higher affinity for the
carbon over a longer contact time.
Once the contaminants/impurities have been removed from the
waste stream onto the carbon, two options are available. The
activated carbon can be (1) disposed of by approved methods
(usually incineration) or (2) regenerated by thermal or chemical
methods for further use.
V
There is a loss of performance with each regeneration step;
therefore, the activity is never restored to its original level.
The number of times that the carbon can be regenerated is
3-26 Rev. 3
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determined by the extent of physical erosion and the loss of
adsorptive capacity. Isotherm tests on the regenerated carbon
can be used to determine adsorptive capacity, thereby aiding in
the prediction of the number of times the carbon can be
regenerated.
(3) Waste Characteristics Affecting Performance
The waste characteristics that will affect an activated
carbon system's performance are as follows: (i) type of organic
contaminants, (ii) concentration of contaminants, and (iii)
suspended solids, grease and oil concentration.
At first, it might appear that pH and temperature would be
significant factors that would affect adsorption. Polarity of
some organic compounds are affected by pH, and polarity changes
influence adsorption. Particularly with heavy metals, the
activated carbon must have the proper pH to achieve satisfactory
removal. Temperature becomes a significant factor when they
become high enough to desorb contaminants from activated carbon
(usually over 100°C). However, these factors are considered to
be easily controlled during the actual process and, as such, are
not major hindrances to efficient adsorption.
3-27 Rev. 3
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i. Type of Organic Contaminants
All organic molecules can be adsorbed by activated carbon to
some degree. Generally, adsorption will increase with molecular
weight until the particle size becomes too large for carbon pore
size. However, the activated carbon usually has a greater
affinity for aromatic compounds than straight chain compounds.
Nonpolar compounds are usually easily adsorbed, whereas polar
ones are not. Halogenated organic compounds (HOCs), if aromatic
(such as PCBs), are readily adsorbed. Finally, it has been
demonstrated in practice that adsorption will increase with
decreasing solubility.
For the carbon adsorption system, the WCAPs are the
molecular weights of the constituents present. The molecular
weights of the major constituents in the waste are as follows:
78.12 for benzene, 123.11 for nitrobenzene, 93.13 for aniline,
94.11 for phenol, and 184.11 for 2,4-dinitrophenol. The cyanides
present are thought to be a mixture of complex organic and
inorganic cyanide compounds, and therefore the molecular weight
cannot be determined. Other important characteristics of the
waste for the carbon adsorption unit are the total organic carbon
content (which is 444 mg/1) and the total suspended solids
content (which is 196 mg/1). The amount of oil and grease in the
waste is not known.
3-28 Rev. 3
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ii. Concentration of Contaminants
In actual practice this process becomes ineffective at
concentrations exceeding a few thousand mg/1. The carbon will
adsorb concentrated contaminants so fast that carbon consumption
will become excessive, and frequent disposal and/or regeneration
of carbon is likely to become a greater problem than removal of
the organic materials from the waste stream. For excessively
concentrated waste streams, other organic compound destruction
techniques would probably be more appropriated (e.g.,
incineration or reuse as a fuel).
iii. Suspended Solids and Grease and Oil Concentration
In powdered activated carbon (PAC) systems, suspended solids
and grease concentrations in the wastewater stream have no
effect, since they are removed from the waste along with the
spent PAC. However, in nonfluidized granular activated carbon
(GAG) systems (see Section 4.4 for a description of these
systems), the column of GAC acts as a filter for suspended
particles and greases. It will eventually become plugged or
binded with solids, or coated with grease and oils, and not be
able to sustain the flow of wastewater. Consequently, the more
suspended solids or grease and oils in the GAC column influent,
the sooner it must be backwashed, hence slowing the dissolved
organic compound removal rate.
3-29 Rev. 3
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(4) Physical Description of the Process
Specific designs will depend on the waste stream to be
treated and the type of end product desired. However, a few
examples will provide some idea of how these systems work.
i. Systems using PAC. PAC can be easily used in exiting
equipment such as tanks, filtration or settling apparatus. Since
it is a fine powder, it is usually put directly into the waste
stream. It needs lower contact times than GAC because it adsorbs
contaminants more quickly. PAC usually has less adsorption
capacity than GAC, so more is required. A few treatment systems
are described below.
(a) Batch system. The incoming waste stream is
thoroughly stirred with the PAC, usually with some type of
mechanical agitator. The stirring time (contact time) is usually
20 to 30 minutes in most cases. After adsorption equilibrium is
reached, the mixture is settled and/or filtered to separate the
PAC from the wastewater. This procedure can be separated to
increase filtrate clarity.
(b) Continuous system. In a continuous system both the
waste liquid and carbon slurry enter mixing tanks simultaneously
and continuously. Continuous settling and/or filtration again
follow the mixing.
3-30 Rev. 3
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ii. Systems using GAG. In GAG systems the carbon is packed
in columns and the liquid is passed through a bed of the carbon.
The liquid flow can be either up or down through the vertical
column. Figure 3-4 shows some common systems.
Typically, the wastewater to be treated is passed downward
through a stationary bed of carbon. The constituent to be
removed is adsorbed most rapidly and effectively by the upper few
layers of fresh carbon during the initial stages of operation.
These upper layers are in contact with the wastewater at its
highest concentration level. The small amounts of target
constituent that escape adsorption in the first few layers of the
activated carbon are removed from solution in the lower or
downstream portion of the bed. Initially, none of the
constituent to be removed escapes form the adsorbent.
As the liquid flows down the column, the adsorption capacity
is reached in the top layers, the adsorption zone starts moving
down the column. As the adsorption zone moves near the end of
the bed, the concentration in the effluent rapidly approaches the
influent concentration. This point in the operation is referred
to as breakthrough. A breakthrough curve (Figure 3-5) is the
plot of the ratio of effluent to influent concentrations versus
V
time of operation. At breakthrough the bed is exhausted and
little additional removal of the constituent will occur. At this
point, the carbon must be replaced or regenerated.
3-31 Rev. 3
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IN
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FIGURE 3-4 TYPICAL COLUMN CONFIGURATIONS
3-32
Rev. 3
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e '
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(5) Design and Operating Parameters
Design Parameters
The system design must account for three parameters that
affect the ability of activated carbon to adsorb contaminants: i)
contact time, ii) carbon particle type and size, and iii)
wastewater flow rate.
i. Contact time. For both PAC/GAC systems, contact time
must be determined by testing individual wastes with different
activated carbon samples. Once contact time is determine for
adequate removal of contaminants, tank sizing is the next step
and it will depend on waste flow rate.
ii. Carbon particle type and size. Activated carbon is
made from a variety of substances (e.g., coal, wood), ground to
many different sizes, and manufactured with "customized" pore
sizes. A range of surface areas and individual pore sizes will
determine the carbon's adsorptive capacity. Bench testing is
recommended to determine the most effective activated carbon
product for a particular waste stream and desired effluent.
iii. Wastewater flow rate. GAG systems are designed for
upflow or downflow operation. For both types, there are
practical limits to the liquid velocity. Once the velocity and
3-34 Rev. 3
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contact time are determined, the bed cross-section and depth are
sized to meet these requirements.
Operating Parameters
A number of parameters must be maintained during operation
to ensure that the adsorption system adheres to the design
specifications. These are: (i) waste liquid concentration, (ii)
suspended oils and solids, and (iii) contact time.
i. Waste liquid concentration. In GAG systems, the
concentration has a direct effect on the operation of an
adsorption system because if the concentration is significantly
higher than the design concentration, column breakthrough will
occur quickly and excessive regeneration will be required.
Conversely, if, during the operation of a column, the waste
liquid concentration decreases significantly, previously adsorbed
molecules can be desorbed from the carbon and be discharged in
the effluent stream. Additionally, changes in the waste
composition can cause previously adsorbed molecules to be
desorbed and replaced by molecules of a different constituent if
the new constituent has a higher affinity for the carbon surface.
These types of situations can lead to effluent concentrations for
V
a particular waste constituent that are higher than influent
concentrations. Waste liquid concentration has a lesser effect
on PAC systems because the PAC is removed as it is spent.
3-35 Rev. 3
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Desorption is not a problem. However, if the concentration
increases significantly over the design concentrations, excessive
quantities of PAC may be required. In any case, the effluent
must be monitored for breakthrough of contaminants.
ii- Suspended oils and solids. Suspended oils and solids
are not usually a problem with PAC systems. However, in GAC
systems, oils and suspended solids in the waste will eventually
plug the column. If the concentration of solids is significant
(typically greater than 200 mg/1), the waste will need to be
pretreated to remove them. In any case, suspended solids and
greases present in the GAC column influent will necessitate
backwashing and/or column cleaning. The need for such cleaning
can be detected with pressure gauges which monitor the degree of
plugging.
iii. Contact time. Contact time requirements vary with the
type of system but must be maintained within design
specifications. Typical contact times vary between 300 and 100
minutes for GAC systems, and are somewhat lower for PAC systems.
For GAC systems, typical downflow rates are between 20 and 330
1/min m2 of bed area. A typical upflow rate is 610 1/min m2 of
bed area, unless the bed is fluidized in which case higher
V
velocities are necessary. Contact time is monitored by measuring
wastewater flow rate, since system volume is predetermined.
3-36 Rev. 3
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3.2.4 Incineration
This section addresses the commonly used incineration
technologies: Liquid injection, rotary kiln, fluidized bed
incineration, and fixed hearth. A discussion is provided
regarding the applicability of these technologies, the underlying
principles of operation, a technology description, waste
characteristics that affect performance, and finally important
design and operating parameters. As appropriate the subsections
are divided by type of incineration unit.
(1) Applicability and Use of this Technology
i. Liquid Injection
Liquid injection is applicable to wastes that have viscosity
values sufficiently low so that the waste can be atomized in the
combustion chamber. A range of literature maximum viscosity
values are reported with the low being 100 SSU and the high being
10,000 SSU. It is important to note that viscosity is
temperature dependent so that while liquid injection may not be
applicable to a waste at ambient conditions, it may be applicable
when the waste is heated. Other factors that affect the use of
liquid injection are particle size and the presence of suspended
solids. Both of these waste parameters can cause plugging of the
burner nozzle.
3-37 Rev. 3
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ii. Rotary Kiln/ Fluidized Bed/ Fixed Hearth
These incineration technologies are applicable to a wide
range of hazardous wastes. They can be used on wastes that
contain high or low total organic content, high or low filterable
solids, various viscosity ranges, and a range of other waste
parameters. EPA has not found these technologies to be
demonstrated on wastes that are comprised essentially of metals
with low organic concentrations. In addition, the Agency expects
that some of the high metal content wastes may not be compatible
with existing and future air emission limits without emission
controls far more extensive than currently practiced.
(2) Underlying Principles of Operation
i. Liquid Injection
The basic operating principle of this incineration
technology is that incoming liquid wastes are volatilized and
then additional heat is supplied to the waste to destabilize the
chemical bonds. Once the chemical bonds are broken, these
constituents react with oxygen to form carbon dioxide and water
vapor. The energy needed to destabilize the bonds is referred to
as the energy of activation.
ii. Rotary Kiln and Fixed Hearth
There are two distinct principles of operation for these
incineration technologies, one for each of the chambers involved.
3-38 Rev. 3
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In the primary chamber, energy, in the form of heat, is
transferred to the waste to achieve volatilization of the various
organic waste constituents. During this volatilization process
some of the organic constituents will oxidize to CO and water
vapor. In the secondary chamber, additional heat is supplied to
overcome the energy requirements needed to destabilize the
chemical bonds and allow the constituents to react with excess
oxygen to form carbon dioxide and water vapor. The principle of
operation for the secondary chamber is similar to liquid
injection.
iii. Fluidized Bed
The principle of operation for this incinerator technology
is somewhat different than for rotary kiln and fixed hearth
incineration relative to the functions of the primary and
secondary chambers. In fluidized bed, the purpose of the primary
chamber is not only to volatilize the wastes but also to
essentially combust the waste. Destruction of the waste organics
can be accomplished to a better degree in the primary chamber of
this technology than for rotary kiln and fixed hearth because of
1) improved heat transfer from fluidization of the waste using
forced air and 2) the fact that the fluidization process provides
sufficient oxygen and turbulence to convert the organics to
V
carbon dioxide and water vapor. The secondary chamber (referred
to as the freeboard) generally does not have an afterburner;
however, additional time is provided for conversion of the
3-39 Rev. 3
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organic constituents to carbon dioxide, water vapor, and
hydrochloric acid if chlorine is present in the waste.
(3) Description of Incineration Technologies
i. Liquid Injection
The liquid injection system is capable of incinerating a
wide range of gases and liquids. The combustion system has a
simple design with virtually no moving parts. A burner or nozzle
atomizes the liquid waste and injects it into the combustion
chamber where it burns in the presence of air or oxygen. A
forced draft system supplies the combustion chamber with air to
provide oxygen for combustion and turbulence for mixing. The
combustion chamber is usually a cylinder lined with refractory
(i.e., heat resistant) brick and can be fired horizontally,
vertically upward, or vertically downward. Figure 3-6
illustrates a liquid injection incineration system.
ii. Rotary Kiln
A rotary kiln is a slowly rotating, refractory-lined
cylinder that is mounted at a slight incline from the horizontal
(see Figure 3-7). Solid wastes enter at the high end of the
kiln, and liquid or gaseous wastes enter through atomizing
nozzles in the kiln or afterburner section. Rotation of the kiln
exposes the solids to the heat, vaporizes them, and allows them
to combust by mixing with air. The rotation also causes the ash
to move to the lower end of the kiln where it can be removed.
3-40 Rev. 3
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WATER
AUXILIARY-
FUEL
BURNER
I
it*
LIQUID OR
GASEOUS
WASTE
INJECTION
BURNER
PRIMARY
COMBUSTION
CHAMBER
AETERBURNER
(SECONDARY
COMBUSTION
CHAMBER)
ASH
SPRAY
CHAMBER
T
GAS TO AIR
POLLUTION
CONTROL
HORIZONTALLY FIRED
LIQUID INJECTION
INCINERATOR
WATER
(D
FIGURE 3-6
LIQUID INJECTION INCINERATOR
-------
GAS TO
AIR POLLUTION
CONTROL
AUXILIARY
FUEL
SOLID WASTE
INFLUENT
FEED
MECHANISM
AFTERBURNER
COMBUSTION
GASES
LIQUID OR
GASEOUS
WASTE INJECTION
ASH
FIGURE 3-7 ROTARY KILN INCINERATOR
3-42
Rev. 3
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Rotary kiln systems usually have a secondary combustion chamber
or afterburner following the kiln for further combustion of the
volatilized components of solid wastes.
iii. Fluidized Bed
A fluidized bed incinerator consists of a column containing
inert particles such as sand which is referred to as the bed.
Air, driven by a blower, enters the bottom of the bed to fluidize
the sand. Air passage through the bed promotes rapid and uniform
mixing of the injected waste material within the fluidized bed.
The fluidized bed has an extremely high heat capacity
(approximately three times that of flue gas at the same
temperature), thereby providing a large heat reservoir. The
injected waste reaches ignition temperature quickly and transfers
the heat of combustion back to the bed. Continued bed agitation
by the fluidizing air allows larger particles to remain suspended
in the combustion zone. (See Figure 3-8).
iv. Fixed Hearth Incineration
Fixed hearth incinerators, also called controlled air or
starved air incinerators, are another major technology used for
hazardous waste incineration. Fixed hearth incineration is a
two-stage combustion process (see Figure 3-9). Waste is ram-fed
*•
into the first stage, or primary chamber, and burned at less than
stoichiometric conditions. The resultant smoke and pyrolysis
products, consisting primarily of volatile hydrocarbons and
3-43 Rev. 3
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WASTE
INJECTION
FREEBOARD
GAS TO AIR
POLLUTION
CONTROL
MAKE-UP
SAND
AIR
ASH
FIGURE 3-8
FLUIDIZED BED INCINERATOR
3-44
Rev. 3
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AIR
GAS TO AIR
POLLUTION
CONTROL
AIR
u>
*fc
in
WASTE
INJECTION
BURNER
PRIMARY
COMBUSTION
CHAMBER
GRATE
SECONDARY
COMBUSTION
CHAMBER
t
AUXILIARY
EUEL
2 - STAGE EIXED HEARTH
INCINERATOR
ASH
o>
FIGURE 3-9 FIXED HEARTH INCINERATOR
-------
carbon monoxide, along with the normal products of combustion,
pass to the secondary chamber. Here, additional air is injected
to complete the combustion. This two-stage process generally
yields low stack particulate and carbon monoxide (CO) emissions.
The primary chamber combustion reactions and combustion gas are
maintained at low levels by the starved air conditions so that
particulate entrainment and carryover are minimized.
v. Air Pollution Controls
Following incineration of hazardous wastes, combustion gases
are generally further treated in an air pollution control system.
The presence of chlorine or other halogens in the waste requires
a scrubbing or absorption step to remover HC1 and other
halo-acids from the combustion gases. Ash in the waste is not
destroyed in the combustion process. Depending on its
composition, ash will either exit as bottom ash, at the discharge
end of a kiln or hearth for example, or as particulate matter
(fly ash) suspended in the combustion gas stream. Particulate
emissions from most hazardous waste combustion systems generally
have particle diameters less than one micron and require high
efficiency collection devices to minimize air emissions. In
addition, scrubber systems provide additional buffer against
accidental releases of incompletely destroyed waste products due
*
to poor combustion efficiency or combustion upsets, such as flame
outs.
3-46 Rev. 3
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(4) Waste Characteristics Affecting Performance (WCAP)
i. Liquid Injection
In determining whether liquid injection is likely to achieve
the same level of performance on an untested waste as a
previously tested waste, the Agency will compare dissociation
bond energies of the constituents in the untested and tested
waste. This parameter is being used as a surrogate indicator of
activation energy which, as discussed previously, destabilizes
molecular bonds. In theory, the bond dissociation energy would
be equal to the activation energy; however, in practice this is
not always the case.Other energy effects (e.g., vibrational, the
formation of intermediates, and interactions between different
molecular bonds) may have a significant influence on activation
energy.
Because of the shortcomings of bond energies in estimating
activation energy, EPA analyzed other waste characteristic
parameters to determine if these parameters would provide a
better basis for transferring treatment standards from an
untested waste to a tested waste. These parameters include heat
of combustion, heat of formation, use of available kinetic data
to predict activation energies, and general structural class.
All of these were rejected for reasons provided below.
3-47 Rev. 3
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The heat of combustion only measures the difference in
energy of the products and reactants; it does not provide
information on the transition state (i.e., the energy input
needed to initiate the reaction). Heat of formation is used as a
predictive tool for whether reactions are likely to proceed;
however, there are a significant number of hazardous constituents
for which these data are not available. Use of kinetic data were
rejected because these data are limited and could not be used to
calculate free energy values (A G) for the wide range of
hazardous constituents to be addressed by this rule. Finally,
EPA decided not to use structural classes because the Agency
believes that evaluation of bond dissociation energies allows for
a more direct determination of whether a constituent will be
destabilized.
ii. Rotary Kiln/Fluidized Bed/Fixed Hearth
Unlike liquid injection, these incineration technologies
also generate a residual ash. Accordingly, in determining
whether these technologies are likely to achieve the same level
of performance on an untested waste as a previously tested waste,
EPA would need to examine the waste characteristics that affect
volatilization of organics from the waste, as well as,
destruction of the organics, once volatilized. Relative to
volatilization, EPA will examine thermal conductivity of the
entire waste and boiling point of the various constituents. As
with liquid injection, EPA will examine bond energies in
3-48 Rev. 3
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determining whether treatment standards for scrubber water
residuals can be transferred from a tested waste to an untested
waste. Below is a discussion of how EPA arrived at thermal
conductivity and boiling point as the best method to assess
volatilization of organics from the waste; the discussion
relative to bond energies is the same for these technologies as
for liquid injection and will not be repeated here.
Thermal Conductivity
Consistent with the underlying principles of incineration, a
major factor with regard to whether a particular constituent will
volatilize is the transfer of heat through the waste. In the
case of rotary kiln, fluidized bed, and fixed hearth
incineration, heat is transferred through the waste by three
mechanisms: radiation, convection, and conduction. For a given
incinerator, heat transferred through various wastes by radiation
is more a function of the design and type of incinerator than the
waste being treated. Accordingly, the type of waste treated will
have a minimal impact on the amount of heat transferred by
radiation. With regard to convection, EPA also believes that the
type of heat transfer will generally be more a function of the
type and design of incinerator than the waste itself. However,
EPA is examining particle size as a waste characteristic that may
significantly impact the amount of heat transferred to a waste by
convection and thus impact volatilization of the various organic
3-49 Rev. 3
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compounds. The final type of heat transfer, conduction, is the
one that EPA believes will have the greatest impact on
volatilization of organic constituents. To measure this
characteristic, EPA will use thermal conductivity; an explanation
of this parameter, as well as, how it can be measured is provided
below.
Heat flow by conduction is proportional to the temperature
gradient across the material. The proportionality constant is a
property of the material and referred to as the thermal
conductivity. (Note: The analytical method that EPA has
identified for measurement of thermal conductivity is named
"Guarded, Comparative, Longitudinal Heat Flow Technique"; it is
described in Appendix F.) In theory, thermal conductivity would
always provide a good indication of whether a constituent in an
untested waste would be treated to the same extent in the primary
incinerator chamber as the same constituent in a previously
tested waste.
In practice, thermal conductivity has some limitations in
assessing the transferability of treatment standards; however,
EPA has not identified a parameter that can provide a better
indication of heat transfer characteristics of a waste. Below is
a discussion of both the limitations associated with thermal
conductivity, as well as other parameters considered.
3-50 Rev. 3
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Thermal conductivity measurements, as part of a treatability
comparison for two different wastes through a single incinerator,
are most meaningful when applied to wastes that are homogeneous
(i.e., major constituents are essentially the same). As wastes
exhibit greater degrees of non-homogeneity (e.g., significant
concentration of metals in soil), then thermal conductivity
becomes less accurate in predicting treatability because the
measurement essentially reflects heat flow through regions having
the greatest conductivity (i.e., the path of least resistance)
and not heat flow through all parts of the waste.
BTU value, specific heat, and ash content were also
considered for predicting heat transfer characteristics. These
parameters can no better account for non-homogeneity than thermal
conductivity; additionally, they are not directly related to heat
transfer characteristics. Therefore, these parameters do not
provide a better indication of heat transfer that will occur in
any specific waste.
Boiling Point
Once heat is transferred to a constituent within a waste,
then removal of this constituent from the waste will depend on
its volatility. As a surrogate of volatility, EPA is using
V
boiling point of the constituent. Compounds with lower boiling
points have higher vapor pressures and, therefore, would be more
likely to vaporize. The Agency recognizes that this parameter
3-51 Rev. 3
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does not take into consideration the impact of other compounds in
the waste on the boiling point of a constituent in a mixture;
however, the Agency is not aware of a better measure of
volatility that can easily be determined.
(5) Incineration Design and Operating Parameters
i. Liquid Injection
For a liquid injection unit, EPA's analysis of whether the
unit is well designed will focus on (1) the likelihood that
sufficient energy is provided to the waste to overcome the
activation level for breaking molecular bonds and (2) whether
sufficient oxygen is present to convert the waste constituents to
carbon dioxide and water vapor. The specific design parameters
that the Agency will evaluate to assess whether these conditions
are met are: temperature, excess oxygen, and residence time.
Below is a discussion of why EPA believes these parameters to be
important, as well as a discussion of how these parameters will
be monitored during operation.
It is important to point out that, relative to the
development of land disposed restriction standards, EPA is only
concerned with these design parameters when a quench water or
v
scrubber water residual is generated from treatment of a
particular waste. If treatment of a particular waste in a liquid
injection unit would not generate a wastewater stream, then the
3-52 Rev. 3
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Agency, for purposes of land disposal treatment standards, would
only be concerned with the waste characteristics that affect
selection of the unit, not the above-mentioned design parameters.
Temperature
Temperature is important in that it provides an indirect
measure of the energy available (i.e., BTUs/hr) to overcome the
activation energy of waste constituents. As the design
temperature increases, the more likely it is that the molecular
bonds will be destabilized and the reaction completed.
The temperature is normally controlled automatically through
the use of instrumentation which senses the temperature and
automatically adjusts the amount of fuel and/or waste being fed.
The temperature signal transmitted to the controller can be
simultaneously transmitted to a recording device, referred to as
a strip chart, and thereby continuously recorded. To fully
assess the operation of the unit, it is important to know not
only the exact location in the incinerator that the temperature
is being monitored but also the location of the design
temperature.
Excess Oxygen
It is important that the incinerator contain oxygen in
excess of the stiochiometric amount necessary to convert the
organic compounds to carbon dioxide and water vapor. If
3-53 Rev. 3
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insufficient oxygen is present, then destabilized waste
constituents could recombine to the same or other BDAT list
organic compounds and potentially cause the scrubber water to
contain higher concentrations of BDAT list constituents than
would be the case for a well operated unit.
In practice, the amount of oxygen fed to the incinerator is
controlled by continuous sampling and analysis of the stack gas.
If the amount of oxygen drops below the design value, then the
analyzer transmits a signal to the valve controlling the air
supply and thereby increases the flow of oxygen to the
afterburner. The analyzer simultaneously transmits a signal to a
recording device so that the amount of excess oxygen can be
continuously recorded. Again, as with temperature, it is
important to know the location from which the combustion gas is
being sampled.
Carbon Monoxide
Carbon monoxide is an important operating parameter because
it provides an indication of the extent to which the waste
organic constituents are being converted to CO- and water vapor.
As the carbon monoxide level increases, it indicates that greater
amounts of organic waste constituents are unreacted or partially
reacted. Increased carbon monoxide levels can result from
insufficient excess oxygen, insufficient turbulence in the
combustion zone, or insufficient residence time.
3-54 Rev. 3
-------
Waste Feed Rate
The waste feed rate is important to monitor because it is
correlated to the residence time. The residence time is
associated with a specific BTU energy value of the feed and a
specific volume of combustion gas generated. Prior to
incineration, the BTU value of the waste is determined through
the use of a laboratory device known as a bomb calorimeter. The
volume of combustion gas generated from the waste to be
incinerated is determined from an analysis referred to as an
ultimate analysis. This analysis determines the amount of
elemental constituents present which include carbon, hydrogen,
sulfur, oxygen, nitrogen, and halogens. Using this analysis plus
the total amount of air added, the volume of combustion gas can
be calculated. Having determined both the BTU content and the
expected combustion gas volume, the feed rate can be fixed at the
desired residence time. Continuous monitoring of the feed rate
will determine whether the unit was operated at a rate
corresponding to the designed residence time.
ii. Rotary Kiln
For this incineration, EPA will examine both the primary and
secondary chamber in evaluating the design of a particular
incinerator. Relative to the primary chamber, EPA's assessment
of design will focus on whether it is likely that sufficient
energy will be provided to the waste in order to volatilize the
waste constituents. For the secondary chamber,
3-55 Rev. 3
-------
analogous to the sole liquid injection incineration chamber, EPA
will examine the same parameters discussed previously under
liquid injection incineration. These parameters will not be
discussed again here.
The particular design parameters to be evaluated for the
primary chamber are: kiln temperature, residence time, and
revolutions per minute. Below is a discussion of why EPA
believes these parameters to be important, as well as a
discussion of how these parameters will be monitored during
operation.
Temperature
The primary chamber temperature is important, in that it
provides an indirect measure of the energy input (i.e., BTUs/hr)
that is available for heating the waste. The higher the
temperature is designed to be in a given kiln, the more likely it
is that the constituents will volatilize. As discussed earlier
under "Liquid Injection", temperature should be continuously
monitored and recorded. Additionally, it is important to know
the location of the temperature sensing device in the kiln.
Residence Time
This parameter is important in that it affects whether
sufficient heat is transferred to a particular constituent in
order for volatilization to occur. As the time that the waste is
3-56 Rev. 3
-------
in the kiln is increased, a greater quantity of heat is
transferred to the hazardous waste constituents. The residence
time will be a function of the specific configuration of the
rotary kiln including the length and diameter of the kiln, the
waste feed rate, and the rate of rotation.
Revolutions Per Minute (RPM)
This parameter provides an indication of the turbulence that
occurs in the primary chamber of a rotary kiln. As the
turbulence increases, the quantity of heat transferred to the
waste would also be expected to increase. However, as
the RPM value increases, the residence time decreases resulting
in a reduction of the quantity of heat transferred to the waste.
This parameter needs to be carefully evaluated because it
provides a balance between turbulence and residence time.
iii. Fluidized Bed
As discussed previously, in the section on "Underlying
Principles of Operation", the primary chamber accounts for almost
all of the conversion of organic wastes to carbon dioxide, water
vapor, and acid gas if halogens are present. The secondary
chamber will generally provide additional residence time for
thermal oxidation of the waste constituents. Relative to the
primary chamber, the parameters that the Agency will examine in
assessing the effectiveness of the design are temperature,
residence time, and bed pressure differential. The first two
3-57 Rev. 3
-------
were discussed under rotary kiln and will not be discussed here.
The latter, bed pressure differential, is important in that it
provides an indication of the amount of turbulence and,
therefore, indirectly the amount of heat supplied to the waste.
In general, as the pressure drop increases, both the turbulence
and heat supplied increase. The pressure drop through the bed
should be continuously monitored and recorded to ensure that the
designed valued is achieved.
iv. Fixed Hearth
The design considerations for this incineration unit are
similar to a rotary kiln with the exception that rate of rotation
(i.e., RPMs) is not an applicable design parameter. For the
primary chamber of this unit, the parameters that the Agency will
examine in assessing how well the unit is designed are the same
as discussed under rotary kiln; for the secondary chamber (i.e.,
afterburner), the design and operating parameters of concern are
the same as previously discussed under "Liquid Injection".
3-58 Rev. 3
-------
3.3 Performance Data for Wastewaters
Of the three demonstrated treatment technology systems
defined in Section 3.2, the Agency collected performance data for
the system consisting of liquid/liquid extraction followed by
steam stripping and activated carbon adsorption. This treatment
system was chosen by the EPA for collecting performance data
because the liquid/liquid extraction step in this three-step
treatment process provides an incremental reduction in the level
of organics over that obtained by either of the other two
treatment processes.
Performance data collected by EPA for liquid/liquid
extraction followed by stream stripping and carbon adsorption are
presented in Tables 3-1 to 3-5. Tables 3-1 through 3-5 present
the analytical data for sample sets I through 5 collected during
the Agency's sampling visit. The untreated K103 and K104 wastes
and the combined treated steam leaving the carbon adsorption beds
for each sample set were analyzed for BOAT volatile and
semivolatile organic compounds, metals, inorganic compounds, and
other parameters.
Included in Tables 3-1 through 3-5 are the design values and
*•
actual operating ranges for the key operating parameters of the
aniline liquid/liquid extractor, nitrobenzene liquid/liquid
3-59 Rev. 3
-------
TABLE 3-1 TREATMENT DATA FOR LIQUID/LIQUID EXTRACTION FOLLOWED BY STEAM STRIPPING AND
ACTIVATED CARBON ADSORPTION - EPA COLLECTED DATA
SAMPLE SET 1
BOAT CONSTITUENTS DETECTED
Volatile Organic Compounds
4 Benzene
48 Trichloromonof luoromethane
Semi volatile Organic Compounds
56 Aniline
101 2,4-Dinitrophenol
126 Nitrobenzene
142 Phenol
Metals
155 Arsenic
156 Barium
159 Chromium
160 Copper
161 Lead
163 Nickel
167 Vanadium
168 Zinc
Inorganics
169 Total Cyanides
170 Fluorides
171 Sulfides
UNTREATED
K103
(mg/l)
81
<2.5
51,000
<7,500
<1.500
<1,500
<0.010
<0.001
<0.007
<0.006
<0.005
<0.011
<0.006
0.021
0.0748
<0.20
89.0
WASTE
K104
240
<10
<150
<750
2,700
<150
<0.010
0.0078
0.432
0.012
<0.050
0.238
<0.006
0.079
6.28
<0.20
<1.0*
TREATED WASTE
(mg/l)
0.042
0.007
<0.030
0.380
<0.030
<0.030
<0.010
0.032
0.0097
<0.006
<0.500
<0.011
0.014
0.058
0.565
0.590
<1.0*
* - Negative Interference Value
Continued
3-60
Rev. 3
-------
TABLE 3-1 (Continued) TREATMENT DATA FOR LIQUID/LIQUID EXTRACTION FOLLOWED BY STEAM
STRIPPING AND ACTIVATED CARBON ADSORPTION - EPA COLLECTED DATA
SAMPLE SET 1
OPERATING PARAMETERS
Design Value
Operating Range
Aniline Liquid/Liquid Extractor :
Feed Rate to the Extractor (Ibs/hr)
Feed pH to the Extractor
Feed Temperature to the
o
Extractor ( C)
7,000 - 25,000
9 - 10**
40.0**
14,400 - 14,500
10.3
13.0
Nitrobenzene Liquid/Liquid Extractor
Feed Rate to the Extractor (Ibs/hr)
Feed pH to the Extractor
Feed Temperature to the
Extractor ( C)
27,000 - 35,000
Max. 2.4
25.0 - 65.0
21,300 - 46,000
0.2
39.0
Steam Stripper :
o
Top Column Temperature ( C)
Pressure Drop Across the
ColumnCinches of water)
Feed Rate to Steam Stripper(Ibs/hr)
Activated Carbon Adsorption:
Feed Rate to the System (Ibs/hr)
Feed pH to the System
Feed Temperature to the
System (°C)
Total Organic Carbon in treated
waste (mg/l)
Calculated Residence time (minutes)
Min. 95.0
Max. 90.0
Min. 20,000, Max. 90,000
Max. 65,300
Min. 7.0
40.0**
Max. 250
Instantaneous
Min. 85
95***
44.26 - 51.00
59,400 - 59,480
61,600 - 68,600
10.6
25.0
79.3
81 - 90
a - Onsite Engineering Report for E. I. duPont de Nemours, Inc., Beaumont, Texas,
Tables 4-1 through 4-3, 6-6, 6-8, and 6-14.
** - Not controlled. Normal operating value is given.
*** - Mid column substituted for top column temperature due to technical difficulties.
3-61
Rev. 3
-------
TABLE 3-2 TREATMENT DATA FOR LIQUID/LIQUID EXTRACTION FOLLOWED BY STEAM STRIPPING AND
ACTIVATED CARBON ADSORPTION - EPA COLLECTED DATA8
SAMPLE SET 2
BOAT CONSTITUENTS DETECTED
Volatile Organic Compounds
4 Benzene
48 Trichloromonof luoromethane
Semivolati le Organic Compounds
56 Aniline
101 2,4-Dinitrophenol
126 Nitrobenzene
142 Phenol
Metals
155 Arsenic
156 Barium
159 Chromium
160 Copper
161 Lead
163 Nickel
167 Vanadium
168 Zinc
Inorganics
169 Total Cyanides
170 Fluorides
171 Sulfides
UNTREATED
K103
(mg/l)
73
<5
33.000
<7,500
<1,500
<1,500
<0.010
<0.001
<0.007
<0.006
<0.005
<0.011
<0.006
0.003
0.0595
<0.20
89.0
WASTE
K104
320
<20
<150
<750
2.200
<150
<0.100
0.0015
0.097
<0.006
<0.100
0.055
<0.006
0.011
3.30
<0.20
<1.0*
TREATED WASTE
(mg/l)
<0.005
0.010
<0.030
0.320
O.030
<0.030
<0.100
0.042
0.024
<0.006
<0.050
<0.011
0.012
0.052
0.597
0.420
<1.0*
* - Negative Interference Value
Cont i nued
3-62
Rev. 3
-------
TABLE 3-2 (Continued) TREATMENT DATA FOR LIQUID/LIQUID EXTRACTION FOLLOWED BY STEAM
STRIPPING AND ACTIVATED CARBON ADSORPTION - EPA COLLECTED DATA
SAMPLE SET 2
OPERATING PARAMETERS
Design Value
Operating Range
Aniline Liquid/Liquid Extractor :
Feed Rate to the Extractor (Ibs/hr)
Feed pH to the Extractor
Feed Temperature to the
Extractor ( C)
7,000 - 25,000
9 - 10**
40.0**
15,900 - 16,000
10.3
22.0
Nitrobenzene Liquid/Liquid Extractor
Feed Rate to the Extractor (Ibs/hr)
Feed pH to the Extractor
Feed Temperature to the
Extractor ( C)
27,000 - 35,000
Max. 2.4
25.0 - 65.0
9,800 - 26,000
0.2
43.0
Steam Stripper :
o
Top Column Temperature ( C)
Pressure Drop Across the
ColumnCinches of water)
Feed Rate to Steam Stripper(lbs/hr)
Min. 95.0
Max. 90.0
Min. 20,000, Max. 90,000
102.2 - 103.3
42.40 - 58.00
49,000 - 60,100
Activated Carbon Adsorption:
Feed Rate to the System (Ibs/hr)
Feed pH to the System
Feed Temperature to the
o
System ( C)
Total Organic Carbon in treated
waste (mg/l)
Calculated Residence time (minutes)
Max. 65,300
Min. 7.0
40.0**
Max. 250
Instantaneous
Min. 85
63,000 - 76,
4.6
28.0
73.5
73 - 88
000
a - Onsite Engineering Report for E. I. duPont de Nemours, Inc., Beaumont, Texas,
Tables 4-1 through 4-3, 6-6, 6-8, and 6-14.
** - Not controlled. Normal operating value is given.
3-63
Rev. 3
-------
TABLE 3-3 TREATMENT DATA FOR LIQUID/LIQUID EXTRACTION FOLLOWED BY STEAM STRIPPING AND
ACTIVATED CARBON ADSORPTION - EPA COLLECTED DATA
SAMPLE SET 3
BOAT CONSTITUENTS DETECTED
Volatile Organic Compounds
4 Benzene
48 Trichlorof luoromethane
Semi volatile Organic Compounds
56 Aniline
101 2,4-Dinitrophenol
126 Nitrobenzene
142 Phenol
Metals
155 Arsenic
156 Barium
159 Chromium
160 Copper
161 Lead
163 Nickel
167 Vanadium
168 Zinc
Inorganics
169 Total Cyanides
170 Fluorides
171 Sulfides
UNTREATED
K103
(mg/l)
65
<2.5
39,000
<15,000
<3,000
<3,000
<0.010
<0.001
<0.007
<0.006
<0.005
<0.011
<0.006
0.0099
0.0411
<0.20
74.0
WASTE
K104
70
<5
<150
<750
2,300
<150
<0.010
0.011
<0.007
0.0075
<0.005
<0.011
<0.006
0.031
5.70
<0.20
<1.0*
TREATED WASTE
(mg/l)
0.018
O.005
4.20
<0.760
<0.150
<0.150
<0.010
0.068
0.008
<0.006
<0.005
<0.011
0.0091
0.016
0.201
0.220
<1.0*
* - Negative Interference Value
Continued
3-64
Rev. 3
-------
TABLE 3-3 (Continued) TREATMENT DATA FOR LIQUID/LIQUID EXTRACTION FOLLOWED BY STEAM
STRIPPING AND ACTIVATED CARBON ADSORPTION - EPA COLLECTED DATA3
SAMPLE SET 3
OPERATING PARAMETERS
Design Value
Operating Range
Aniline Liquid/Liquid Extractor :
Feed Rate to the Extractor (Ibs/hr)
Feed pH to the Extractor
Feed Temperature to the
Extractor ( C)
7,000 - 25,000
9 - 10**
40.0**
17,600 - 17,800
10.1
24.0
Nitrobenzene Liquid/Liquid Extractor
Feed Rate to the Extractor (Ibs/hr)
Feed pH to the Extractor
Feed Temperature to the
Extractor ( C)
27,000 - 35,000
Max. 2.4
25.0 - 65.0
24,100 - 33,000
5.7
42.5
Steam Stripper :
o
Top Column Temperature ( C)
Pressure Drop Across the
ColumnCinches of water)
Feed Rate to Steam Stripper(Ibs/hr)
Min. 95.0
Max. 90.0
Min. 20,000, Max. 90,000
102.6 - 103.0
46.42 - 50.33
60,200 - 60,400
Activated Carbon Adsorption:
Feed Rate to the System (Ibs/hr)
Feed pH to the System
Feed Temperature to the
o
System ( C)
Total Organic Carbon in treated
waste (mg/l)
Calculated Residence time (minutes)
Max. 65,300
Min. 7.0
40.0**
Max. 250
Instantaneous
Min. 85
57,700 - 58,140
3.1
44.0
10.8
96 - 97
a - Onsite Engineering Report for E. I. duPont de Nemours, Inc., Beaumont, Texas,
Tables 4-1 through 4-3, 6-6, 6-8, and 6-14.
** - Not controlled. Normal operating value is given.
3-65
Rev. 3
-------
TABLE 3-4 TREATMENT DATA FOR LIQUID/LIQUID EXTRACTION FOLLOWED BY STEAM STRIPPING AND
ACTIVATED CARBON ADSORPTION - EPA COLLECTED DATA8
* - Negative Interference Value
SAMPLE SET 4
BOAT CONSTITUENTS DETECTED
Volatile Organic Compounds
4 Benzene
48 Trichlorof luoromethane
Semi volatile Organic Compounds
56 Aniline
101 2,4-Dinitrophenol
126 Nitrobenzene
142 Phenol
Metals
155 Arsenic
156 Barium
159 Chromium
160 Copper
161 Lead
163 Nickel
167 Vanadium
168 Zinc
Inorganics
169 Total Cyanides
170 Fluorides
171 Sulfides
UNTREATED
K103
(mg/l)
55
<2.5
39.000
<15.000
<3.000
<3.000
0.021
<0.001
<0.007
<0.006
<0.005
<0.011
<0.006
0.018
<0.0100
<0.20
62.0
WASTE
K104
11
<0.5
<300
<1,500
2,900
<300
<0.010
0.017
<0.007
<0.006
<0.005
<0.011
<0.006
0.064
3.06
<0.20
<1.0*
TREATED WASTE
(mg/l)
0.019
<0.005
<0.030
0.260
<0.030
<0.030
<0.500
0.076
<0.007
<0.006
<0.005
0.015
<0.006
0.033
0.156
0.220
<1.0*
Cont i nued
3-66
Rev. 3
-------
TABLE 3-4 (Continued) TREATMENT DATA FOR LIQUID/LIQUID EXTRACTION FOLLOWED BY STEAM
STRIPPING AND ACTIVATED CARBON ADSORPTION - EPA COLLECTED DATA
SAMPLE SET 4
OPERATING PARAMETERS
Design Value
Operating Range
Aniline Liquid/Liquid Extractor :
Feed Rate to the Extractor (Ibs/hr)
Feed pH to the Extractor
Feed Temperature to the
o
Extractor ( C)
7,000 - 25,000
9 - 10**
40.0**
14,900 - 15,200
10.0
31.0
Nitrobenzene Liquid/Liquid Extractor
Feed Rate to the Extractor (Ibs/hr)
Feed pH to the Extractor
Feed Temperature to the
Extractor <°C>
27,000 - 35,000
Max. 2.4
25.0 - 65.0
12,800 - 35,000
0.8
50.0
Steam Stripper :
o
Top Column Temperature ( C)
Pressure Drop Across the
ColumnCinches of water)
Feed Rate to Steam Stripper(Ibs/hr)
Activated Carbon Adsorption:
Feed Rate to the System (Ibs/hr)
Feed pH to the System
Feed Temperature to the
System (°C)
Total Organic Carbon in treated
waste (mg/l)
Calculated Residence time (minutes)
Min. 95.0
Max. 90.0
Min. 20,000, Max. 90,000
Max. 65,300
Min. 7.0
40.0**
Max. 250
Instantaneous
Min. 85
102.9 - 103.0
44.05 - 46.10
60,300
59,900 - 60,000
4.0
38.0
10.0
90 - 93
a - Onsite Engineering Report for E. I. duPont de Nemours, Inc., Beaumont, Texas,
Tables 4-1 through 4-3, 6-6, 6-8, and 6-14.
** - Not controlled. Normal operating value is given.
3-67
Rev. 3
-------
TABLE 3-5 TREATMENT DATA FOR LIQUID/LIQUID EXTRACTION FOLLOWED BY STEAM STRIPPING AND
ACTIVATED CARBON ADSORPTION - EPA COLLECTED DATA°
SAMPLE SET 5
BOAT CONSTITUENTS DETECTED
Volatile Organic Compounds
4 Benzene
48 Trichlorof luoromethane
Semi volatile Organic Compounds
56 Aniline
101 2,4-Dinitrophenol
126 Nitrobenzene
142 Phenol
Metals
155 Arsenic
156 Barium
159 Chromium
160 Copper
161 Lead
163 Nickel
167 Vanadium
168 Zinc
Inorganics
169 Total Cyanides
170 Fluorides
171 Sulfides
UNTREATED WASTE
K103 K104
(mg/l)
32
<2.5
53,000
<15,000
<3,000
<3,000
<0.500
O.001
<0.007
<0.006
0.006
<0.011
<0.006
0.014
0.0384
<0.20
80.0
4.5
<0.25
<300
<1,500
3,900
<300
<0.500
0.013
0.0071
<0.006
<0.050
0.014
<0.006
0.014
4.44
<0.20
<1.0*
TREATED WASTE
(mg/l)
0.011
<0.005
0.960
0.230
O.030
0.150
<0.010
0.073
0.017
<0.006
<0.100
0.030
<0.006
0.012
0.129
0.620
<1.0*
* - Negative Interference Value
Cont i nued
3-68
Rev. 3
-------
TABLE 3-5 (Continued) TREATMENT DATA FOR LIQUID/LIQUID EXTRACTION FOLLOWED BY STEAM
STRIPPING AND ACTIVATED CARBON ADSORPTION - EPA COLLECTED DATA
SAMPLE SET 5
OPERATING PARAMETERS
Design Value
Operating Range
Aniline Liquid/Liquid Extractor :
Feed Rate to the Extractor (Ibs/hr)
Feed pH to the Extractor
Feed Temperature to the
o
Extractor ( C)
7,000 - 25,000
9 - 10**
40.0**
14,800 - 14,900
10.2
28.0
Nitrobenzene Liquid/Liquid Extractor
Feed Rate to the Extractor (Ibs/hr)
Feed pH to the Extractor
Feed Temperature to the
Extractor (°C)
27,000 - 35,000
Max. 2.4
Z5.0 - 65.0
24,700 - 31,500
1.5
47.5
Steam Stripper :
o
Top Column Temperature ( C)
Pressure Drop Across the
Column(inches of water)
Feed Rate to Steam Stripper(Ibs/hr)
Min. 95.0
Max. 90.0
Min. 20,000, Max. 90,000
102.6 - 102.7
44.80 - 51.80
57,590 - 57,660
Activated Carbon Adsorption:
Feed Rate to the System (Ibs/hr)
Feed pH to the System
Feed Temperature to the
o
System ( C)
Total Organic Carbon in treated
waste (mg/l)
Calculated Residence time (minutes)
Max. 65,300
Min. 7.0
40.0**
Max. 250
Instantaneous
Min. 85
52,200 - 61,500
3.5
33.5
7.0
91 - 107
a - Onsite Engineering Report for E. I. duPont de Nemours, Inc., Beaumont, Texas,
Tables 4-1 through 4-3, 6-6, 6-8, and 6-14.
** - Not controlled. Normal operating value is given.
3-69
Rev. 3
-------
extractor, steam stripper, and activated carbon adsorption beds
for each sample set collected.
3.4 Other Applicable Treatment Technologies
The Agency does not believe that other technologies are
applicable for treatment of K103 and K104 wastewaters because of
various physical and chemical characteristics of the wastewaters.
For a detailed description of the physical and chemical
characteristics affecting treatment selection, see BOAT
Background Document for the First Third Wastes,. Volume 1,
Section 2.
Liquid/liquid extraction followed by steam stripping and
activated carbon adsorption is judged to be available to treat
K103 and K104 wastewaters, and incineration is judged to be
available to treat K103 and K104 nonwastewaters. The Agency
believes these technologies to be available because (1) the
Agency does not have information showing that this technology
poses a greater total risk to human health and the environment
that land disposal; (2) this technology is commercially
available; and (3) this technology provides a substantial
reduction in the levels of BOAT constituents present in waste
K103 and K104.
3-70 Rev. 3
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4. IDENTIFICATION OF BEST DEMONSTRATED AVAILABLE TREATMENT
TECHNOLOGY FOR K103 AND K104
4.1 Introduction
The previous section described applicable treatment
technologies for waste codes K103 and K104, and the available
performance data for these technologies. This section describes
how the performance data collected by the Agency was evaluated to
determine which treatment technology system should be considered
BOAT for waste codes K103 and K104. Several treatment trains are
considered in this section as BOAT for wastewaters. They consist
of:
o liquid/liquid extraction,
o liquid/liquid extraction followed by steam stripping,
o liquid/liquid extraction followed by steam stripping
and activated carbon adsorption.
The use of activated carbon adsorption for treatment of K103
and K104 wastewaters generates a nonwastewater, spent carbon.
The treatment considered in this section as BOAT for the
nonwastewaters is rotary kiln incineration.
The topics covered in this section include descriptions of
V
the data screening process employed for selecting BOAT, the
methods used to ensure accuracy of the analytical data, and the
4-1 Rev. 3
-------
analysis of variance (ANOVA) tests performed in identifying the
best technology for the treatment of K103 and K104 wastes.
As discussed in Section 3, the Agency collected performance
data for the treatment of waste codes K103 and K104 from one
treatment technology system: liquid/liquid extraction followed
by steam stripping and activated carbon adsorption. No
additional performance data were available for the treatment of
K103 and K104 wastes. However, the Agency is using and comparing
data taken from various components of the treatment train to
determine BOAT. Performance data were not available for the
treatment of K103 and K104 nonwastewaters.
In general, performance data are screened according to the
following three conditions:
o proper design and operation of the treatment system;
o the existence of quality assurance/quality control
measures in the data analysis; and
o the use of proper analytical tests in assessing
treatment performance.
Sets of performance data which do not meet these three conditions
are not considered in the selection of BDAT. In addition, if
performance data indicate that the treatment system was not well-
designed and well-operated at the time of testing, these data
V
would also not be used.
4-2 Rev. 3
-------
The remaining performance data are then corrected to account
for incomplete recovery of certain constituents during the
analyses. Finally, in cases where the Agency has adequate
performance data for treatment of the waste by more than one
technology, an analysis of variance (ANOVA) test is used to
select the best treatment technology.
4.2 Data Screening
In the selection of BOAT for treatment of K103 and K104
wastewaters, the only performance data available were those
collected during the Agency's sampling visit. Five data sets
were collected by the Agency for treatment of the wastewaters by
liquid/liquid extraction followed by steam stripping and carbon
adsorption. These data were evaluated to determine whether any
of the data represented poor design or operation of the system.
One of the data sets (Sample Set #3) was deleted due to poor
operation of the carbon adsorption unit during the time data were
being collected. This was indicated by a higher than normal
system temperature and a relatively high aniline concentration in
the treated waste. The four remaining data sets were used for
the development of treatment standards for K103 and K104
wastewaters. These data sets are sample sets 1, 2, 4 and 5.
V
Toxic Characteristic Leaching Procedure (TCLP) data were not
used in setting treatment standards for waste codes K103 and K104
4-3 Rev. 3
-------
because metals were not identified as one of the classes of BDAT
list constituents for regulation (see Section 5 for further
details). For a discussion on the use of TCLP data in setting
treatment standards, refer to Section 1 of this background
document.
In instances where a selected constituent was not detected
in the treated waste, the treated value for that constituent was
assumed to be the practical quantification level. This was the
case for the following constituents: (1) benzene in Sample Set
#2; (2) aniline in Sample Sets #1, #2, and #4; (3) nitrobenzene
in Sample Sets #1, #2, #4, and #5; (4) phenol in Sample Sets #1,
#2, and #4. Analytical values for the treated waste are
presented in Table 4-1.
4.3. Data Accuracy
After data were eliminated from consideration for analysis
of BDAT based on the screening tests, the Agency adjusted the
remaining data using analytical recovery values in order to take
into account analytical interferences and incomplete recoveries
associated with the chemical makeup of the sample. The Agency
developed the recovery data (also referred to as accuracy data),
V
by first analyzing a waste for a given constituent and then by
adding a known amount of the same constituent (i.e., spike) to
the waste material. The total amount recovered after spiking,
4-4 Rev. 3
-------
TABLE 4-1 Treatment Data Used for Regulation of K103 and K104 Uastewaters
ANALYTICAL CONCENTRATIONS (1)
BOAT List
Const i tuent
Benzene
Aniline
2,4-Dinitrophenol
Nitrobenzene
Phenol
Total Cyanides
Sample Set 1
(total)
(mg/l)
0.042
<0.030
0.380
<0.030
<0.030
0.565
Sample Set 2
(total)
(mg/l)
<0.005
<0.030
0.320
<0.030
<0.030
0.597
Sample Set 4
(total)
(mg/l)
0.019
<0.030
0.260
<0.030
<0.030
0.156
Sample Set 5
(total)
(mg/l)
0.011
0.960
0.230
<0.030
0.150
0.129
ACCURACY-CORRECTED CONCENTRATIONS (2)
BOAT List
Constituent
Benzene
Aniline
2,4-Dinitrophenol
Nitrobenzene
Phenol
Total Cyanides
Sample Set 1
(total)
(mg/l)
0.055
0.033
0.475
0.026
0.143
0.785
Sample Set 2
(total)
(mg/l)
0.007
0.033
0.400
0.026
0.143
0.830
Sample Set 4
(total)
(mg/l)
0.025
0.033
0.325
0.026
0.143
0.217
Sample Set 5
(total)
(mg/l)
0.015
1.056
0.288
0.026
0.714
0.179
1. Onsite Engineering Report for E.I. du Pont de Nemours, Inc., Beaumont,
Texas, Tables 6-14.
2. Calculations shown in Appendix D of this Background Document.
4-5
Rev. 3
-------
minus the initial concentration in the sample, divided by the
amount added, is the recovery value. At least two recovery
values were calculated for spiked constituents, and the
analytical data were adjusted for accuracy using the lowest
recovery value for each constituent.
This was accomplished by calculating an accuracy factor from
the percent recoveries for each selected constituent. The
reciprocal of the lower of the two recovery values divided by
100, yields the accuracy factor. The corrected concentration for
each sample set is obtained by multiplying the accuracy factor by
the raw data value. The actual recovery values and accuracy
factors for the selected constituents are presented in
Appendix E.
The accuracy factors calculated for the selected
constituents varied from a high value of 4.76 for phenol to a low
value of 0.87 for nitrobenzene. The corrected concentration
values for the selected constituents are shown for the four data
sets in Table 6-1. These corrected concentrations values were
obtained by multiplying the accuracy factors (Appendix E) by the
concentration values for the selected constituents in the treated
waste. An arithmetic average value, representing the treated
waste concentration, was calculated for each selected constituent
from the four corrected values. These averages are presented in
Table 6-1. These adjusted values for the treatment technology
4-6 Rev. 3
-------
system consisting of liquid/liquid extraction followed by steam
stripping and activated carbon adsorption were then used to
determine BOAT for waste codes K103 and K104.
4.4 Analysis of Variance
In cases where the Agency has adequate performance data on
treatment of the same or similar wastes using more than one
technology, an analysis of variance (ANOVA) test is performed to
determine if one of the technologies provides significantly the
best treatment than the others. In cases where a particular
treatment technology is shown to provide better treatment, the
treatment standards will be used on this best technology. The
procedure followed for the analysis of variance (ANOVA) test is
described in Appendix A.
In order to determine BDAT for waste codes K103 and K104,
three combinations of demonstrated technologies, for which
adequate performance data were available, were considered for the
treatment of these wastes:
o Liquid/liquid extraction,
o Liquid/liquid extraction followed by steam stripping,
and
o Liquid/liquid extraction followed by steam stripping
and activated carbon adsorption.
4-7 Rev. 3
-------
The corrected data for sample sets 1, 2, 4, and 5 were used
to perform analysis of variance (ANOVA) tests to compare these
three technology combinations. The three combinations of
treatment technologies were compared based on the concentration
of primary waste constituents (benzene, aniline, nitrobenzene,
phenol, 2,4-dinitrophenol, and total cyanides) in the treated
waste. The rationale for selecting these constituents for the
ANOVA comparison is presented in Section 6.
The statistical results of the ANOVA test for liquid/liquid
extraction followed by steam stripping versus liquid/liquid
extraction indicate the following:
1) Liquid/liquid extraction followed by steam stripping
provides significantly better treatment for benzene and
nitrobenzene in waste codes K103 and K104 than
liquid/liquid extraction alone.
2) Liquid/liquid extraction followed by steam stripping
provides equivalent treatment for total cyanides in
waste codes K103 and K104 compared to liquid/liquid
extraction alone.
*•
3) Insufficient data exist to compare the treatment for
phenol, aniline, and 2,4-dinitrophenol achieved by
4-8 Rev. 3
-------
liquid/liquid extraction alone with that achieved by
liquid/liquid extraction followed by steam stripping.
The statistical results of the ANOVA test of liquid/liquid
extraction followed by steam stripping and activated carbon
adsorption versus liquid/liquid extraction followed by steam
stripping indicate the following:
1) Liquid/liquid extraction followed by steam stripping
and activated carbon adsorption provides significantly
better treatment for aniline, 2,4-dinitrophenol, phenol
and total cyanides in waste codes K103 and K104 than
liquid/liquid extraction followed by steam stripping.
2) Liquid/liquid extraction followed by steam stripping
and activated carbon adsorption provides equivalent
treatment for benzene in waste codes K103 and K104
compared to liquid/liquid extraction followed by steam
stripping.
3) Insufficient data exist to compare the treatment for
nitrobenzene achieved by liquid/liquid extraction
followed by steam stripping with that achieved by
V
liquid/liquid extraction followed by steam stripping
and activated carbon adsorption.
4-9 Rev. 3
-------
The three-step treatment technology system consisting of
liquid/liquid extraction followed by steam stripping and
activated carbon adsorption provides significantly better or
equivalent treatment overall for the primary constituents present
in waste codes K103 and K104 when compared either liquid/liquid
extraction alone or liquid/liquid extraction followed by steam
stripping. Therefore, the Agency has chosen this three-step
treatment system to be BOAT for waste codes K103 and K104.
4-10 Rev. 3
-------
5. SELECTION OF REGULATED CONSTITUENTS
In the previous section, the best demonstrated available
technology (BDAT) for treating the wastewater forms of waste
codes K103 and K104 was determined to be liquid/liquid extraction
followed by steam stripping and activated carbon adsorption.
The two nonwastewater forms of K103 and K104 are as follows:
spent carbon from the activated carbon adsorber and the solvent-
extract stream from the nitrobenzene liquid/liquid extractor.
Based on analysis of the influent and effluent streams (see
Tables 6-13 and 6-14 in the OER for K103 and K104) from the
activated carbon adsorber, the Agency expects the spent carbon to
contain the following constituents: benzene, aniline, 2,4-
dinitrophenol, nitrobenzene, phenol, and cyanides. Rotary kiln
incineration has been demonstrated on wastes that are similar to
the spent carbon from the activated carbon adsorber. Therefore,
the Agency believes that rotary kiln incineration is BDAT for the
spent carbon from the activated carbon adsorber.
Rotary kiln incineration has also been demonstrated on
wastes that are similar to the solvent-extract stream from the
nitrobenzene liquid/liquid extractor. Therefore, the Agency
believes that rotary kiln incineration is BDAT for the solvent-
extract from the nitrobenzene liquid/liquid extractor. In this
section, the necessary constituents are identified for assuring
5-1 Rev. 3
-------
the most effective treatment of the wastes. This is done by
following a three-step procedure:
o identifying the BOAT list constituents found in both
the untreated and treated waste;
o determining the classes of BOAT list constituents
present, and
o selecting the regulated constituents.
As discussed in Section 1, the Agency has developed a list
of hazardous constituents (Table 1-1) from which the constituents
to be regulated are selected. The list is a "growing list" that
does not preclude the addition of new constituents as additional
key parameters are identified. The list is divided into the
following categories: volatile organics, semivolatile organics,
metals, inorganics, organochlorine pesticides, phenoxyacetic acid
herbicides, organophosphorous pesticides, PCBs, and dioxins and
furans. The constituents in each category have similar chemical
properties and are expected to behave similarly during treatment,
with the exception of the inorganics.
5.1 Identification of BOAT List Constituents in the Untreated
and Treated Waste
Using EPA-collected data, the Agency identified those
constituents that were detected in the untreated and treated
waste. The BOAT list of constituents (see Table 1-1, Section
1.0) provided the target list of constituents. EPA collected
five sets of data at one facility (see the Onsite Engineering
5-2 Rev. 3
-------
Report for K103 and K104 for more details) to evaluate the
treatment of the wastewater forms of waste codes K103 and K104 by
liquid/liquid extraction followed by steam stripping and
activated carbon adsorption. One of the five data sets (data set
#3) was eliminated because the activated carbon adsorber was not
well-operated during the sampling interval. Poor operation of
the activated carbon adsorption system was indicated by a higher
than normal system temperature and a relatively high aniline
concentration in the treated waste. The remaining four data sets
were used to identify the constituents detected in the untreated
and treated waste. The detection limits for the BDAT list of
constituents are presented in Appendix C.
Table 5-1 presents the BDAT list as discussed in Section 1.
It indicates which of the BDAT list constituents were analyzed in
the untreated and treated waste. This table also gives the
concentrations of those BDAT list constituents which were
detected. As shown in Table 5-1, the following constituents were
detected in the untreated waste K103: benzene, aniline, arsenic,
lead, zinc, total cyanides, and sulfides. The following
constituents were detected in the untreated waste K104: benzene,
nitrobenzene, barium, chromium, copper, nickel, zinc, total
cyanides, and sulfides. The following constituents were detected
V
in the treated waste (K103 and K104): benzene, aniline,
2,4-dinitrophenol, trichloromonofluoromethane, phenol, barium,
chromium, nickel, vanadium, zinc, total cyanides, and fluorides.
5-3 Rev. 3
-------
TABLE 5-1 BOAT List Constituents in Untreated and Treated Waste
Parameter
Untreated
K103
(mg/l)
Untreated
K104
(mg/l)
Treated
K103/K104
(mg/l)
Volatiles
222
1
2
3
4
5
6
223
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
224
225
226
30
227
31
214
32
Acetone
Acetonitrile
Acrolein
Acrylonitrile
Benzene
Bromodi ch I oromethane
Bromomethane
n-Butyl alcohol
Carbon Tetrachloride
Carbon disulfide
Chlorobenzene
2-Chloro-1,3-butadiene
Ch lorodibromomethane
Chloroe thane
2-Chloroethyl vinyl ether
Chloroform
Chi oromethane
3 - Ch I oropr opene
1 ,2-Dibromo-3-chloropropane
1 , 2-D i bromoethane
Dibromomethane
trans- 1,4-Dichloro-2-butene
Dichlorodif luoromethane
1,1-Dichloroethene
1 , 2 - D i ch I oroethane
1,1-Dichloroethylene
trans-1,2-Dichloroethene
1,2-Dichloropropane
trans- 1 , 3-D i ch loropropene
cis-1,3-Dichloropropene
1,4-Dioxane
2-Ethoxyethanol
Ethyl acetate
Ethyl benzene
Ethyl cyanide
Ethyl ether
Ethyl methacrylate
Ethylene oxide
lodomethane
ND
ND
ND
ND
32 - 81
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
4.5 - 320
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
0.011 - 0.042
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND - Not detected
Cont i nued
5-4
Rev. 3
-------
TABLE 5-1 BOAT List Constituents in Untreated and Treated Waste (Continued)
Parameter
Volatiles (continued)
33 Isobutyl alcohol
228 Methanol
34 Methyl ethyl ketone
229 Methyl isobutyl ketone
35 Methyl methacrylate
37 Methylacrylom'trile
38 Methylene chloride
230 2-Nitropropane
39 Pyridine
40 1,1,1,2-Tetrachloroethane
41 1, 1.2,2-Tetrachloroethane
42 Tetrachloroethene
43 Toluene
44 Tribromome thane
45 1,1,1-Trichloroethane
46 1,1,2-Trichloroethane
47 Trichloroethene
48 Trichloromonof luromethane
49 1,2,3-Trichloropropane
231 1, 1,2-Trichloro- 1,2, 2- trif luoroethane
50 Vinyl chloride
215 1,2-Xylene
216 1,3-Xylene
217 1,4-Xylene
Semivolatiles
51 Acenaphthalene
52 Acenaphthene
53 Acetophenone
54 2-Acetylaminof luorene
55 4-Aminobiphenyl
56 Aniline
57 Anthracene
58 Aramite
59 Benz(a)anthracene
218 Benzal chloride
60 Benzenethiol
61 Benzidine
62 Benzo(a)pyrene
Untreated Untreated
K103 K104
(mg/l) (mg/l)
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
33000 - 53000
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
Treated
K103/K104
(mg/l)
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
0.007 - 0.010
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
0.96**
ND
ND
ND
ND
ND
ND
ND
ND - Not detected
** - Indicates that only one sample contained this constituent at detectable levels.
5-5
Cont i nued
Rev. 3
-------
TABLE 5-1 BOAT List Constituents in Untreated and Treated Waste (Continued)
Parameter
Untreated
K103
(mg/l)
Untreated
K104
(mg/l)
Treated
K103/K104
(mg/l)
Semivolatiles (continued)
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
232
83
84
85
86
87
88
89
90
91
92
93
94
95
96
97
98
99
100
101
Benzo(b) f I uoranthene
Benzo(ghi )perylene
Benzo( k) f t uoranthene
p-Benzoquinone
Bis(2-chloroethoxy)ethane
Bis(2-chloroethyl)ether
Bis(2-chloroisopropy)ether
Bis(2-ethylhexy)phthalate
4-Bromophenyl phenyl ether
Butyl benzyl phthlate
2-sec-Butyl-4,6-dinitrophenol
p-Chloroaniline
Chlorobenzilate
p-Chloro-m-cresol
2-Chloronaphthalene
2-Chlorophenol
3-Chloropropionitrile
Chrysene
ortho-Cresol
para-Cresol
Cyclohexanone
Dibenz(a,h)anthracene
Dibenzo(a,e)pyrene
Dibenzo(a, i )pyrene
m-D i ch I orobenzene
o-Dichlorobenzene
p- D i ch I orobenzene
3,3'-Dichlorobenzidine
2,4-Dichlorophenol
2,6-Dichlorophenol
Di ethyl phthalate
3,3'-Dimethyoxlbenzidine
p-D i methyl ami noazobenzene
3,3'-Dimethylbenzidine
2,4-Dimethylphenol
Dimethyl phthalate
Di-n-butyl phthalate
1,4-Dinitrobenzene
4,6-Dinitro-o-cresol
2,4-Dinitrophenol
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
0.23 - 0.38
ND - Not detected
5-6
Rev. 3
-------
TABLE 5-1 BOAT List Constituents in Untreated and Treated Waste (Continued)
Parameter
Untreated
K103
(mg/l)
Untreated
K104
(mg/l)
Treated
K103/K104
(mg/l)
Semivotatiles (cont.)
102
103
104
105
106
219
107
108
109
110
111
112
113
114
115
116
117
118
119
120
36
121
122
123
124
125
126
127
128
129
130
131
132
133
134
135
136
137
138
2,4-Dinitrotoluene
2,6-Dinitrotoluene
Di-n-octyl phthalate
Di-n-propylnitrosamine
Diphenylamine
Diphenylni trosamine
1,2-Diphenylhydrazine
Fluoranthene
Fluorene
Hexach I orobenzene
Hexach 1 orobutadi ene
Hexach I orocyc I opentadi ene
Hexach I oroethane
Hexach loroph ene
Hexach I oropropene
Indeno(1,2,3-cd)pyrene
Isosafrole
Hethapyrilene
3-Methycholanthrene
4,4'-Methylenebis(2-chloroaniline)
Methyl methanesulfonate
Napthalene
1,4-Naphthoquinone
1-Napthylamine
2-Napthylamine
p-Nitroaniline
Nitrobenzene
4-Nitrophenol
N-Nitrosodi-n-butylamine
N-Nitrosodiethylamine
N-Nitrosodimethylamine
N-Nitrosomethylethylamine
N-N i trosomorphol ine
N-Nitrosopiperidine
n-Nitrosopyrrol idine
5-Nitro-o-toluidine
Pentach I orobenzene
Pentach loroethane
Pentach t oroni t robenzene
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
NO
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
2200 - 3900
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
NO
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND - Not detected
5-7
Rev. 3
-------
TABLE 5-1 BOAT List Constituents in Untreated and Treated Waste (Continued)
Parameter
Semivolatiles (cont.)
139 Pentachlorophenol
140 Phenacetin
141 Phenanthrene
142 Phenol
220 Phthalic anhydride
143 2-Picoline
144 Pronamide
145 Pyrene
146 Resorcinol
147 Safrole
148 1,2,4,5-Tetrachlorobenzene
149 2, 3, 4, 6-Tetrachlorophenol
150 1,2,4-Trichlorobenzene
151 2,4,5-Trichlorophenol
152 2,4,6-Trichlorophenol
153 Tris(2,3-dibromopropyl)phosphate
Metals
154 Antimony
155 Arsenic
156 Barium
157 Beryllium
158 Cadmium
159 Chromium
221 Chromium (hexavalent)
160 Copper
161 Lead
162 Mercury
163 Nickel
164 Selenium
165 Si Iver
166 Thallium
167 Vanadium
168 Zinc
Inorganics
169 Cyanide
170 Fluoride
171 Sulfide
Untreated
K103
(mg/l)
NO
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
0.021**
ND
ND
ND
ND
ND
ND
0.006**
ND
ND
ND
ND
ND
ND
0.003 - 0.021
0.038 - 0.075
ND
62.0 - 89.0
Untreated
K104
(mg/l)
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
0.0015 - 0.017
ND
ND
0.007 - 0.432
ND
0.012**
ND
ND
0.014 - 0.238
ND
ND
ND
ND
0.011 - 0.079
3.06 - 6.28
ND
ND
Treated
K103/K104
(mg/l)
ND
ND
ND
0.15**
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
0.032 - 0.076
ND
ND
0.0097 - 0.024
ND
ND
ND
ND
0.015 - 0.030
ND
ND
ND
0.012 - 0.014
0.012 - 0.058
0.129 - 0.597
0.220 - 0.620
ND
** - Indicates that only one sample contained this constituent at detectable levels.
5-8
Cont i nued
Rev. 3
-------
TABLE 5-1 BOAT List Constituents in Untreated and Treated Waste (Continued)
Parameter
Organochlorine Pesticides
172 Aldrin
173 alpha-BHC
174 beta-BHC
175 delta-BHC
176 gamma -BHC
177 Chlordane
178 ODD
179 DDE
180 DDT
181 Dieldrin
182 Endosulfan I
183 Endosulfan II
184 Endrin
185 Endrin aldehyde
186 Heptachlor
187 Heptachlor epoxide
188 Isodrin
189 Kepone
190 Mehoxychlor
191 Toxaphene
Phenoxyacetic Acid Herbicides
192 2,4-Dichlorophenoxyacetic acid
193 Si I vex
194 2,4, 5-T
Organophosphorous Insecticides
195 Disulfoton
196 Famphur
197 Methyl parathion
198 Paration
199 Phorate
PCBs
200 Aroclor 1016
201 Aroclor 1221
202 Aroclor 1232
Untreated
K103
(ing/ 1)
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
ND
ND
ND
Untreated
K104
(mg/l)
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
V
ND
ND
ND
Treated
K103/K104
(mg/l)
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
ND
ND
ND
ND - Not detected
NA - Not analyzed
5-9
Rev. 3
-------
TABLE 5-1 BOAT List Constituents in Untreated and Treated Waste (Continued)
Parameter
PCBs (continued)
203 Aroclor 1242
204 Aroclor 1248
205 Aroclor 1254
206 Aroclor 1260
Dioxins and Furans
207 Hexachlorodibenzo-p-dioxins
208 Hexachlorodibenzofuran
209 Pentachlorodibenzo-p-dioxins
210 Pentachlorodibenzofuran
211 Tetrachlorodibenzo-p-dioxins
212 Tetrachlorodibenzofuran
213 2,3,7,8-Tetrachlorodibenzo-p-dioxin
Untreated
K103
dug/ 1)
ND
NO
ND
ND
ND
ND
ND
ND
ND
ND
ND
Untreated
K104
(ing/ 1)
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
Treated
K103/K104
(ing/ 1)
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND
ND - Not detected
5-10
Rev. 3
-------
Since the waste codes K103 and K104 are mixed before the steam
stripping step, the analytical data for the treated waste are the
same for both waste codes.
The untreated and treated waste samples were not analyzed
for other classes of BDAT organics (organochlorine pesticides,
phenoxyacetic acid herbicides, and organophosphorus pesticides)
because there is no in-process source of these constituents and
because of the extreme unlikelihood of finding these constituents
at treatable levels in the waste.
5.2 Determination of Classes of Constituents
The BDAT list constituents in waste codes K103 and K104
belong to the following four classes: volatiles, semivolatiles,
metals, and inorganics (See Table 5-1). Two volatile
constituents, benzene and trichloromonofluoromethane, were
detected. Four semivolatile constituents, aniline,
2,4-dinitrophenol, nitrobenzene, and phenol were also detected.
Six metal constituents were also detected: arsenic, chromium,
lead, nickel, vanadium, and zinc. The inorganic pollutants
detected were cyanide, fluoride, and sulfide.
v
The metal constituents were present in untreatable
concentrations in the untreated waste codes K103 and K104. None
of the metals in either untreated K103 or untreated K104 were
5-11 Rev. 3
-------
detected at a concentration level higher than 1 mg/1. Also, by
comparing the concentration of metals in the untreated and
treated waste for both waste codes K103 and K104, the Agency
concluded that metals were not substantially treated. For a
discussion of how the Agency decides when treatment is
substantial, see Section 1 of this background document.
The BDAT metal constituents in K103 and K104 were not
present at treatable levels in the waste. Therefore, metals were
eliminated as a class of BDAT list constituents to be regulated
in waste codes K103 and K104. However, the remaining three
classes of pollutants, namely, volatiles, semivolatiles, and
inorganics, were generally present at treatable concentration
levels in the untreated wastes and were judged to be
substantially treated when the untreated and treated constituent
data were compared for both waste codes.
5.3 Selecting the Regulated Constituents
The Agency evaluated the analytical data for each
constituent to determine if the constituent should be selected
for regulation. In general, the Agency was guided by the
criteria for selecting regulated constituents as described in
»•
Section 1 of this background document.
5-12 Rev. 3
-------
The rationale for selecting the regulated constituents from
the four classes of constituents is presented below.
Volatiles
Benzene was present in significant concentrations in both
the untreated K103 and untreated K104 streams. Benzene was
selected as a regulated constituent for waste codes K103 and K104
because it was substantially treated in both waste codes. The
benzene concentration in untreated K103 and untreated K104 was
reduced by the treatment system to below treatable levels.
Trichloromonofluoromethane was not detected in either
untreated K103 or untreated K104, but was detected in the treated
waste. Although this compound was reported as not detected in
the untreated waste, the Agency has judged that it was present,
but was masked due to high concentrations of aniline and
nitrobenzene. The Agency believes that effective treatment of
benzene will effectively treat trichloromonofluoromethane as
well. Trichloromonofluoromethane is less soluble in water than
benzene, and is soluble in nitrobenzene. This indicates that
trichloromonofluoromethane will also be effectively treated by
the solvent extraction step of the treatment system.
V
Trichloromonofluoromethane has a higher vapor pressure than
benzene at 40°C, which indicates that trichloromonofluoromethane
will be effectively treated by the steam stripping step of the
5-13 Rev. 3
-------
treatment system. As a result, trichloromonofluoromethane was not
selected as a regulated constituent for either waste code K103 or
waste code K104, because treatment for benzene will also treat
trichloromonofluoromethane.
Semivolatiles
Aniline was detected in untreated K103 at high concentration
levels. Aniline was reported as not detected in untreated K104
but it was found in the treated waste at low concentration
levels. Based on data analysis, the concentration of aniline in
the untreated K103 waste was substantially reduced (to be below
treatable levels) by the treatment system. The Agency assumes
aniline was not detected in untreated K104 because the Practical
Quantification Levels were high due to matrix interferences. The
Agency believes that aniline was present in untreated K104 and
that it was effectively treated by the treatment system. As a
result, aniline was selected as a regulated constituent for both
waste codes K103 and K104.
The BOAT list constituent 2,4-dinitrophenol was not detected
in either untreated K103 or untreated K104. It was, however,
detected in the treated waste. The Agency assumes that
V-
2,4-dinitrophenol was not detected in both untreated K103 and
untreated K104 because the Practical Quantification Levels were
high (see Appendix C) due to matrix interferences. The Agency
5-14 Rev. 3
-------
believes that 2,4-dinitrophenol was present in both untreated
K103 and untreated K104 and that it was effectively treated by
the treatment system. As a result, 2,4-dinitrophenol was
selected as a regulated constituent for both waste codes K103 and
K104.
Nitrobenzene was not detected in untreated K103. It was
detected in untreated K104, and it was not detected in the
treated waste. The concentration of nitrobenzene in untreated
K104 was substantially reduced by the treatment system. The
Agency assumes that nitrobenzene was not detected in untreated
K103 because the Practical Quantification Levels were high (see
Appendix C) due to matrix interferences. The Agency believes
that nitrobenzene was present in untreated K103 and that it was
effectively treated by the treatment system. As a result,
nitrobenzene was selected as a regulated constituent for both
waste codes K103 and K104.
Phenol was not detected in either untreated K103 or
untreated K104. It was detected, however, in the treated waste.
The Agency assumes that phenol was not detected in both untreated
K103 and untreated K104 because the Practical Quantification
Levels were high (see Appendix C) due to matrix interferences.
V-
The Agency believes that phenol was present in both untreated
K103 and untreated K104 and that it was effectively treated by
5-15 Rev. 3
-------
the treatment system. As a result, phenol was selected as a
regulated constituent for both waste codes K103 and K104.
Inorganics
Cyanide was detected in untreated K103 and untreated K104,
and also in the treated waste. Because the concentration of
cyanide in untreated K103 increased when the waste was treated,
the Agency concluded that cyanide in untreated K103 was not
effectively treated. This apparent increase in cyanide
concentration for waste code K103 was thought to be due to the
mixing with waste code K104. The cyanide concentration was
higher in untreated K104 than in untreated K103. The
concentration of cyanide in untreated K104 was substantially
reduced by the treatment system. Therefore, the Agency believes
that cyanide in untreated K104 was effectively treated by the
treatment system. As a result, the Agency selected cyanide as a
regulated constituent for K104 but not for K103.
Fluoride was not detected in either untreated K103 or
untreated K104. It was, however, detected in the treated waste.
The Agency has judged that fluoride was present in both untreated
K103 and untreated K104 at concentration levels below the
Practical Quantification Level for the untreated waste matrix and
that it was not effectively treated by the treatment system. As
5-16 Rev. 3
-------
a result, fluoride was not selected as a regulated constituent
for either waste code K103 or waste code K104.
Sulfide was detected in untreated K103, but was not detected
in either untreated K104 or in the treated waste. The Agency
recognizes that the sulfide concentration was diminished in the
treated waste, but considers this an incidental treatment since
the treatment technology tested is not demonstrated for the
treatment of sulfides. As a result, sulfide was not selected as
a regulated constituent for either waste code K103 or waste code
K104.
The regulated constituents for K103 are as follows:
o benzene
o aniline
o 2,4-dinitrophenol
o nitrobenzene
o phenol
The regulated constituents for K104 are as follows:
o benzene
o aniline
o 2,4-dinitrophenol
o nitrobenzene
o phenol
o total cyanides
For the nonwastewater forms of K103 and K104, the same BOAT
list constituents were chosen for regulation as shown above for
wastewaters. This was done because the Agency did not have any
data available for determining the concentration of BOAT list
constituents in the nonwastewaters.
5-17 Rev. 3
-------
6. CALCULATION OF BOAT TREATMENT STANDARDS
In this section, the actual treatment standards for waste
codes K103 and K104 are presented. These standards were
calculated based on the performance of the demonstrated treatment
system which was determined by the Agency to be the best for
treating both waste codes. In Section 4, BOAT for the wastewater
forms of waste codes K103 and K104 was determined to be
liquid/liquid extraction followed by steam stripping and
activated carbon adsorption. BOAT for the nonwastewater forms of
K103 and K104 was determined to be incineration. The previous
section identified the constituents to be regulated for the
wastewater and nonwastewater forms of K103 and K104 wastes.
As discussed in Section 1, the Agency calculated the BOAT
treatment standards for waste codes K103 and K104 by following a
four-step procedure: (1) editing the data; (2) correcting the
remaining data for analytical interference; (3) calculating
adjustment factors (variability factors) to account for process
variability; and (4) calculating the actual treatment standards
using variability factors and average treatment values. The four
steps in this procedure are discussed in detail in Sections 6.1
through 6.4.
6-1 Rev. 3
-------
6 .1 Editing the Data
Five sets of treatment data for waste codes K103 and K104
were collected by the Agency at one facility which operated a
treatment system consisting of liquid/liquid extraction followed
by steam stripping and activated carbon adsorption. The Agency
evaluated the five data sets to determine if the treatment system
was well operated at the time of the sampling visit. The Agency
eliminated one data set, sample set #3, because the treatment
system was not well operated when the samples were collected (as
discussed in Section 5). For further details on the five data
sets, see the Onsite Engineering Report for K103 and K104. The
remaining four data sets were used to calculate treatment
standards.
Toxic Characteristic Leaching Procedure (TCLP) data were not
used in setting treatment standards for waste codes K103 and K104
because metals were not one of the classes of BOAT list
constituents identified for regulation (see Section 5 for further
details). For a discussion on the use of TCLP data in setting
treatment standards, refer to Section 1 of this background
document.
In instances where a selected constituent was not detected
in the treated waste, the treated value for that constituent was
assumed to be the Practical Quantification Level. This was the
6-2 Rev. 3
-------
case for the following constituents: (1) benzene in sample set
#2; (2) aniline in sample sets #1, #2, and #4; (3) nitrobenzene
in sample sets #1, #2, #4, and #5; (4) phenol in sample sets #1,
#2, and #4. Analytical values for the treated waste are
presented in Section 3, Tables 3-1 through 3-5 of this report.
6.2 Correcting the Remaining Data
Data values for the constituents selected for regulation
were taken from the four data sets (sample sets 1, 2, 4 and 5).
These values were corrected in order to take into account
analytical interferences associated with the chemical make-up of
the treated sample. This was accomplished by calculating an
accuracy factor from the percent recoveries for each selected
constituent. The reciprocal of the lower of the two recovery
values divided by 100, yields the accuracy factor. The corrected
concentration for each sample set is obtained by multiplying the
accuracy factor by the uncorrected data value. The calculation
of recovery values is described in Section 1 of this background
document. The actual recovery values and accuracy factors for
the selected constituents are presented in Appendix E.
The accuracy factors calculated for the selected
V
constituents varied from a high value of 4.76 for phenol to a low
value of 0.87 for nitrobenzene. The corrected concentration
values for the selected constituents are shown for the four data
6-3 Rev. 3
-------
sets in Table 6-1. These corrected concentration values were
obtained by multiplying the accuracy factors (Appendix E) by the
concentration values for the selected constituents in the treated
waste. An arithmetic average value, representing the treated
waste concentration, was calculated for each selected constituent
from the four corrected values. These averages are presented in
Table 6-1.
6.3 Calculating Variability Factors
It is expected that in normal operation of a well-designed
and well-operated treatment system there will be some variability
in performance. Based on the test data, a measure of this
variability is expressed by the variability factor (see Appendix
A). These factors were calculated for each of the selected
regulated constituents. The methodology for calculating
variability factors is explained in Appendix A of this report.
Table 6-1 presents the results of calculations for the selected
constituents. Appendix D of this report shows how the actual
values in Table 6-1 were calculated.
The variability factors calculated for the selected
constituents vary from a high value of 15.40 for aniline to a low
value of 1.65 for 2,4-dinitrophenol. A variability factor of i.o
represents test data from a process measured without variation
and analytical interferences. Nitrobenzene was not detected in
6-4 Rev. 3
-------
1
0\
I
en
Table 6-1 Regulated Constituents and Calculated Treatment Standards for K103 and IC104 Wastewaters
Accuracy-Corrected Concentration (mg/l)
Sample Sample Sample Sample
Set #1 Set #2 Set #4 Set #5
Constituent
Volatiles:
4. Benzene 0.055 0.007 0.025 0.015
Semivolati les:
56. Aniline 0.033 0.033 0.033 1.056
101. 2,4-Dinitrophenol* 0.475 0.400 0.325 0.288
126. Nitrobenzene 0.026 0.026 0.026 0.026
142. Phenol » 0.143 0.143 0.143 0.714
Inorganics:
169. Total Cyanides** 0.785 0.830 0.217 0.179
Average
T f»Aa^ &s4
i reateo
Waste
Concentration
(mg/l)
0.026
0.289
0.372
0.026
0.286
0.503
Variability
Factor
(VF)
5.654
15.398
1.648
2.800
4.864
5.334
Treatment
C +• arwlo r*ek
standard
(mg/l)
(Average
X VF)
0.147
4.450
0.613
0.073
1.391
2.683
1 - Accuracy Corrrection Factors and Variability Factors were determined as discussed in Appendix D.
* - Percent recovery of 4-Nitrophenol was used in the calculation of the standard for 2,4-Dinitrophenol.
** - Total cyanides are regulated for K104 only.
-------
the treated waste, and concentration values for the treated waste
were set at the Practical Quantification Level for nitrobenzene.
This resulted in no apparent variation among the treated values
and a calculated variability factor of 1.0. Instead of using the
calculated value of 1.0, the variability factor for nitrobenzene
was fixed at 2.8 as justified in Appendix D of this document.
6.4 Calculating the Treatment Standards
The treatment standards for the selected constituents were
calculated by multiplying the variability factors by the average
concentration values for the treated waste. The treatment
standards are presented in Table 6-1. Standards were calculated
for wastewaters only. The treatment standards for K103 and K104
nonwastewaters are transferred from the treatment tests of K019
and K048/K051 wastes.
The BOAT Wastewater Treatment Standard for waste code K103
is as follows:
Constituent Total Composition (mg/1)
Benzene 0.147
Aniline 4.450
2,4-Dinitrophenol 0.613
Nitrobenzene O.Q73
Phenol 1.391
6-6 Rev. 3
-------
The BOAT Wastewater Treatment Standard for waste code K104
is as follows:
Constituent Total Composition (mcf/1)
Benzene 0.147
Aniline 4.450
2,4-Dinitrophenol 0.613
Nitrobenzene 0.073
Phenol 1.391
Total Cyanides (CN) 2.683
The treatment standards for waste codes K103 and K104 vary
from 4.45 mg/1 for aniline to 0.073 mg/1 for nitrobenzene.
Nonwastewater treatment standards for waste codes K103 and
and K104 were also determined by the Agency. These treatment
standards apply to the spent carbon from the carbon adsorber;
these treatment standards do not apply to the nitrobenzene
solvent from the liquid/liquid extractor because the Agency
believes that no ash is formed when this stream is incinerated.
No performance data were available for the treatment of K103
and K104 nonwastewaters. The Agency therefore decided to
transfer treatment standards from the treatment of wastes which
were determined to be similar to K103 and K104 nonwastewaters
based on waste characteristics affecting ^performance. The
nonwastewater treatment standards for waste codes K103 and K104
were transferred from treatment data for wastes K019 and
K048/K051. The thermal conductivities of wastes K019, K048, and
6-7 Rev. 3
-------
K051 were compared with the thermal conductivities of waste codes
K103 and K104. Waste K019 was selected for transferring
treatment standards to wastes K103 and K104 because its thermal
conductivity was lower than that of both wastes K103 and K104.
The treated waste concentrations and treatment standards for K019
are presented in Table 6-2. The boiling points of the selected
constituents in waste codes K103 and K104 were compared to the
boiling points of the regulated constituents in waste code K019.
Constituents were matched as closely as possible on the basis of
the boiling point (see Table 6-2).
Chlorinated organic constituents in K019 with three or more
chlorine atoms in their structure were eliminated from
consideration for this matching. All chlorinated organics with
three or more chlorine atoms were below detectable levels in
treated K019. The treated concentrations were therefore set at
the detection limit for these constituents. However, the
detection limits for these constituents were abnormally high in
treated K019 due to matrix interferences, leading to high
treatment standards. Therefore, chlorinated organic constituents
with three or more chlorine atoms were not considered when
matching constituents from K103 and K104 with those from K019.
The remaining constituents in K019 were matched as closely as
possible with those in K103 and K104 on the basis of boiling
6-8 Rev. 3
-------
Table 6-2 Regulated Constituents and Calculated Treatment Standards for K019 Nonwasteuaters
I
vo
JO
(D
Constituent
Volatiles:
9. Chlorobenzene
14. Chloroform
23. 1,2-Dichloroethane
42. Tetrachloroethene*
45. 1,1,1-Trichloroethane*
Semivolati les:
68. Bis(2-chloroethyl)ether
113. Hexachloroethane*
121. Naphthalene
141. Phenanthrene
150. 1,2,4-Trichlorobenzene*
Treated
Waste
Concentration
Range
(mg/kg)
<2
<2
<2
<2
<2
<2
<2
<2
<2
<5
Average
Corrected
Waste
Concentration
(mg/kg)
2.02
2.13
2.13
2.13
2.13
1.94
9.71
1.94
1.94
6.68
Variability
Factor
(VF)
2.8
2.8
2.8
2.8
2.8
2.8
2.8
2.8
2.8
2.8
Treatment
Standard
(mg/kg)
(Average
X VF)
5.66
5.96
5.96
5.96
5.96
5.44
27.2
5.44
5.44
18.7
Boiling
Point
(deg. C)
132
61.7
83.5
121
74.1
116
186
218
340
213.5
2 - Treatment standard calculations are described in detail in the Background Document for K019.
* - The Agency believes the detection limits for these constituents were abnormally high due to matrix interferences. These
constituents were therefore eliminated from consideration when transferring treatment standards to K103 and K104 nonwastewaters.
-------
point.1 Treatment standards were then transferred from waste
code K019 to the matched constituent. Cyanide treatment
standards were transferred from the treatment of K048/K051, since
cyanide was not present in K019 waste.
The BOAT nonwastewater treatment standards for waste codes
K103 and K104 are as follows:
Constituent
Benzene
Aniline
2,4-Dinitrophenol
Nitrobenzene
Phenol
Total Cyanides (CN)
Total Composition (mg/kg)
K103 K104
5,
5,
5,
.96
.44
.44
5.44
5.44
NR
5,
5,
.96
.44
5.44
5.44
5.44
1.48
NR - Not regulated for this waste code.
1. The removal of highly chlorinated organic constituents in
K019 from consideration for transfer affected the treatment
standards for the following constituents in K103 and K104:
nitrobenzene (naphthalene was used rather than 1,2,4-tri-
chlorobenzene) , aniline, and phenol (naphthalene was used
rather than hexachloroethane or 1,2,4-trichlorobenzene).
6-10
Rev. 3
-------
7. CONCLUSIONS
The Agency has proposed treatment standards for waste codes
K103 and K104 generated by the nitrobenzene/aniline industry.
Standards for wastewater and nonwastewater forms of these wastes
are presented in Tables 7-1 and 7-2 respectively.
The treatment standards proposed for waste code K103 and
K104 have been developed consistent with EPA's promulgated
methodology for BOAT (November 7, 1986, 51 FR 40572). Both waste
codes are generated by the treatment of process wastewaters from
the nitrobenzene/aniline industry. Based on a careful review of
available data for the industrial processes which generate these
wastes and all available data characterizing these wastes, the
Agency has determined that these two waste codes represent a
separate waste treatability group. Wastes in this treatability
group are primarily comprised of water, with nitrobenzene or
aniline present in smaller but significant quantities. Although
the concentrations of specific constituents will vary from
facility to facility, all of the wastes are expected to contain
similar BOAT list organics and are expected to be treatable to
the same levels using the same technology.
The BOAT list constituents generally present in wastes of
this treatability group are benzene, aniline, 2,4-dinitrophenol,
nitrobenzene, phenol, and cyanides. Additionally the Agency
7-1 Rev. 3
-------
TABLE 7-1 BOAT TREATMENT STANDARDS FOR WASTEWATER: K103 AND
K104 WASTES
Regulated Constituents Total Composition (mg/1)
K103 K104
Benzene
Aniline
2 , 4-Dinitrophenol
Nitrobenzene
Phenol
Total Cyanides
0.147
4.450
0.613
0.073
1.391
NR
0.147
4.450
0.613
0.073
1.391
2.683
NR - Not regulated for this waste code.
TABLE 7-2 BOAT TREATMENT STANDARDS FOR NONWASTEWATER:
K103 AND K104 WASTES
Regulated Constituents Total Composition (rag/kg)
K103 K104
Benzene 5.96 5.96
Aniline 5.44 5.44
2,4-Dinitrophenol 5.44 5.44
Nitrobenzene 5.44 5.44
Phenol 5.44 5.44
Total Cyanides NR 1.48
NR - Not regulated for this waste code.
7-2 Rev. 3
-------
expects that these wastes could be mixed together prior to
treatment. As a result, EPA has examined the sources of the
wastes, applicable technologies, and waste treatment performance
in order to support a single regulatory approach for these six
waste constituents. Through available data bases, the Agency has
identified the following demonstrated technologies for treatment
of constituents present in the wastes which are part of this
treatability group: solvent (liquid/liquid) extraction, steam
stripping, activated carbon adsorption, and biological treatment.
In the development of treatment standards for these wastes,
the Agency examined all available treatment data. The Agency
also conducted performance tests on a commercial scale treatment
system consisting of liquid/liquid extraction followed by steam
stripping and activated carbon adsorption for waste codes K103
and K104. Design and operating data collected during the testing
of the treatment system indicate that the treatment system was
properly operated during four of the five sample sets.
Accordingly, the treatment performance data from four sample sets
were used in the development of the BOAT treatment standards.
Two categories of treatment standards were developed for
wastes in the K103 and K104 treatability group: wastewater and
nonwastewater wastes. (For the purpose of the land disposal
restrictions rule, wastewaters are defined as wastes containing
7-3 Rev. 3
-------
less than 1% by weight filterable solids and less than 4% by
weight total organic carbon. For K103 and K104 wastes, this
definition was amended to include wastewaters with a TOC content
up to 4%).
BOAT for the wastewater forms of waste codes K103 and K104
was determined to be liquid/liquid extraction followed by steam
stripping and activated carbon adsorption. This was based on a
statistical comparison of the Agency's test and performance data
from this treatment train to other available treatment data. The
wastewater treatment standards for waste codes K103 and K104 are
based on EPA's test of liquid/liquid extraction followed by steam
stripping and activated carbon adsorption.
Two nonwastewater forms of waste codes K103 and K104 were
identified by the Agency as spent carbon from the activated
carbon adsorber and nitrobenzene solvent from the nitrobenzene
liquid/liquid extractor.
Incineration was determined to be BDAT for the nonwastewater
forms of wastes K103 and K104. Nonwastewater treatment standards
for K103 and K104 are based on a transfer of treatment data from
K019 and K048/K051 wastes. BDAT for wastes K019 and K048/K051
v
was determined to be rotary kiln incineration. Treatment data
for BDAT list organics were transferred from waste K019 based on
a comparison of the thermal conductivities between waste code
7-4 Rev. 3
-------
K019 and waste codes K103 and K104. Data were transferred for
constituents selected for regulation on a constituent by
constituent basis. This was done by matching constituents on the
basis of boiling points. Treatment standards for cyanide were
transferred from the treatment of K048/K051, since cyanide was
not present in K019 waste.
Nonwastewater standards are established only for the spent
carbon from the activated carbon adsorber because the Agency
believes that the incineration of the nitrobenzene solvent from
the nitrobenzene liquid/liquid extractor will not produce ash.
The transfer of data for these nonwastewaters was determined to
be appropriate due to the similarity in physical and chemical
composition of the wastes such that the wastes would be expected
to be treated to similar levels by the same technology.
Regulated constituents were selected on the basis of
substantial treatment, which was determined by comparing the
constituent concentrations detected in the untreated and treated
wastes. All waste characterization data and applicable treatment
data consistent with the type and quality of data needed by the
Agency in this program were used to make this determination. For
waste codes K103 and K104, the regulated constituents also
V
represent the BDAT list constituents present at the highest
concentrations. However, if the performance data for the
technology selected as BDAT indicated that the constituent was
7-5 Rev. 3
-------
not significantly treated, then that constituent was not
regulated. Some constituents present at treatable concentrations
in the untreated waste were not regulated if it was determined
that they would be adequately controlled by regulation of another
constituent.
Treatment standards for these wastes were derived after
correction of laboratory data to account for recovery
(Section 6). Subsequently, the mean of the corrected data points
was multiplied by a variability factor to derive the standards.
The variability factor corrects the lab data for reasonable
variations measured in the treatment process and imprecision in
sampling and analytical methods. Variability factors were
determined using a statistical method which accounts for
variability in the results for a number of data points for a
given constituent. A variability factor of 2.8 was chosen for
constituents for which a specific variability factor could not be
calculated (See Appendix A for justification).
Wastewater and nonwastewater forms of waste codes K103 and
K104 may be land disposed if they meet the concentration
standards at the point of disposal. The BOAT technology upon
which the treatment standards are based (liquid/liquid extraction
followed by steam stripping and activated carbon adsorption for
wastewater, and incineration for nonwastewater) need not be
specifically utilized prior to land disposal, provided that the
7-6 Rev. 3
-------
actual technology utilized meets the standard, does not involve
dilution or other methods deemed unacceptable by the Agency, and
does not pose a greater risk to human health and the environment
than land disposal.
These standards become effective as of August 8, 1988, as
per the schedule set forth in 40 CFR 268.10. The Agency
estimates that there is a lack of nationwide treatment capacity
at this time for the nonwastewater forms of waste codes K103 and
K104. Therefore, the Agency has proposed to grant a 2-year
nationwide variance to the effective date of the land disposal
ban for these wastes. A detailed discussion of the Agency's
determination that a lack of nationwide incineration capacity
exists is presented in the Capacity Background Document which is
available in the Administrative Record for the First Sixths7
Rule.
Consistent with Executive Order 12291, EPA prepared a
regulatory impact analysis (RIA) to assess the economic effect of
compliance with this proposed rule. The RIA prepared for this
proposal rule is available in the Administrative Record for the
First Sixths' Rule.
7-7 Rev. 3
-------
REFERENCES
Ackerman D.G., J.F. McGaughey, D.E. Wagoner, "At Sea Incineration
of PCB-Containing Wastes on Board the M/T Vulcanus." USEPA
600/7-83-024, April 1983.
Authur D. Little, Inc. (1977). "Physical, Chemical and
Biological Treatment Techniques for Industrial Wastes."
Vol. I - NTIS PB275-054. pp. 1-1 to 1-18 and 1-37 to 1-41.
Bonner T.A., et al., Engineering Handbook for Hazardous Waste
Incineration. SW889. Prepared by Monsanto Research
Corporation for U.S. EPA, NTIS PB 81-248163. June 1981.
De Renzo, D.J. (editor). (1978). Unit Operations for Treatment
of Hazardous Industrial Wastes. Noyes Data Corporation,
Park Ridge, New Jersey.
Enckenfelder, W., et al. (September 2,1985). "Wastewater
Treatment." Chemical Engineering.
Gallacher, Lawrence V. (February 1981). "Liquid Ion Exchange in
Metal Recovery and Recycling." 3rd Conference on Advanced
Pollution Control for the Metal Finishing Industry. U.S.
EPA 600/2-81-028. pp. 39-41.
GCA Corp. (October 1984). Technical Assessment of Treatment
Alternatives for Wastes Containing Halogenated Organics.
Prepared for USEPA, Contract 68-01-6871. pp. 150-160.
Hackman, Ellsworth. (1978). Toxic Organic Chemicals.
Destruction and Waste Treatment. Noyes Data Corporation,
Park Ridge, New Jersey, pp. 109-111.
Hanson, Carl. (August 26, 1968). "Solvent Extraction Theory,
Equipment, Commercial Operations, and Economics." Chemical
Engineering, p. 81.
Hutchins, R. (1979). "Activated Carbon Systems for Separation
of Liquids." pp. 1-415 through 1-486 as published in
Handbook of Separation Techniques for Chemical Engineers.
Philip A. Schweitzer (editor). McGraw-Hill.
Humphrey, Jimmy L., J. Antonia Rocha, and James R. Fair.
(September 17, 1984). "The Essentials of Extraction."
Chemical Engineering, pp. 76-95.
Kirk & Othmer. (1965). Encyclopedia of Chemical Technology.
2nd ed., Vol. 7, John Wiley and Sons, New York. pp. 204-
248.
Rev. 3
-------
REFERENCES (Continued)
Kirk & Othmer. Encyclopedia of Chemical Technology. Volume 2
(p. 37-361), Vol. 15 (p. 916-925).
Ku, W. and Peters, R.W. (May 1987). "Innovative Uses or Carbon
Adsorption of Heavy Metals from Plating Wastewaters:
I. Activated Carbon Polishing Treatment." Environmental
Progress.
Lo, Teh C., Malcolm H. I. Baird, and Carl Manson (editors). 1983.
Handbook of Solvent Extraction. John Wiley and Sons. New
York. pp. 53-89.
McCabe, Warren L., Julian C. Smith, and Peter Harriot. (1985).
Unit Operations of Chemical Engineering. McGraw-Hill Book
Company, New York. pp. 533-606.
Metcalf and Eddy Inc. (1985). "Briefing, Technologies
Applicable to Hazardous Waste." Prepared for USEPA, ORD,
HWERL. Section 2.13.
Mitre Corp. "Guidance Manual for Waste Incinerator Permits."
NTIS PB84-100577. July 1983.
Novak R.G., W.L. Troxler, T.H. Dehnke, "Recovering Energy from
Hazardous Waste Incineration." Chemical Engineering
Progress 91:146 (1984).
Oppelt E.T., "Incineration of Hazardous Waste." JAPCA, Volume
37, No. 5. May 1987.
Patterson, J. (1985). Industrial Wastewater Treatment
Technology. 2nd ed., Butterworth Pub. pp. 329-340.
Perry, Robert H. and Cecil H. Chilton. (1973). Chemical
Engineer's Handbook. 5th edition. McGraw-Hill Book Company,
New York. pp. 13-1 to 13-60 and pp. 15-1 to 15-24.
Rose, L.M. (1985). Distillation Design in Practice. Elsevier,
New York. pp. 1-307.
Santoleri J.J., "Energy Recovery-A By-Product of Hazardous Waste
Incineration Systems." In Proceedings of the 15th Mid-
Atlantic Industrial Waste Conference, on Toxic and Hazardous
Waste, 1983.
SRI. (1985). Stanford Research Institute. Chemical Economics
Handbook (CEH). Menlo Park. California.
Rev. 3
-------
REFERENCES (Continued)
Touhill, Shuckrow & Assoc. (February 1981). "Concentration
Technologies for Hazardous Aqueous Waste Treatment." NTIS
PB81-150583. pp. 53-55.
U. S. Environmental Protection Agency. (May 1981).
Identification and Listing Hazardous Waste under RCRA.
Subtitle C. Section 3001, Background Document.
U.S. EPA. (1987). Onsite Engineering Report of Treatment
Technology Performance and Operation for E.I, du Pont de
Nemours & Co.. Inc. - Beaumont. TX.
USEPA (October 1973). Process Design Manual for Carbon
Adsorption. NTIS PB227-157. pp. 3-21 and 53.
USEPA (1986). Best Demonstrated Available Technology (BOAT)
Background Document for F001-F005 Spent Solvents. Vol. 1.
EPA/530-SW-86-056, November, 1986.
Van Winkle, Matthew. (1967). Distillation. McGraw-Hill Book
Company, New York. pp. 1-684.
Versar (1985). Versar, Inc. An Overview of Carbon Adsorption.
Draft Final Report. U.S. Environmental Protection Agency:
Exposure Evaluation Division Office of Toxic Substances,
Washington, D.C. EPA Contract No. 68-02-3968, Task No. 58.
Vogel G., et al., "Incineration and Cement Kiln Capacity for
Hazardous Waste Treatment." In Proceedings of the 12th
Annual Research Symposium. Incineration and Treatment of
Hazardous Wastes. Cincinnati, Ohio. April 1986.
Water Chemical Corporation. (August 1984). Process Design Manual
of Stripping of Organics. NTIS PB84-232628. Prepared for
the Industrial Environmental Research Laboratory Office of
Research and Development, U.S. Environmental Protection
Agency. pp. 1-1 to F4.
Rev. 3
-------
-------
APPENDIX A - STATISTICAL ANALYSIS
A.1 F Value Determination for ANOVA Test
As noted earlier in Section 1.0, EPA is using the
statistical method known as analysis of variance in the
determination of the level of performance that represents "best"
treatment where more than one technology is demonstrated. This
method provides a measure of the differences between data sets.
If the differences are not statistically significant, the data
sets are said to be homogeneous.
If the Agency found that the levels of performance for one
or more technologies are not statistically different (i.e., the
data sets are homogeneous), EPA would average the long term
performance values achieved by each technology and then multiply
this value by the largest variability factor associated with any
of the acceptable technologies. If EPA found that one technology
performs significantly better (i.e., the data sets are not
homogeneous), BDAT would be the level of performance achieved by
the best technology multiplied by its variability factor.
To determine whether any or all of the treatment performance
V
data sets are homogeneous using the analysis of variance method,
it is necessary to compare a calculated "F value" to what is
known as a "critical value." (See Table A-l.) These critical
Appendix A-l Rev. 3
-------
values are available in most statistics texts (see, for example,
Statistical Concepts and Methods by Bhattacharyya and Johnson,
1977, John Wiley Publications, New York).
Where the F value is less than the critical value, all
treatment data sets are homogeneous. If the F value exceeds the
critical value, it is necessary to perform a "pair wise F" test
to determine if any of the sets are homogeneous. The "pair wise
F" test must be done for all of the various combinations of data
sets using the same method and equation as the general F test.
The F value is calculated as follows:
(i) All data are natural logtransformed.
(ii) The sum of the data points for each data set is
computed (T.) .
(iii) The statistical parameter known as the sum of the
squares between data sets (SSB) is computed:
SSB =
k
I
i = l
i i
r Ti2i
n •
1
—
f I T-'
i=l
N
Z •
where:
k = number of treatment technologies
n. = number of data points for technology i
N = number of data points for all technologies
T. = sum of natural logtransformed data points for each
technology.
Appendix A-2
Rev. 3
-------
(iv) The sum of the squares within data sets (SSW) is
computed:
SSW =
k n;
l
I X
. 1=1 j=l
"
*2i,j
k
-.1
i s 1
' T •
ni -
where:
x. . = the natural logtransformed observations (j) for
1'-1 treatment technology (i) .
(v) The degrees of freedom corresponding to SSB and SSW are
calculated. For SSB, the degree of freedom is given by
k-1. For SSW, the degree of freedom is given by N-k.
(vi) Using the above parameters, the F value is calculated
as follows:
MSB
F = MSW
where:
MSB = SSB/(k-1) and
MSW = SSW/(N-k).
Appendix A-3
Rev. 3
-------
A computational table summarizing the above parameters is
shown below.
Computational Table for the F Value
Source
Between
Within
Degrees of
freedom
K-l
N-k
Sum of
squares
SSB
SSW
Mean square
MSB = SSB/k-1
MSW = SSW/N-k
F
MSB/MSW
Below are three examples of the ANOVA calculation. The
first two represent treatment by different technologies that
achieve statistically similar treatment; the last example
represents a case where one technology achieves significantly
better treatment than the other technology.
Appendix A-4
Rev. 3
-------
Table A-l
F Distribution at the 95 Percent Confidence Level
Denominator
degree! of
freedom 1
1
2
3
4
S
6
7
8
9
10
11
12
13
14
15
16
' 17
18
19
20
21
22
23
24
25
26
27
28
29
30
40
60
120
00
161 4
1851
1013
7 71
661
599
559
532
5.12
496
484
4 75
467
460
454
449
445
4 41
438
435
432
430
428
426
424
423
421
420
4 18
417
408
400
392
3.84
2
1995
1900
955
694
579
5.14
474
446
426
410
398
389
381
374
368
363
359
355
352
349
347
344
3.42
340
3.39
337
335
334
333
3.32
323
3.15
307
300
Numerator degrees of freedom
34567
2157
1916
928
659
5.41
4 76
435
407
386
3.71
3 59
349
341
334
329
324
320
316
313
310
307
305
303
301
299
298
296
295
2.93
292
284
2.76
2.68
2.60
2246
1925
912
639
5.19
453
412
384
363
348
336
3.26
3.18
311
306
301
296
293
290
287
284
282
280
278
276
274
273
271
2.70
269
2.61
253
245
237
2302
19.30
901
626
5.05
439
397
3.69
3.48
3.33
320
311
3.03
2.96
290
2.85
2.81
2.77
274
271
268
266
2.64
262
260
259
257
256
255
253
2.45
237
2.29
2.21
2340
1933
894
616
495
428
3.87
3.58
337
3.22
3.09
3.00
2.92
2.85
2.79
2.74
2.70
266
263
260
2.57
255
2.53
2.51
249
247
246
2.45
243
2.42
234
2.25
2.17
2.10
2368
1935
889
609
488
421
3.79
3.50
3.29
3.14
3.01
2.91
2.83
2.76
2.71
2.66
2.61
2.58
2.54
2.51
249
2.46
244
242
2.40
2.39
2.37
2.36
2.35
2.33
225
* 2.17
2.09
2.01
8
2389
1937
885
604
482
415
3.73
344
3.23
3.07
2.95
2.85
2.77
2.70
2.64
2.59
2.55
2.51
2.48
2.45
2.42
2.40
2.37
236
234
2.32
231
2.29
2.28
2.27
2.18
2.10
2.02
1 94
9
2405
1938
881
600
477
410
368
339
3.18
302
290
280
2.71
265
259
254
249
246
242
239
237
234
232
2.30
228
2.27
225
224
2.22
221
212
204
1 96
188
Appendix A-5
Rev. 3
-------
Example 1
Hethylene Chloride
Steam stripping
Influent
(mg/l)
1550.00
1290.00
1640.00
5100.00
1450.00
4600.00
1760.00
2400.00
4800.00
12100.00
Effluent
(mg/l)
10.00
10.00
10.00
12.00
10.00
10.00
10.00
10.00
10.00
10.00
In(effluent)
2.30
2.30
2.30
2.48
2.30
2.30
2.30
2.30
2.30
2.30
2
[ln(ef fluent)]
5.29
5.29
5.29
6.15
5.29
5.29
5.29
5.29
5.29
5.29
Influent
(mg/l)
1960.00
2568.00
1817.00
1640.00
3907.00
Biological treatment
Effluent In(effluent)
(mg/l)
10.00 2.30
10.00 2.30
10.00 2.30
26.00 3.26
10.00 2.30
2
tln( effluent)]
5.29
5.29
5.29
10.63
5.29
Sum:
23.18
53.76
12.46
31.79
Sample Size:
10 10
10
Mean:
3669
10.2
Standard Deviation:
3328.67 .63
Variability Factor:
1.15
2.32
.06
2378
923.04
13.2
7.15
2.48
2.49
.43
ANOVA Calculations:
SSB
£ 'Ti2
k
.2,
SSW
MSB = SSB/(k-1)
MSU = SSU/(N-k)
A"
Hi
nt
Appendix A-6
Rev. 3
-------
Example 1 (continued)
F = MSB/MSW
where:
k = number of treatment technologies
n. = number of data points for technology i
N = number of natural log transformed data points for alt technologies
T. = sum of log transformed data points for each technology
X = the nat. log transformed observations (j) for treatment technology (i)
ij
n = 10, n2 = 5, N = 15, k = 2, T = 23.18, T = 12.46, T = 35.64, T = 1270.21
T = 537.31 T = 155.25
„„„
SSB
537.31 155.25
10 5
1270.21
15
= 0.10
(53.76 + 31.79) -
10
= 0.77
MSB = 0.10/1 = 0.10
MSW = 0.77/13 = 0.06
0.10
F =
0.06
= 1.67
Source
Degrees of
freedom
Between(B)
Uithin(U)
1
13
ANOVA Table
SS
0.10
0.77
MS
0.10
0.06
1.67
The critical value of the F test at the 0.05 significance level is 4.67. Since the
F value is less than the critical value, the means are not significantly different
(i.e., they are homogeneous).
Note: All calculations were rounded to two decimal places. Results may differ
depending upon the number of decimal places used in each step of the calculations.
Appendix A-7
Rev. 3
-------
Example 2
Trichloroethylene
Steam stripping
Influent
(mg/l)
1650.00
5200.00
5000.00
1720.00
1560.00
10300.00
210.00
1600.00
204.00
160.00
Effluent
(mg/l)
10.00
10.00
10.00
10.00
10.00
10.00
10.00
27.00
85.00
10.00
In(effluent)
2.30
2.30
2.30
2.30
2.30
2.30
2.30
3.30
4.44
2.30
2
[In(effluent)]
5.29
5.29
5.29
5.29
5.29
5.29
5.29
10.89
19.71
5.29
Biological treatment
Influent
(mg/l)
200.00
224.00
134.00
150.00
484.00
163.00
182.00
Effluent
(mg/l)
10.00
10.00
10.00
10.00
16.25
10.00
10.00
ln( effluent)
2.30
2.30
2.30
2.30
2.79
2.30
2.30
2
Cln( effluent)]
5.29
5.29
5.29
5.29
7.78
5.29
5.29
Sum:
Sample Size:
10 10
Mean:
2760
19.2
Standard Deviation:
3209.6 23.7
Variability Factor:
3.70
26.14
10
2.61
.71
72.92
220
120.5
10.89
2.36
1.53
16.59
2.37
.19
39.52
ANOVA Calculations:
SSB
Ti?
k
z, . _
i-l n,
SSW '
MSB = SSB/(k-1)
MSW = SSW/(N-k)
Z, Ti
•&(£)
Appendix A-8
Rev. 3
-------
Example 2 (continued)
F = HSB/MSW
where:
k = number of treatment technologies
n. = number of data points for technology i
M = number of data points for all technologies
T = sum of natural log transformed data points for each technology
i
X = the natural log transformed observations (j) for treatment technology (i)
U
N = 10, N = 7, N = 17, k = 2, T = 26.14, T = 16.59, T = 42.73, T = 1825.85, T = 683.30,
I2 = 275.23
SSB »[683'30 * 275'23 - ' - 0.25
10 7 I 17
SSWM72.92 + 39.52) - LIi::*-—! = *'79
I 10 7
MSB = 0.25/1 = 0.25
MSU = 4.79/15 = 0.32
0.32
ANOVA Table
Source
Between(B)
Within(W)
Degrees of
freedom SS MS f
1 0.25 0.25 0.78
15 4.79 0.32
The critical value of the f test at the 0.05 significance level is 4.54. Since the
F value is less than the critical value, the means are not significantly different
(i.e., they are homogeneous).
Note: All calculations were rounded to two decimal places. Results may differ
depending upon the number of decimal places used in each step of the calculations.
Appendix A-9 Rev. 3
-------
Example 3
Chlorobenzene
Activated sludge
followed by carbon adsorption
2
Influent Effluent In(effluent) [InCeff luent)]"
(mg/l)
7200.00
6500.00
6075.00
3040.00
(mg/l)
80.00 4.38 19.18
70.00 4.25 18.06
35.00 3.56 12.67
10.00 2.30 5.29
Biological
Influent
(mg/l)
9206.00
16646.00
49775.00
14731.00
3159.00
6756.00
3040.00
treatment
Effluent
(mg/l)
1083.00
709.50
460.00
142.00
603.00
153.00
17.00
ln( effluent)
6.99
6.56
6.13
4.96
6.40
5.03
2.83
2
InC(effluent)]
48.86
43.03
37.58
24.60
40.96
25.30
8.01
Sum:
Sample Size:
4
Mean:
5703
49
Standard Deviation:
1835.4 32.24
Variability Factor:
7.00
14.49
55.20
3.62
.95
14759
16311.86
452.5
379.04
15.79
38.90
5.56
1.42
228.34
ANOVA Calculations:
SSB
ssw
n.
-1 J.1
MSB = SSB/(k-1)
MSW = SSW/(N-k)
F = MSB/HSW
-i fid]
i=l I nTj
Appendix A-10
Rev. 3
-------
Example 3 (continued)
where,
k = lumber of treatment technologies
n. = number of data points for technology i
N = number of data points for all technologies
T. = sun of natural log transformed data points for each technology
X = the natural log transformed observations (j) for treatment technology (i)
ij
N = 4, N = 7, N = 11, k = 2, T = 14.49, T = 38.90, T = 53.39, J2= 2850.49, T2 = 209.96
T2 = 1513.21
(209.96 1513.21 } 2850.49
SS8 "! + I - = 9.52
11
. 209.96 1513.2H
SSW = (55.20 + 228.34) - + =14.88
MSB = 9.52/1 = 9.52
MSW = 14.88/9 = 1.65
F = 9.52/1.65 = 5.77
ANOVA Table
Degrees of
Source freedom
Between(B) 1
Uithin(U) 9
SS MS F
9.53 9.53 5.77
14.89 1.65
The critical value of the F test at the 0.05 significance level is 5.12. Since the
F value is larger than the critical value, the means are significantly different
(i.e., they are heterogeneous).
Note: All calculations were rounded to two decimal places. Results may differ depending
upon the number of decimal places used in each step of the calculations.
Appendix A-ll Rev. 3
-------
A.2. Variability Factor
C99
VF = Mean
where:
VF = estimate of daily maximum variability factor
determined from a sample population of daily data.
Cgg = Estimate of performance values for which 99 percent
of the daily observations will be below. C is
calculated using the following equation:
C = Exp(y +2.33 Sy) where y and Sy are the mean
and standard deviation, respectively, of the
logtransformed data.
Mean = average of the individual performance values.
EPA is establishing this figure as an instantaneous maximum
because the Agency believes that on a day-to-day basis the waste
should meet the applicable treatment standards. In addition,
establishing this requirement makes it easier to check compliance
on a single day. The 99th percentile is appropriate because it
accounts for almost all process variability.
In several cases, all the results from analysis of the
residuals from BOAT treatment are found at concentrations less
than the detection limit. In such cases, all the actual
concentration values are considered unknown and hence, cannot be
used to estimate the variability factor of the analytical
results. Below is a description of EPA's, approach for
calculating the variability factor for such cases with all
concentrations below the detection limit.
Appendix A-12 Rev. 3
-------
It has been postulated as a general rule that a lognormal
distribution adequately describes the variation among
concentrations. Therefore, the lognormal model has been used
routinely in the EPA development of numerous regulations in the
Effluent Guidelines program and is being used in the BDAT
program. The variability factor (VF) was defined as the ratio of
the 99th percentile (C_q) of the lognormal distribution to its
arithmetic mean (Mean) .
VF = 99 (1)
Mean
The relationship between the parameters of the lognormal
distribution and the parameters of the normal distribution
created by taking the natural logarithms of the
lognormally-distributed concentrations can be found in most
mathematical statistics texts (see for example: Distribution in
Statistics-Volume 1 by Johnson and Kotz, 1970) . The mean of the
lognormal distribution can be expressed in terms of the mean (ju. )
and standard deviation ( g- ) of the normal distribution as
follows:
Cgg = Exp ( JU + 2.334CT) (2)
Mean = Exp ( ^ + • 54
-------
VF = Exp (2.33 CT - .54cr2) (4)
For residuals with concentrations that are not all below the
detection limit, the 99th percentile and the mean can be
estimated from the actual analytical data and accordingly, the
variability factor (VF) can be estimated using equation (1). For
residuals with concentrations that are below the detection limit,
the above equations can be used in conjunction with the
assumptions below to develop a variability factor.
Step 1: The actual concentrations follow a lognormal
distribution. The upper limit (UL) is equal to the detection
limit. The lower limit (LL) is assumed to be equal to one tenth
of the detection limit. This assumption is based on the fact
that data from well-designed and well-operated treatment systems
generally falls within one order of magnitude.
Step 2: The natural logarithms of the concentrations have a
normal distribution with an upper limit equal to In (UL) and a
lower limit equal to In (LL).
Step 3: The standard deviation ( cr ) of the normal distribution
is approximated by
V
CT = [(In (UL) - In (LL)] / [(2)(2.33)] = [ln(UL/LL)] /4.66
when LL = (0.1) (UL) then cr = (InlO) / 4.66 = 0.494
Appendix A-14 Rev. 3
-------
Step 4: Substitution of the value from Step 3 in equation (4)
yields the variability factor, VF.
VF = 2.8
Appendix A-15 Rev. 3
-------
APPENDIX B - ANALYSIS OF VARIANCE TESTS
ANOVA #1
Comparison of L/L Extraction with L/L Extraction Followed by
Steam Stripping
Compare sample point SD-5 (Untreated Waste to Steam Stripper)
with sample point SD-6 (Treated Waste From Steam Stripper)
Regulated Constituents: Benzene
Nitrobenzene
2,4-Dinitrophenol
Phenol
Aniline
Cyanide
Regulated Constituents Present in Untreated Waste (SD-5):
Benzene
Nitrobenzene
Cyanide
Regulated Constituents Present in Treated Waste (SD-6):
Benzene
2,4-Dinitrophenol (*)
Cyanide
* - An ANOVA analysis could not be completed on this
constituent, since no information is available on the
concentration of this constituent in the untreated waste
(SD-5).
Appendix B - 1 Rev. 3
-------
1) Benzene (ug/1)
AF = 1.32
Raw SD-5
Corr. SD-5
Raw SD-6
Corr. SD-6
170,000
224,400
(5)
6.6
2) Nitrobenzene (ug/1)
AF = 0.87
Raw SD-5
Corr. SD-5
Raw SD-6
Corr. SD-6
3) Cyanide (mg/1)
AF = 1.39
190,000
250,800
8
10.6
26,000
34,320
(5)
6.6
17,000
22,440
(5)
6.6
2.3X106
2.0X106
(3000)
2610
2.8X106
2.4X106
(3000)
2610
2.0X106
1.7X106
(1500)
1305
2.0X10
1.7x10
(3000)
2610
Raw SD-5 4.36
Corr. SD-5 6.06
3.45
4.80
2.54
3.53
2.27
3.16
Raw SD-6 4.77
Corr. SD-6 6.63
3.87
5.38
2.08
2.89
1.70
2.36
Note; Numbers in parentheses indicate that the compound was
not detected in this sample. The detection limit has
been used in place of the actual value for this
compound.
(Above raw values are taken from the EPA's Onsite Engineering
Report for K103 and K104. Tables 6-10 and 6-11).
Appendix B - 2
Rev. 3
-------
1) Benzene
Treatment 1 Treatment 2 x1— x2_
SSI 224,400 6.6 12.32 1.89
SS2 250,800 10.6 12.43 2.36
SS4 34,320 6.6 10.44 1.89
SS5 22,440 6.6 10.02 1.89
k = 2
n^ = 4 n2 = 4
N = 8
SSB = (T12/n1 + T22/n2) - T2/N
= (2043.94/4 + 64.48/4) - 2834.5/8
= (510.99 +16.12) - 354.31
= 527.11 - 354.31
= 172/80
MSB = SSB/k-1 = 172.80/1 = 172.80
SSW = E E Xi i2 - 527.11
= 531.97- 527.11
= 4.86
MSW = SSW/N-k = 4.86/6 =0.81
F = MSB/MSW = 172.80/0.81 = 213.3
Fk-l N-k = Fl 6 = 5-" (critical value for 95% confidence)
Appendix B - 3 Rev. 3
-------
2) Nitrobenzene
Treatment 1 Treatment 2 _x1 x2
SSI 2.00X106 2610 14.51 7.87
SS2 2.44X106 2610 14.71 7.87
SS4 1.74X106 1305 14.37 7.17
SS5 1.74X106 2610 14.37 7.87
k = 2
nl = 4 n2 = 4
N = 8
SSB = (T12/n1 + T22/n2) - T2/N
= (3359.36/4 + 947.41/4) - 7874.79/8
= (839.84 + 236.85) - 984.35
= 1076.69 - 984.35
= 92.34
MSB = SSB/k-1 = 92.34/1 = 92.34
SSW = E E Xi j2 - 1076.69
= 1077.l4 - 1076.69
= .45
MSW = SSW/N-k = 0.45/6 =0.08
F = MSB/MSW = 92.34/0.08 = 1154.25
Fk-l N-k = Fl 6 = 5-99 (critical value for 95% confidence)
Appendix B - 4 Rev. 3
-------
3) Cyanide
Treatment 1 Treatment 2 _xi_ X2
SSI 6.06 6.63 1.80 1.89
SS2 4.80 5.38 1.57 1.68
SS4 3.53 2.89 1.26 1.06
SS5 3.16 2.36 1.15 0.86
k = 2
n^ = 4 n2 = 4
N = 8
SSB = (T12/n1 + T22/n2) - T2/N
= (33.41/4 + 30.14/4) - 127.01/8
= (8.35 + 7.54) - 15.88
= 15.89 - 15.88
= 0.01
MSB = SSB/k-1 = 0.01/1 =0.01
SSW = E E Xi i2 - 15.89
= 16.87 - 15.89
= 0.98
MSW = SSW/N-k = 0.98/6 =0.16
F = MSB/MSW = 0.01/0.16 =0.06
^k-1 N-k = Fl 6 = 5.99 (critical value for 95% confidence)
Appendix B - 5 Rev. 3
-------
Computational Table for the F Value
Constituent
Benzene
Nitrobenzene
Total Cyanides
Source
Between
Within
Between
Within
Between
Within
Sum of
Squares
172.80
4.86
92.34
0.45
0.01
0.98
Degrees of
Freedom
1
6
1
6
1
6
Mean
Square
172.80
0.81
92.34
0.08
0.01
0.16
F
213.3*
1154.25*
0.06
* - Indicates that the calculated F value exceeds the critical value.
Conclusion
L/L Extraction followed by steam stripping is more efficient at
reducing the concentration of benzene and nitrobenzene in
K103/K104 than L/L extraction alone, but is not more efficient at
reducing the concentration of total cyanides in K103/K104 than
L/L extraction alone.
Appendix B - 6
Rev. 3
-------
ANOVA #2
Comparison of L/L Extraction Followed by Steam Stripping with L/L
Extraction Followed by Steam Stripping Followed by Activated
Carbon Adsorption
Compare sample point SD-8 (Untreated Waste to Activated Carbon
Adsorption Beds) with sample point SD-9 (Treated Waste from
Carbon Adsorption System)
Regulated Constituents: Benzene
Nitrobenzene
2,4-Dinitrophenol
Phenol
Aniline
Cyanide
Regulated Constituents Present in Untreated Waste (SD-8):
Benzene
Aniline
2,4-Dinitrophenol
Phenol
Cyanide
Regulated Constituents Present in Treated Waste (SD-9):
Benzene
Aniline
2,4-Dinitrophenol
Phenol
Cyanide
Appendix B - 7 Rev. 3
-------
1) Benzene (ug/1)
AF = 1.32
Raw SD-8
Corr. SD-8
Raw SD-9
Corr. SD-9
880
1161.60
42
55.44
2) Aniline (ug/1)
AF = 1.10
Raw SD-8
Corr. SD-8
Raw SD-9
Corr. SD-9
57000
62700
(30)
33
130
171.60
(5)
6.6
ND
ND
(30)
33
3) 2,4-Dinitrophenol (ug/1)
AF = 1.25
39
51.48
19
25.08
56000
61600
(30)
33
20
26.40
11
14.52
300000
330000
960
1056
Raw SD-8
Corr. SD-8
53000
66250
ND
ND
24000
30000
24000
30000
Raw SD-9 380
Corr. SD-9 475
320
400
260
325
230
288
Numbers in parentheses indicate that the compound was
not detected in this sample. The detection limit has
been used in place of the actual value for this
compound. "ND" indicates that this compound was not
detected in the untreated waste (SD-8), and hence this
reading was not used in the ANOVA calculations.
Appendix B - 8
Rev. 3
-------
4) Phenol (ug/1)
AF = 4.76
Raw SD-8 ND
Corr. SD-8 ND
29000
138040
39000
185640
41000
195160
Raw SD-9 (30)
Corr. SD-9 142.8
(30)
142.8
(30)
142.8
150
714
5) Cyanide (mg/1)
AF = 1.39
Raw
Corr.
SD-8
SD-8
1
6.850
9.52
4.590
6.38
3.470
4.82
0.952
1.32
Raw SD-9
Corr. SD-9
0.565
0.79
0.597
0.83
0.156
0.22
0.129
0.18
Note; Numbers in parentheses indicate that the compound was
not detected in this sample. The detection limit has
been used in place of the actual value for this
compound. "ND" indicates that this compound was not
detected in the untreated waste (SD-8), and hence this
reading was not used in the ANOVA calculations.
(Above raw values are taken from the EPA's Onsite Engineering
Report for K103 and K104. Tables 6-13 and 6-14).
Appendix B - 9
Rev. 3
-------
1) Benzene
Treatment 1 Treatment 2 _*i_ x2
SSI 1161.6 55.4 7.06 4.01
SS2 171.6 6.6 5.15 1.89
SS4 51.5 25.1 3.94 3.22
SS5 26.4 14.5 3.27 2.67
k = 2
nl = 4 n2 = 4
N = 8
SSB = (T12/n1 + T22/n2) - T2/N
= (377.14/4 + 139.00/4) - 974.06/8
= (94.29 + 34.75) - 121.76
= 129.04 - 121.76
= 7.28
MSB = SSB/k-1 = 7.28/1 =7.28
SSW = E E Xi -j2 - 129.04
- 139.73- 129.04
= 10.69
MSW = SSW/N-k = 10.69/6 =1.78
F = MSB/MSW = 7.28/1.78 =4.09
Fk-l,N-k = Fl,6 = 5-99 (critical value for 95% confidence)
Appendix B - 10 Rev. 3
-------
2) Aniline
Treatment 1 Treatment 2
SSI 62700 33 11.05 3.50
SS2 ND 33 ND 3.50
SS4 61600 33 11.03 3.50
SS5 330000 1056 12.71 6.96
k = 2
n^ = 3 r\2 = 4
N = 7
SSB = (T12/n1 + T22/n2) - T2/N
= (1210.34/3 + 304.85/4) - 2730.06/7
= (403.45 + 76.21) - 390.01
= 479.66 - 390.01
= 89.65
MSB = SSB/k-1 = 89.65/1 = 89.65
SSW = E E Xji2 - 479.66
= 490.49- 479.66
= 10.83
MSW = SSW/N-k = 10.83/5 =2.17
F = MSB/MSW = 89.65/2.17 = 41.31
Fk-l N-k ~ Fl 5 = 6-61 (critical value for 95% confidence)
Appendix B - 11 Rev. 3
-------
3) 2,4-Dinitrophenol
Treatment 1 Treatment 2 x^_ x2
SSI 66250 475 11.10 6.16
SS2 ND 400 ND 5.99
SS4 30000 325 10.31 5.78
SS5 30000 288 10.31 5.66
k = 2
HI = 3 n2 = 4
N = 7
SSB = (T^/n! + T22/n2) ~ T2/N
= (1006.16/3 + 556.49/4) - 3059.20/7
= (335.39 + 139.12) - 437.03
= 474.51 - 437.03
= 37.48
MSB = SSB/k-1 = 37.48/1 = 37.48
SSW = E E Xi -j2 - 474.51
= 475.07 - 474.51
= 0.56
MSW = SSW/N-k = 0.56/5 =0.11
F = MSB/MSW = 37.48/0.11 = 340.73
Fk-l,N-k = Fl,5 = 6.61 (critical value for 95% confidence)
Appendix B - 12 Rev. 3
-------
4) Phenol
Treatment 1 Treatment 2 x1— x2
SSI ND 142.8 ND 4.96
SS2 138040 142.8 11.84 4.96
SS4 185640 142.8 12.13 4.96
SS5 195160 714.0 12.18 6.57
k = 2
R! = 3 n2 = 4
N = 7
SSB = (T12/n1 + T22/n2) - T2/N
= (1306.82/3 + 460.10/4) - 3317.76/7
= (435.61 + 115.02) - 473.97
= 550.63 - 473.97
= 76.66
MSB = SSB/k-1 = 76.66/1 = 76.66
SSW = E E Xji2 - 550.63
= 552.64- 550.63
= 2.01
MSW = SSW/N-k = 2.01/5 =0.40
F = MSB/MSW = 76.66/0.40 = 191.65
Fk-l N-k = Fl 5 = 6-61 (critical value for 95% confidence)
Appendix B - 13 Rev. 3
-------
5) Cyanide
Treatment 1 Treatment 2 Xj x2_
SSI 9.52 0.79 2.25 -0.24
SS2 6.38 0.83 1.85 -0.19
SS4 4.82 0.22 1.57 -1.51
SS5 1.32 0.18 0.28 -1.71
k = 2
n± = 4 n2 = 4
N = 8
SSB = (T^/n! + T22/n2) - T2/N
= (35.4/4 + 13.3/4) - 5.29/8
= (8.85 + 3.33) - 0.66
= 12.18 - 0.66
= 11.52
MSB = SSB/k-1 = 11.52/1 = 11.52
SSW = E E Xi -j2 - 12.18
= 16.33 - 12.18
= 4.15
MSW = SSW/N-k = 4.15/6 =0.69
F = MSB/MSW = 11.52/0.69 = 16.70
Fk-l,N-k = Fl 6 = 5-99 (critical value for 95% confidence)
Appendix B - 14 Rev. 3
-------
Computational Table for the F Value
Constituent
Benzene
Aniline
2,4-Dinitro-
phenol
Phenol
Total Cyanides
Source
Between
Within
Between
Within
Between
Within
Between
Within
Between
Within
Sum of
Squares
7.28
10.69
89.65
10.83
37.48
0.56
76.66
2.01
11.52
4.15
Degrees of
Freedom
1
6
1
5
1
5
1
5
1
6
Mean
Square
7.28
1.78
89.65
2.17
37.48
0.11
76.66
0.40
11.52
0.69
F
4.09
41.31*
340.73*
191.65*
16.70*
* - Indicates that the calculated F value exceeds the critical value.
Conclusion
L/L extraction followed by steam stripping and activated carbon
adsorption is more efficient at reducing the concentration of
aniline, 2,4-dinitrophenol, phenol and cyanide in K103/K104 than
L/L extraction followed by steam stripping alone, but is not more
efficient at reducing the concentration of benzene in K103/K104
than L/L extraction followed by steam stripping alone.
Appendix B - 15
Rev. 3
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 1
(D
3
a
H-
X
o
I
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
BOAT
CONSTITUENT
VOLATILE ORGANICS(ug/L)
Acetonitrile
Acrolein
Acrylonitrile
Benzene
Bromodichloromethane
Bromomethane
Carbon Tetrachloride
Carbon Disulfide
Chlorobenzene
2-Chloro-l, 3-Butadiene
Chlorodibromomethane
Chloroethane
2-Chloroethylvinylether
Chloroform
Chloromethane
3 -Chloropropene
1 , 2-Dibromo-3-Chloropropane
1 , 2-Dibromoethane
Dibromomethane
Trans-1 , 4-Dichloro-2-Butene
Dichlorodif luoromethane
1, 1-Dichloroethane
1 , 2-Dichloroethane
1 , 1-Dichloroethene
Trans-1 , 2-Dichloroethene
1 , 2-Dichloropropane
Trans-1 , 3-Dichloropropene
cis-1 , 3 , Dichloropropene
1 , 4-Dioxane
Ethyl Cyanide
Ethyl Methacrylate
lodomethane
Isobutyl Alcohol
Methyl ethyl ketone
Methyl Methacrylate
UNTREATED
K103
10000
10000
10000
500
500
1000
500
500
500
10000
500
1000
1000
500
1000
10000
1000
500
500
10000
1000
500
500
500
500
500
500
500
20000
10000
10000
5000
20000
10000
10000
UNTREATED
K104
10000
10000
10000
500
500
1000
500
500
500
10000
500
1000
1000
500
1000
10000
1000
500
500
10000
1000
500
500
500
500
500
500
500
20000
10000
10000
5000
20000
10000
10000
TREATED
K103 & K104
100
100
100
5
5
10
5
5
5
100
5
10
10
5
10
100
10
5
5
100
10
5
5
5
5
5
5
5
200
100
100
50
200
100
100
(Continued)
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 1
X
o
I
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
BOAT
CONSTITUENT
VOLATILE ORGANICS (ug/L) (Continued)
Methyl Methanesulfonate*
Methacrylonitrile
Methylene Chloride
Pyridine
1,1,1,2 -Tetrachloroe thane
1,1,2, 2-Tetrachloroethane
Tetrachloroethene
Toluene
Tribromome thane
1,1, 1-Trichloroethane
1,1, 2-Trichloroethane
Trichloroethene
Trichloromonof luoromethane
1,2, 3-Trichloropropane
Vinyl Chloride
SEMI -VOLATILE ORGANICS (ug/L)
Acenaphthalene
Acenaphthene
Acetophenone
2-Acetylaminofluorene
4-Aminobiphenyl
Aniline
Anthracene
Aramite
Benzo (a) anthracene
Benzenethiol
Benzidine
Benzo ( a ) py rene
Benzo (b) fluoranthene
UNTREATED
K103
ND
10000
500
40000
500
500
500
500
500
500
500
500
500
500
1000
1500000
1500000
3000000
3000000
3000000
1500000
1500000
NA
1500000
ND
7500000
1500000
1500000
UNTREATED
K104
ND
10000
500
40000
500
500
500
500
500
500
500
500
500
500
1000
150000
150000
300000
300000
300000
150000
150000
NA
150000
ND
750000
150000
150000
TREATED
K103 & K104
ND
100
5
400
5
5
5
5
5
5
5
5
5
5
10
30
30
60
60
60
30
30
NA
30
ND
150
30
30
(Continued)
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 1
T)
(D
H-
X
O
I
u>
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
93
94
95
96
BOAT
CONSTITUENT
UNTREATED
K103
UNTREATED
K104
TREATED
K103 & K104
SEMI-VOLATILE ORGANICS (ug/L) (Continued)
Benzo(g,h,i) perylene
Benzo(k) fluoranthene
p-Benzoquinone
Bis (2-Chloroethoxy) methane
Bis (2 -Chloroethy 1) Ether
Bis (2-chloroisopropyl) ether
Bis(2-ethylhexyl) phthalate
4-Bromophenyl phenyl ether
Butyl benzyl phthalate
2-Sec-Butyl-4 , 6-Dinitrophenol
p-Chloroaniline
Chi orobenzi late
p-Chloro-m-cresol
2 -Chloronaphthalene
2 -Chlorophenol
3-Chloropropionitrile
Chrysene
Ortho-cresol
para-cresol
Dibenz (a,h) anthracene
Dibenzo (a,e, ) Pyrene
Dibenzo(a,i) Pyrene
1 , 3-Dichlorobenzene
1 , 2-Dichlorobenzene
1 , 4-Dichlorobenzene
3,3' Dichlorobenzidine
2 , 4-Dichlorophenol
2 , 6-Dichlorophenol
Diethyl phthalate
3,3' -Dimethoxybenzidine
p-Dimethylaminoazobenzene
3,3' -Dimethylbenzidine
2 , 4-Dimethylphenol
1500000
1500000
ND
1500000
1500000
1500000
1500000
1500000
1500000
7500000
1500000
NA
1500000
1500000
1500000
NA
1500000
1500000
1500000
1500000
NA
NA
1500000
1500000
1500000
3000000
1500000
ND
1500000
1500000
3000000
ND
1500000
150000
150000
ND
150000
150000
150000
150000
150000
150000
750000
150000
NA
150000
150000
150000
NA
150000
150000
150000
150000
NA
NA
150000
150000
150000
300000
150000
ND
150000
150000
300000
ND
150000
30
30
ND
30
30
30
30
30
30
150
30
NA
30
30
30
NA
30
30
30
30
NA
NA
30
30
30
60
30
ND
30
30
60
ND
30
(Continued)
-------
Q
W
EH
W
OH
EH
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w 3
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EH O
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2 W
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L. <
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OH 5
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C*-t O
w
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H EH
Q
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EH
W
Q
U
X
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Q
2
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OH
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Appendix C - 5
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 1
•a
3
a
H-
X
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**
**
154
155
156
157
158
159
160
161
162
163
164
165
166
167
168
BOAT
CONSTITUENT
SEMI-VOLATILE ORGANICS (ug/L)
3-Nitroaniline
2-Nitrophenol
METALS (ug/L)
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Mercury
Nickel
Selenium
Silver
Thallium
Vanadium
Zinc
UNTREATED
K103
(Continued)
7500000
1500000
32.0
10.0
1.0
1.0
4.0
7.0
6.0
5.0
20.0
11.0
5.0
6.0
10.0
6.0
2.0
UNTREATED
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750000
150000
32.0
10.0
1.0
1.0
4.0
7.0
6.0
50.0
20.0
11.0
500.0
6.0
10.0
6.0
2.0
TREATED
K103 & K104
150
30
32.0
10.0
1.0
1.0
4.0
7.0
6.0
500.0
20.0
11.0
50.0
6.0
1000.0
6.0
2.0
ND - Constituent was not Detected, however, a matrix detection limit has not
been determined.
NA - The standard is not available;compound was searched using an NBS library of
42,000 compounds.
* - This constituent was analyzed as a semivolatile by Method 8270. The Generic Quality
Assurance Project Plan for Land Disposal Restrictions Program("BOAT"),EPA/530-SW-87
-Oil,March 1987,lists this compound as a Volatile ,however,it may be analyzed as
either a volatile or semivolatile organic
** - This constituent is not on the list of constituents in the Generic
Quality Assurance Project Plan for Land Disposal Restrictions Program ("BOAT"),
EPA/530-SW-011,March 1987. It is a ground-water monitoring constituent as listed
in Appendix IX, Page 26639, of the Fedral Register,Vol. 51, No.142.
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-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 2
>
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1
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36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
BOAT
CONSTITUENT
VOLATILE ORGANICS (ug/L)
Methyl Methanesul f onate*
Methacrylonitrile
Methylene Chloride
Pyridine
1,1,1,2 -Tetrachloroethane
1,1,2, 2 -Tetrachloroethane
Tetrachloroethene
Toluene
Tribromomethane
1,1, 1-Trichloroethane
1,1, 2-Trichloroethane
Trichloroethene
Trichloromonof luoromethane
1,2, 3 -Tr ichloropropane
Vinyl Chloride
SEMI-VOLATILE ORGANICS (ug/L)
Acenaphthalene
Acenaphthene
Acetophenone
2 -Acety laminof luorene
4-Aminobiphenyl
Aniline
Anthracene
Aramite
Benzo ( a ) anthracene
Benzenethiol
Benzidine
Benzo(a)pyrene
Benzo (b) fluoranthene
UNTREATED
K103
ND
10000
500
40000
500
500
500
500
500
500
500
500
500
500
1000
1500000
1500000
3000000
3000000
3000000
1500000
1500000
NA
1500000
ND
7500000
1500000
1500000
UNTREATED
K104
ND
10000
500
40000
500
500
500
500
500
500
500
500
500
500
1000
150000
150000
300000
300000
300000
150000
150000
NA
150000
ND
750000
150000
150000
TREATED
K103 & K104
ND
100
5
400
5
5
5
5
5
5
5
5
5
5
10
30
30
60
60
60
30
30
NA
30
ND
150
30
30
(Continued)
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 2
•O
•a
a>
3
a
o
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
93
94
95
96
BOAT
CONSTITUENT
UNTREATED
K103
UNTREATED
K104
TREATED
K103 & K104
SEMI-VOLATILE ORGANICS (ug/L) (Continued)
Benzo(g,h,i) perylene
Benzo(k) fluoranthene
p-Benzoquinone
Bis(2-Chloroethoxy) methane
Bis(2-Chloroethyl) Ether
Bis(2-chloroisopropyl) ether
Bis(2-ethylhexyl) phthalate
4-Bromophenyl phenyl ether
Butyl benzyl phthalate
2-Sec-Butyl-4 , 6-Dinitrophenol
p-Chloroaniline
Chlorobenzilate
p-Chloro-m-cresol
2 -Chloronaphthalene
2 -Chlorophenol
3-Chloropropionitrile
Chrysene
Ortho-cresol
para-cresol
Dibenz ( a , h) anthracene
Dibenzo(a,e, ) Pyrene
Dibenzo(a,i) Pyrene
1, 3-Dichlorobenzene
1 , 2-Dichlorobenzene
1 , 4-Dichlorobenzene
3,3' Dichlorobenz idine
2 , 4-Dichlorophenol
2 , 6-Dichlorophenol
Diethyl phthalate
3,3' -Dimethoxybenz idine
p-Dimethylaminoazobenzene
3,3' -Dimethylbenz idine
2 , 4-Dimethylphenol
1500000
1500000
ND
1500000
1500000
1500000
1500000
1500000
1500000
7500000
1500000
NA
1500000
1500000
1500000
NA
1500000
1500000
1500000
1500000
NA
NA
1500000
1500000
1500000
3000000
1500000
ND
1500000
1500000
3000000
ND
1500000
150000
150000
ND
150000
150000
150000
150000
150000
150000
750000
150000
NA
150000
150000
150000
NA
150000
150000
150000
150000
NA
NA
150000
150000
150000
300000
150000
ND
150000
150000
300000
ND
150000
30
30
ND
30
30
30
30
30
30
150
30
NA
30
30
30
NA
30
30
30
30
NA
NA
30
30
30
60
30
ND
30
30
60
ND
30
(Continued)
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 2
•O
"g
3
O
,
97
98
99
100
101
102
103
104
105
106
107
108
109
110
ill
112
113
H4
115
116
117
118
119
120
121
122
123
124
125
126
127
128
BOAT UNTREATED
CONSTITUENT K103
UNTREATED
K104
TREATED
K103 & K104
SEMI -VOLATILE ORGANICS (ug/L) (Continued)
Dimethyl Phthalate
Di-n-butyl phthalate
1 , 4-Dinitrobenzene
4 , 6-dinitro-o-cresol
2 , 4-Dinitrophenol
2 , 4-Dinitrotoluene
2 , 6-Dinitrotoluene
Di-n-octyl phthalate
Di-n-propylnitrosoamine
Diphenylamine (1)
1,2, -Diphenylhydrazine
Fluoranthene
Fluorene
Hexachlorobenzene
Hexachlorobutadiene
Hexachlorocyclopentadiene
Hexachloroethane
Hexachlorophene
Hexachloropropene
Indeno(l,2,3,-cd) Pyrene
Isosafrole
Methapyrilene
3-Methylcholanthrene
4,4' -Methylene-bis- (2-chloroaniline)
Naphthalene
1 , 4-Naphthoquinone
1-Naphthylamine
2-Naphthylamine
p-Nitroanil ine
Nitrobenzene
4-Nitrophenol
N-Nitrosodi-n-butylamine
1500000
1500000
7500000
7500000
7500000
1500000
1500000
1500000
1500000
3000000
7500000
1500000
1500000
1500000
1500000
1500000
1500000
NA
ND
1500000
3000000
NA
3000000
3000000
1500000
NA
7500000
7500000
7500000
1500000
7500000
ND
150000
150000
750000
750000
750000
150000
150000
150000
150000
300000
750000
150000
150000
150000
150000
150000
150000
NA
ND
150000
300000
NA
300000
300000
150000
NA
750000
750000
750000
150000
750000
ND
30
30
150
150
150
30
30
30
30
60
150
30
30
30
30
30
30
NA
ND
30
60
NA
60
60
30
NA
150
150
150
30
150
ND
(Continued)
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+•" +* -t-1 •+•*
n n p.
0 0 N C C 0
O O 0 JH 4U di
i— 1 rH XI CX Qj O
O U r-l >H rH O
(0 (0 O O O r-J
rH rH rH rH rH ^ T3
•P -P X3 J3 ^ 'H -H
rH OJQJOOO'OO
O EH EH -H -H -H 1 <;
•HOJinvoEHEHEH ^O
C W O "^ ^* ^* LO ^D ^^^ O
0 0
2 2 2 "
O O
o o
0 Q Q Q 0
02220
in in
o o
o o
o o
0 Q Q Q 0
02220
in in
0)
c c c -H
0) Q) Q) 6
rH C C C W
O (!) 0) 0) O
O O O O -P
O C C C -H
rH -rH -H -H C
(0 (0 (0 >i
^^ ^^ C*] ^^ ^
Nl 1 1 r^
1 1 I rC
rti k ^ ^ _j
\y •* ^ •* •(—)
0
1-1
o
o
o
o
LO
f*x
o
o
o
o
o
in
0)
c
^
•H
c
o
^J
"*"^
•H
ro
-a
Q)
c
•H
-P
c
o
U
HHHHHHHHHHHi-HrHrHHHHrHrHHHHrHHH
Appendix C - 11
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 2
x
o
I
M
N)
**
**
154
155
156
157
158
159
160
161
162
163
164
165
166
167
168
BOAT
CONSTITUENT
SEMI -VOLATILE ORGANICS (ug/L)
3-Nitroaniline
2-Nitrophenol
METALS (ug/L)
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Mercury
Nickel
Selenium
Silver
Thallium
Vanadium
Zinc
UNTREATED
K103
(Continued)
7500000
1500000
32.0
10.0
1.0
1.0
4.0
7.0
6.0
5.0
20.0
11.0
5.0
6.0
10.0
6.0
2.0
UNTREATED
K104
750000
150000
32.0
100.0
1.0
1.0
4.0
7.0
6.0
100.0
20.0
11.0
50.0
6.0
10.0
6.0
2.0
TREATED
K103 & K104
150
30
32.0
100.0
1.0
1.0
4.0
7.0
6.0
50.0
20.0
11.0
50.0
6.0
100.0
6.0
2.0
ND - Constituent was not Detected, however, a matrix detection limit has not
been determined.
NA - The standard is not available;compound was searched using an NBS library of
42,000 compounds.
* - This constituent was analyzed as a semivolatile by Method 8270. The Generic Quality
Assurance Project Plan for Land Disposal Restrictions Program("BOAT"),EPA/530-SW-87
-Oil,March 1987,lists this compound as a Volatile ,however,it may be analyzed as
either a volatile or semivolatile organic
** - This constituent is not on the list of constituents in the Generic
Quality Assurance Project Plan for Land Disposal Restrictions Program ("BOAT"),
EPA/530-SW-011,March 1987. It is a ground-water monitoring constituent as listed
in Appendix IX, Page 26639, of the Fedral Register,Vol. 51, No.142.
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 3
p-
X
o
I
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
BOAT
CONSTITUENT
VOLATILE ORGANICS (ug/L)
Acetonitrile
Acrolein
Acrylonitrile
Benzene
Bromodichlorome thane
Bromomethane
Carbon Tetrachloride
Carbon Disulfide
Chlorobenzene
2-Chloro-l , 3-Butadiene
Chi or odibromome thane
Chloroethane
2-Chloroethylvinylether
Chloroform
Chloromethane
3 -Chloropropene
1 , 2-Dibromo-3-Chloropropane
1 , 2-Dibromoethane
Dibromomethane
Trans-1, 4-Dichloro-2-Butene
Dichlorodif luorome thane
1 , l-Dichloroethane
1 , 2-Dichloroethane
1 , 1-Dichloroethene
Trans-1 , 2-Dichloroethene
1 , 2-Dichloropropane
Trans-1, 3-Dichloropropene
cis-1 , 3 , Dichloropropene
1,4-Dioxane
Ethyl Cyanide
Ethyl Methacrylate
lodomethane
Isobutyl Alcohol
Methyl ethyl ketone
Methyl Methacrylate
UNTREATED
K103
50000
50000
50000
2500
2500
5000
2500
2500
2500
50000
2500
5000
5000
2500
5000
50000
5000
2500
2500
50000
5000
2500
2500
2500
2500
2500
2500
2500
100000
50000
50000
25000
100000
50000
50000
UNTREATED
K104
20000
20000
20000
1000
1000
2000
1000
1000
1000
20000
1000
2000
2000
1000
2000
20000
2000
1000
1000
20000
2000
1000
1000
1000
1000
1000
1000
1000
40000
20000
20000
10000
40000
20000
20000
TREATED
K103 & K104
100
100
100
5
5
10
5
5
5
100
5
10
10
5
10
100
10
5
5
100
10
5
5
5
5
5
5
5
200
100
100
50
200
100
100
(Continued)
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 3
•o
•o
X
o
I
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
BOAT
CONSTITUENT
VOLATILE ORGANICS(ug/L) (Continued)
Methyl Methanesulfonate*
Methacrylonitrile
Methylene Chloride
Pyridine
1,1,1, 2 -Tetrachloroethane
1,1,2,2 -Tetrachloroethane
Tetrachloroethene
Toluene
Tribromomethane
1,1, 1-Tr ichloroethane
1,1, 2-Trichloroethane
Trichloroethene
Trichloromonof luoromethane
1,2, 3-Trichloropropane
Vinyl Chloride
SEMI -VOLATILE ORGANICS (ug/L)
Acenaphthalene
Acenaphthene
Acetophenone
2-Acetylaminof luorene
4-Aminobiphenyl
Aniline
Anthracene
Aramite
Benzo (a) anthracene
Benzenethiol
Benzidine
Benzo ( a ) pyrene
Benzo (b) fluoranthene
UNTREATED
K103
ND
50000
2500
200000
2500
2500
2500
2500
2500
2500
2500
2500
2500
2500
5000
3000000
3000000
6000000
6000000
6000000
3000000
3000000
NA
3000000
ND
15000000
3000000
3000000
UNTREATED
K104
ND
20000
1000
80000
1000
1000
1000
1000
1000
1000
1000
1000
1000
1000
2000
150000
150000
300000
300000
300000
150000
150000
NA
150000
ND
750000
150000
150000
TREATED
K103 & K104
ND
100
5
400
5
5
5
5
5
5
5
5
5
5
10
150
150
300
300
300
150
150
NA
150
ND
750
150
150
(Continued)
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 3
TJ
fl>
3
a
H-
x
0
I
H
U)
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
93
94
95
96
BOAT
CONSTITUENT
UNTREATED
K103
UNTREATED
K104
TREATED
K103 & K104
SEMI-VOLATILE ORGANICS (ug/L) (Continued)
Benzo(g,h,i) perylene
Benzo(k) fluoranthene
p-Benzoquinone
Bis(2-Chloroethoxy) methane
Bis(2-Chloroethyl) Ether
Bis(2-chloroisopropyl) ether
Bis(2-ethylhexyl) phthalate
4-Bromophenyl phenyl ether
Butyl benzyl phthalate
2-Sec-Butyl-4 , 6-Dinitrophenol
p-Chloroaniline
Chlorobenzilate
p-Chloro-m-cresol
2 -Chloronaphthalene
2-Chlorophenol
3 -Chloropropionitrile
Chrysene
Ortho-cresol
para-cresol
Dibenz (a,h) anthracene
Dibenzo(a,e, ) Pyrene
Dibenzo(a,i) Pyrene
1, 3-Dichlorobenzene
1 , 2-Dichlorobenzene
1 , 4-Dichlorobenzene
3,3' Dichlorobenzidine
2 , 4-Dichlorophenol
2 , 6-Dichlorophenol
Diethyl phthalate
3,3' -Dimethoxybenz idine
p-Dimethylaminoazobenzene
3,3' -Dimethylbenzidine
2 , 4-Dimethylphenol
3000000
3000000
ND
3000000
3000000
3000000
3000000
3000000
3000000
15000000
3000000
NA
3000000
3000000
3000000
NA
3000000
3000000
3000000
3000000
NA
NA
3000000
3000000
3000000
6000000
3000000
ND
3000000
3000000
6000000
ND
3000000
150000
150000
ND
150000
150000
150000
150000
150000
150000
750000
150000
NA
150000
150000
150000
NA
150000
150000
150000
150000
NA
NA
150000
150000
150000
300000
150000
ND
150000
150000
300000
ND
150000
150
150
ND
150
150
150
150
150
150
750
150
NA
150
150
150
NA
150
150
150
150
NA
ND
150
150
150
300
150
ND
150
150
300
ND
150
(Continued)
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 3
T)
T)
0»
3
x
o
I
97
98
99
100
101
102
103
104
105
106
107
108
109
110
111
112
113
114
115
116
117
118
119
120
121
122
123
124
125
126
127
128
BOAT
CONSTITUENT
SEMI-VOLATILE ORGANICS (ug/L)
Dimethyl Phthalate
Di-n-butyl phthalate
1 , 4-Dinitrobenzene
4 , 6-dinitro-o-cresol
2 , 4-Dinitrophenol
2 , 4-Dinitrotoluene
2 , 6-Dinitrotoluene
Di-n-octyl phthalate
Di-n-propylnitrosoamine
Diphenylamine (1)
1,2, -Diphenylhydrazine
Fluoranthene
Fluorene
Hexachlorobenzene
Hexachlorobutadiene
Hexachlorocyclopentadiene
Hexachloroethane
Hexachlorophene
Hexachloropropene
Indeno(l, 2 , 3 , -cd) Pyrene
Isosaf role
Methapyrilene
3 -Methy Icholanthrene
UNTREATED
K103
(Continued)
3000000
3000000
15000000
15000000
15000000
3000000
3000000
3000000
3000000
6000000
15000000
3000000
3000000
3000000
3000000
3000000
3000000
NA
ND
3000000
6000000
NA
6000000
4,4' -Methylene-bis- (2-chloroaniline) 6000000
Naphthalene
1 , 4-Naphthoquinone
1-Naphthylamine
2-Naphthylamine
p-Nitroaniline
Nitrobenzene
4-Nitrophenol
N-Nitrosodi-n-butylamine
3000000
NA
15000000
15000000
15000000
3000000
15000000
ND
UNTREATED
K104
150000
150000
750000
750000
750000
150000
150000
150000
150000
300000
750000
150000
150000
150000
150000
150000
150000
NA
ND
150000
300000
NA
300000
300000
150000
NA
750000
750000
750000
150000
750000
ND
TREATED
K103 & K104
150
150
750
760
760
150
150
150
150
300
750
150
150
150
150
150
150
NA
ND
150
300
NA
300
300
150
NA
750
750
760
150
760
ND
(Continued)
-------
Q
W
EH
W
EH
2
W ro
K
EH EH
W
2 CO
H
W
EH PJ
W rt!
D CO
EH
H fc
EH 0
CO
2 W
O EH
U CO
a £l
o
tn Q
U
CO EH
EH *C
H W
S K
H EH
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W
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(0 rH ^J *rH
rH >i 0) rH
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4-^ Q) .XH CX
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S-i J-i J_j ^
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1 1 1 1
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m in o
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rt\ /it (i\ rti
W W Ur1 QJ
CU £L| CU CU
OOOO O
O LO LO tO O LO rij
CO rH rH rH ^ rH ^
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o o o o 2 o 2
o in in in in
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o o o o 2 o 2
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r"1 r* r"1 1 Lj *^ rt\
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in
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c c c e
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N N N O
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XI X! XI rH
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3 £ 6 rH
(0 (0 (0 >>i
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Q Q Q O
1 1 1 r4
1 I 1 A
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vo vo in -p
r** r^ H c
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in in in
r^ t~- H
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in in n
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0 0
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rH rH C
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C C £
trt trt O|
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*******
*******
HHHH
Appendix C - 17
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 3
Append j
X
o
1
154
155
156
157
158
159
160
161
162
163
164
165
166
167
168
BOAT
CONSTITUENT
METALS (ug/L)
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Mercury
Nickel
Selenium
Silver
Thallium
Vanadium
Zinc
ND - Constituent was not
UNTREATED
K103
32.0
10.0
1.0
1.0
4.0
7.0
6.0
5.0
20.0
11.0
5.0
6.0
10.0
6.0
2.0
Detected, however, a
UNTREATED
K104
32.0
10.0
1.0
1.0
4.0
7.0
6.0
5.0
20.0
11.0
50.0
6.0
10.0
6.0
2.0
matrix detection
TREATED
K103 & K104
32.0
10.0
1.0
1.0
4.0
7.0
6.0
5.0
20.0
11.0
50.0
6.0
10.0
6.0
2.0
limit has
not
oo
been determined.
NA - 'The standard is not available,'compound was searched using an NBS library of
42,000 compounds.
* - This constituent was analyzed as a semivolatile by Method 8270. The Generic Quality
Assurance Project Plan for Land Disposal Restrictions Program("BOAT"),EPA/530-SW-87
-Oil,March 1987,lists this compound as a Volatile ,however,it may be analyzed as
either a volatile or semivolatile organic
** - This constituent is not on the list of constituents in the Generic
Quality Assurance Project Plan for Land Disposal Restrictions Program ("BOAT"),
EPA/53O-SW-011,March 1987. It is a ground-water monitoring constituent as listed
in Appendix IX, Page 26639, of the Fedral Register,Vol. 51, No.142.
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 4
3
a
H-
x
o
I
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
BOAT
CONSTITUENT
VOLATILE ORGANICS(ug/L)
Acetonitrile
Acrolein
Acrylonitrile
Benzene
Bromodichloromethane
Bromomethane
Carbon Tetrachloride
Carbon Disulfide
Chlorobenzene
2-Chloro-l, 3-Butadiene
Chlorodibromomethane
Chloroethane
2-Chloroethylvinylether
Chloroform
Chloromethane
3 -Chloropropene
1 , 2-Dibromo-3-Chloropropane
1 , 2-Dibromoethane
Dibromomethane
Trans-l,4-Dichloro-2-Butene
Dichlorodif luoromethane
1 , l-Dichloroethane
1 , 2-Dichloroethane
1 , 1-Dichloroethene
Trans-1 , 2-Dichloroethene
1 , 2-Dichloropropane
Trans-1 , 3-Dichloropropene
cis-1 , 3 , Dichloropropene
1, 4-Dioxane
Ethyl Cyanide
Ethyl Methacrylate
lodomethane
Isobutyl Alcohol
Methyl ethyl ketone
Methyl Methacrylate
UNTREATED
K103
50000
50000
50000
2500
2500
5000
2500
2500
2500
50000
2500
5000
5000
2500
5000
50000
5000
2500
2500
50000
5000
2500
2500
2500
2500
2500
2500
2500
100000
50000
50000
25000
100000
50000
50000
UNTREATED
K104
10000
10000
10000
500
500
1000
500
500
500
10000
500
1000
1000
500
1000
10000
1000
500
500
10000
1000
500
500
500
500
500
500
500
20000
10000
10000
5000
20000
10000
10000
TREATED
K103 & K104
100
100
100
5
5
10
5
5
5
100
5
10
10
5
10
100
10
5
5
100
10
5
5
5
5
5
5
5
200
100
100
50
200
100
100
(Continued)
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 4
T3
3
a
H-
X
o
1
to
o
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
BOAT
CONSTITUENT
VOLATILE ORGANICS(ug/L) (Continued)
Methyl Methanesulfonate*
Methacrylonitrile
Methylene Chloride
Pyridine
1,1,1,2 -Tetrachloroethane
1,1,2, 2 -Tetrachloroethane
Tetrachloroethene
Toluene
Tribroroome thane
1,1, 1-Trichloroethane
1,1, 2-Trichloroethane
Trichloroethene
Trichloromonof luoromethane
1,2, 3-Trichloropropane
Vinyl Chloride
SEMI-VOLATILE ORGANICS (ug/L)
Acenaphthylene
Acenaphthene
Acetophenone
2-Acetylaminofluorene
4-Aminobiphenyl
Aniline
Anthracene
Aramite
Benzo ( a ) anthracene
Benzenethiol
Benzidine
Benzo (a) Pyrene
Benzo (b) Fluoranthene
UNTREATED
K103
ND
50000
2500
200000
2500
2500
2500
2500
2500
2500
2500
2500
2500
2500
5000
3000000
3000000
6000000
6000000
6000000
3000000
3000000
NA
3000000
ND
15000000
3000000
3000000
UNTREATED
K104
ND
10000
500
40000
500
500
500
500
500
500
500
500
500
500
1000
300000
300000
600000
600000
600000
300000
300000
NA
300000
ND
1500000
300000
300000
TREATED
K103 & K104
ND
100
5
400
5
5
5
5
5
5
5
5
5
5
10
30
30
60
60
60
30
30
NA
30
ND
150
30
30
(Continued)
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 4
•o
a
H-
X
o
I
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
93
94
95
96
BOAT
CONSTITUENT
SEMI-VOLATILE ORGANICS (ug/L)
Benzo(g,h,i) perylene
Benzo(k) fluoranthene
p-Benzoquinone
Bis (2-Chloroethoxy) methane
Bis(2-Chloroethyl) Ether
Bis (2-chloroisopropyl) ether
Bis (2-ethylhexyl) phthalate
4-Bromophenyl phenyl ether
Butyl benzyl phthalate
2-Sec-Butyl-4 , 6-Dinitrophenol
p-Chloroaniline
Chlorobenzilate
p-Chloro-m-cresol
2-Chloronaphthalene
2-Chlorophenol
3-Chloropropionitrile
Chrysene
Ortho-cresol
para-cresol
Dibenz (a,h) anthracene
Dibenzo(a, e, ) Pyrene
Dibenzo(a,i) Pyrene
1 , 3-Dichlorobenzene
1 , 2-Dichlorobenzene
1 , 4-Dichlorobenzene
3,3' Dichlorobenzidine
2 , 4-Dichlorophenol
2 , 6-Dichlorophenol
Diethyl phthalate
3,3' -Dimethoxybenzidine
p-Dimethylaminoazobenzene
3,3' -Dimethylbenzidine
2 , 4-Dimethylphenol
UNTREATED
K103
(Continued)
3000000
3000000
ND
3000000
3000000
3000000
3000000
3000000
3000000
15000000
3000000
NA
3000000
3000000
3000000
NA
3000000
3000000
3000000
3000000
NA
NA
3000000
3000000
3000000
6000000
3000000
ND
3000000
3000000
6000000
ND
3000000
UNTREATED
K104
300000
300000
ND
300000
300000
300000
300000
300000
300000
1500000
300000
NA
300000
300000
300000
NA
300000
300000
300000
300000
NA
NA
300000
300000
300000
600000
300000
ND
300000
300000
600000
ND
300000
TREATED
K103 & K104
30
30
ND
30
30
30
30
30
30
150
30
NA
30
30
30
NA
30
30
30
30
NA
NA
30
30
30
60
30
ND
30
30
60
ND
30
(Continued)
-------
Q
Pa
pa
fn
2
pa ^
K
EH EH
pa
2 CO
pa
CO hi
EH ft
pa «i
ED co
EH
H fa
EH O
2 pa
O EH
U CO
& 5
O
E*H Q
pa
CO EH
EH <
H pa
s &
H EH
Q
2 2
O <
H
EH
u
pa
EH
Q
U
X
H
Q
2
pa
ft
/••i
t-M
O
Q H
EH
< c*
pa
a r>
EH 0
H
Q
pa
EH
pa o
a H
HI^J*
HH
^
Q
pa
EH
pa o
OS H
r . \*/
C™1 HM
2
EH
2
1
H
EH
EH CO
ri| 2
PQ U
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13
0)
C
•H
jj
C
O
CJ
•~-
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1^
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^
p
co
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o
pa
H
EH
3
o
1
H
riE*
CO
T3
Q>
C
OOOOOOOOOOOOOOOOO OO OOO OOOOO -H
ro^iOiOLnfOfO^rovoiOfororocofOfOri^QfOvOriJvDvoro^iriioiOroLOi^-p
HHH H 22 2 2HHHH2C
O
U
OOOOOOOOOOOOOOOOO OO OOO OOOOO
OOOOOOOOOOOOOOOOO OO OOO OOOOO
ooooooooooooooooo.m ininmnin
HHH H HHHH
^^
0)
c
•H
rH
•H
C
(0
o
^-1
o
0) H
c o) x: a)
at o) c u c
CO) -H 0) 1 -H
•H c TJ M H-H C -P
(0(ca)^oo)0)(OOHT3 c-naa) c-o xi^s o d
r-H f! N U C 3 3 X« VH ^^^ ^i Q) 'O O C 0) 0) O -P 1 C 0) 0) Q
(C4-)CIO)HH4->-P £! N (0 rH (T3 C a 1 CO) -HCCO) 1
x3x3Q)ox;oox3-Ha)rH C-POXJQJO - QJIOC 3 -H --H c H c
J.J o. o | Q. i i i i p r^ r* ^. nj 0) P »^i -P .^i M fO C *"H 0) O^ € G "fH 0) O 1
x3 ooooo H-HCC j2x>uo)aa~ o)OrHa)o-lJ-lV-l^-lH>-(6,3CCCCCU^ >I-H C CHHHHH^H — M >i>i (0 a-P-P O 0) O O
f< Q ,,—j .,_f ,,—j >f_j
-------
Q
W
EH
W
EH
ED
W TJ-
SC
EH EH
W
55 w
tJ
EH
W
I
H
g
CO
oooooo
oooooo
oo
ooo
a)
3
c
•H
-P
o
U
OOOOOO OOOOOO O OO OOO O O
oooooo oooooo o oo ooo o o
QOOOOOOQi invo roino in
fO H H H H
o
in
H
oooooo oooooo o oo ooo o o
oooooo oooooo o oo ooo o o
oooooo oooooo o oo ooo o o
QOOOOOOQrt3OOOOOOQOii 0)
0)
C 0)
0)
c
0)
N
c
0)
C M
0) O
N C
C 0)
0)
-P
(0
o
(X
xi a o) o o a
o o N c c o
ccc
a)Q)a)
H-H g O-H >,4J 0 0 0 0 C
T5T36eaaiMM>H>-ico)
00000000000 -H ^
WWWWMWIrHrHrHM^JX!
OOOOX!43iJX!(l)-P
o>
CO)
-HT3
0
C
-HXlJinvD
4J4J£ J3J3-H-H 0 0 OrH
.0)(C
H H H H
HHHHHHHHHHrHHHHHH
Appendix C - 23
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 4
n
<0
a
H-
X
o
NJ
**
**
154
155
156
157
158
159
160
161
162
163
164
165
166
167
168
BOAT
CONSTITUENT
SEMI -VOLATILE ORGANICS (ug/L)
3-Nitroaniline
2-Nitrophenol
METALS (ug/L)
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Mercury
Nickel
Selenium
Silver
Thallium
Vanadium
Zinc
UNTREATED
K103
(Continued)
15000000
3000000
32.0
10.0
1.0
1.0
4.0
7.0
6.0
5.0
20.0
11.0
5.0
6.0
10.0
6.0
2.0
UNTREATED
K104
1500000
300000
32.0
10.0
1.0
1.0
4.0
7.0
6.0
5.0
20.0
11.0
50.0
6.0
10.0
6.0
2.0
TREATED
K103 & K104
150
30
32.0
500.0
1.0
1.0
4.0
7.0
6.0
5.0
20.0
11.0
50.0
6.0
10.0
6.0
2.0
ND - Constituent was not Detected, however, a matrix detection limit has not
been determined.
NA - The standard is not available;compound was searched using an NBS library of
42,000 compounds.
* - This constituent was analyzed as a semivolatile by Method 8270. The Generic Quality
Assurance Project Plan for Land Disposal Restrictions Program("BOAT"),EPA/53O-SW-87
-Oil,March 1987,lists this compound as a Volatile ,however,it may be analyzed as
either a volatile or semivolatile organic
** - This constituent is not on the list of constituents in the Generic
Quality Assurance Project Plan for Land Disposal Restrictions Program ("BOAT"),
EPA/530-SW-011,March 1987. It is a ground-water monitoring constituent as listed
in Appendix IX, Page 26639, of the Fedral Register,Vol. 51, No.142.
-------
Q
W
EH
W
EH
2
W
5C
EH
H
W
EH
2
W
EH
M
EH
5*
O
U
o
w
EH
H
S
H
i_3
2
O
H
EH
U
W
EH
W
Q
U
X
H
Q
2
W
cx
&
Q
EH
< O
W O
« H
C. to*
r1 *-H
2
D
EH
p^
JD
EH
H
EH
EH W
Q 0
CQ U
oooininoininmoinoo
o o o H o H H
H H H H
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in in in in
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fl "H 'O fl rH
X! H fl X! ^
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0) H *O ^ O -H
6 X! -H pa 6 >
<1) O O «H Q) 1 O H
fl) rH HQ)flHCnGr^ C 1 EHQ<1)O-H4->O
•H 'H C fl) "H Q) ,n M ^ (1) M
ctuocTieccooooo
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4J 1 -H O O O 1
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g - 0 XI X! X! -
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Q EH Q H ,—j ,_) c^
in in in
000
in in in
O) CM (M
O O O
O O O
in in in
fl)
C
fl) fl)
Q. C
O fl)
fl) CX O
C O H
fC ^ O|
a o o
O *™H M
H X! 0
0-H Xi
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rH fl Q
£*••»•
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1 C 1
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0
0
CM
0
0
o
0
H
O
O
0
0
H
fl)
C
(0
X
.,-1
Q
'
v
,—j
000
o o in
H H
o o o
o o o
o o in
in in CN
o o o
o o o
o o o
in in (N
fl)
-P
fl
rH
fl)r7
T3 0
C X! C
(0 4^ (0
>i Q) X!
fl)
rH H £
>i>i 0
f^ r* fQ
1 i 1) Q
W W H
O 0
0 0
CM H
0 0
0 0
o in
H
0 0
o o
o o
o in
H
Q)
c
o
rH 4J
O fl)
o
rH ^i
< XI
4.)
rH 0)
^1
-P rH
3 s^
X! Xi
U fl)
H S
T5
fl)
c
O -H
0 4J
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0
U
o
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in
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fl
rH
>1
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XI
.p
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s
,_!
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x:
fl)
s
Appendix C - 25
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 5
(0
3
X
o
I
to
CT*
36
37
38
39
40
41
42
43
44
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
BOAT
CONSTITUENT
VOLATILE ORGANICS(ug/L) (Continued)
Methyl Methanesulfonate*
Methacrylonitrile
Methylene Chloride
Pyridine
1,1,1, 2-Tetrachloroethane
1,1,2,2 -Tetrachloroethane
Tetrachloroethene
Toluene
Tribromomethane
1,1, l-Trichloroethane
1,1, 2-Trichloroethane
Trichloroethene
Trichloromonof luoromethane
1,2, 3-Trichloropropane
Vinyl Chloride
SEMI-VOLATILE ORGANICS (ug/L)
Acenaphthalene
Acenaphthene
Acetophenone
2-Acetylaminofluorene
4 -Aminobipheny 1
Aniline
Anthracene
Aramite
Benz o ( a ) anthracene
Benzenethiol
Benzidine
Benzo(a) pyrene
Benzo(b) fluoranthene
UNTREATED
K103
ND
50000
2500
200000
2500
2500
2500
2500
2500
2500
2500
2500
2500
2500
5000
3000000
3000000
6000000
6000000
6000000
3000000
3000000
NA
3000000
ND
15000000
3000000
3000000
UNTREATED
K104
ND
5000
250
20000
250
250
250
250
250
250
250
250
250
250
500
300000
300000
600000
600000
600000
300000
300000
NA
300000
ND
1500000
300000
300000
TREATED
K103 & K104
ND
100
5
400
5
5
5
5
5
5
5
5
5
5
10
30
30
60
60
60
30
30
NA
30
ND
150
30
30
(Continued)
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 5
T)
(D
X
o
I
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
82
83
84
85
86
87
88
89
90
91
92
93
94
95
96
BOAT
CONSTITUENT
SEMI-VOLATILE ORGANICS (ug/L)
Benzo(g,h,i) perylene
Benzo(k) fluoranthene
p-Benzoquinone
Bis(2-Chloroethoxy) methane
Bis(2-Chloroethyl) Ether
Bis(2-chloroisopropyl) ether
Bis(2-ethylhexyl) phthalate
4-Bromophenyl phenyl ether
Butyl benzyl phthalate
2-Sec-Butyl-4 , 6-Dinitrophenol
p-Chloroaniline
Chlorobenzilate
p-Chloro-m-cresol
2-Chloronaphthalene
2-Chlorophenol
3-Chloropropionitrile
Chrysene
Ortho-cresol
para-cresol
Dibenz (a , h) anthracene
Dibenzo(a,e, ) Pyrene
Dibenzo(a,i) Pyrene
1, 3-Dichlorobenzene
1 , 2-Dichlorobenzene
1 , 4-Dichlorobenzene
3,3' Dichlorobenz idine
2 , 4-Dichlorophenol
2 , 6-Dichlorophenol
Diethyl phthalate
3,3' -Dimethoxybenz idine
p-Dimethylaminoazobenzene
3,3' -Dimethylbenz idine
2 , 4-Dimethylphenol
UNTREATED
K103
(Continued)
3000000
3000000
ND
3000000
3000000
3000000
3000000
3000000
3000000
15000000
3000000
NA
3000000
3000000
3000000
NA
3000000
3000000
3000000
3000000
NA
NA
3000000
3000000
3000000
6000000
3000000
ND
3000000
3000000
6000000
ND
3000000
UNTREATED
K104
300000
300000
ND
300000
300000
300000
300000
300000
300000
1500000
300000
NA
300000
300000
300000
NA
300000
300000
300000
300000
NA
NA
300000
300000
300000
600000
300000
ND
300000
300000
600000
ND
300000
TREATED
K103 & K104
30
30
ND
30
30
30
30
30
30
150
30
NA
30
30
30
NA
30
30
30
30
NA
NA
30
30
30
60
30
ND
30
30
60
ND
30
(Continued)
-------
Q
W
EH
W
tf
EH
2
w m
EH EH
W
2 W
H
03 (J
EH OH
2 Sj
W 5
D W
EH
H PK
EH O
03
2 M
O EH
U 03
£3
c
-H
-p
c
o
u
•—'
^^
(-5
*s^
O1
3
s-'
u
H
5z
^
o
ptj
o
H
EH
3
0
1
H
S3
u
03
0)
4->
0) (0
•P rH
(0 (0
«5
43
CM rH
>1
rH 4J
>1 3
•P 1
0) C
g 1
•H -H
Q O
OOOOOOOOOOOOOOOOO OO
HHH H 22
OOO
OOOOO
0)
3
C
•H
H 2 C
O
U
OOOOOOOOOOOOOOO OO
OOOOOOOOOOOOOOO OO
OOOOOOOOOOOOOOOrtJQOO
00000000000000022
OOOOOOOOOOOOOOO
droir>ininmnr>r>voionr>r>cor>o
HHH H
OOO OOOOO
OOO OOOOO
vo
0)
C
•H
0) g
-P (0
0)
•H
N
0)
G
0) 0)
0)
0)
•rl
(0
4J
C
0)
0)T3OC
0)
0)
M
fr
C T(
0) 0) O
OOO
OOO
OOO
OOO
OOO
000
VO VO M
0)
c
•H
c
o
I
OrHQ)O(0(OrHCC-H
rH4J-H-H-H-H-H4J OH cu-p Q) o o o o o OH o ^rHjJrHxjxJx: us c aw
>,3CCCCCOM >1-H C CHrHrHrHHrH^^ >,>,Q) (0 CX -P -P O 0) O O
fa-oaaai i oil ^Muuooooc(0(0-Pi-P2aa-po-P-P
D^'tfvoi iar733XXXXXXT3O-PS3'*a^<222-P22
^^v^.H-HvH ^rHrHfl)Q)(l)0)a)Q)CinQ)l * <0 - I I I -HI I
CTlOlCTvOOOOOOOOOOHHHHH
HHHHHHHHHHHHHHH
H H H H H H H
HHHHH
Appendix C - 28
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 5
BOAT
CONSTITUENT
UNTREATED
K103
UNTREATED
K104
TREATED
K103 & K104
SEMI -VOLATILE ORGANICS (ug/L) (Continued)
>
13
'O
(D
**
a
H-
X
1
CO
vD
129
130
131
132
133
134
135
136
137
138
139
140
141
142
143
144
145
146
147
148
149
150
151
152
153
**
**
**
**
**
**
**
N-Nitrosodiethylamine
N-Nitrosodimethylamine
N-Nitrosomethylethylamine
N-Nit r osomorphol ine
1-Nitrosopiperidine
N-Nitrosopyrrolidine
5-Nitro-o-toluidine
Pentachlorobenzene
Pentachloroethane
Pentachloronitrobenzene
Pentachlorophenol
Phenacetin
Phenanthrene
Phenol
2-Picoline
Pronamide
Pyrene
Resorcinol
Safrole
1,2,4, 5-Tetrachlorobenzene
2,3,4, 6-Tetrachlorophenol
1,2, 4-Trichlorobenzene
2,4, 5-Trichlorophenol
2,4, 6-Trichlorophenol
Tris (2, 3-dibromopropyl) phosphate
Benzoic Acid
Benzyl Alcohol
1 , 2-Diaminobenzene
1 , 3-Diaminobenzene
1 , 4-Diaminobenzene
Diphenylnitrosoamine
2-Nitroaniline
ND
3000000
3000000
6000000
3000000
15000000
3000000
ND
NA
30000000
15000000
6000000
3000000
3000000
3000000
ND
3000000
NA
15000000
6000000
ND
3000000
15000000
3000000
ND
15000000
3000000
ND
ND
ND
15000000
15000000
ND
300000
300000
600000
300000
1500000
300000
ND
NA
3000000
1500000
600000
300000
300000
300000
ND
300000
NA
1500000
600000
ND
300000
1500000
300000
ND
1500000
300000
ND
ND
ND
1500000
1500000
ND
30
30
60
30
150
60
ND
NA
300
150
60
30
30
30
ND
30
NA
150
60
ND
30
150
30
ND
150
30
ND
ND
ND
150
150
(Continued)
-------
APPENDIX C
DETECTION LIMITS FOR CONSTITUENTS IN THE UNTREATED
AND TREATED WASTE OF SAMPLE SET 5
(D
a
M-
X
o
I
U)
o
**
**
154
155
156
157
158
159
160
161
162
163
164
165
166
167
168
BOAT
CONSTITUENT
SEMI-VOLATILE ORGANICS (ug/L)
3-Nitroaniline
2 -Nitrophenol
METALS (ug/L)
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Copper
Lead
Mercury
Nickel
Selenium
Silver
Thallium
Vanadium
Zinc
UNTREATED
K103
(Continued)
15000000
3000000
32.0
500.0
1.0
1.0
4.0
7.0
6.0
5.0
20.0
11.0
5.0
6.0
10.0
6.0
2.0
UNTREATED
K104
1500000
300000
32.0
500.0
1.0
1.0
4.0
7.0
6.0
50.0
20.0
11.0
50.0
6.0
10.0
6.0
2.0
TREATED
K103 & K104
150
30
32.0
10.0
1.0
1.0
4.0
7.0
6.0
100.0
20.0
11.0
50.0
6.0
10.0
6.0
2.0
ND
NA
** —
been determined.
The standard is not available;compound was searched using an NBS library of
42,000 compounds.
This constituent was analyzed as a semivolatile by Method 8270. The Generic Quality
Assurance Project Plan for Land Disposal Restrictions Program("BOAT"),EPA/530-SW-87
-Oil,March 1987,lists this compound as a Volatile ,however,it may be analyzed as
either a volatile or semivolatile organic
This constituent is not on the list of constituents in the Generic
Quality Assurance Project Plan for Land Disposal Restrictions Program ("BOAT"),
EPA/530-SW-011,March 1987. It is a ground-water monitoring constituent as listed
in Appendix IX, Page 26639, of the Fedral Register,Vol. 51, No.142.
-------
APPENDIX 0 Calculation of Treatment Standards
Constituent: Benzene
Effluent 1 Accuracy 3 Corrected 4
Sample Set Concentration Percent 2 Correction Concentration Log 5
(ing/ 1) Recovery Factor (ing/ 1) Transform
1 0.042 76 1.32 0.055
2 0.005 76 1.32 0.007
4 0.019 76 1.32 0.025
5 0.011 76 1.32 0.015
x = 0.026 y =
s =
-2.900
-4.962
-3.689
-4.200
-3.938
0.867
1 - Obtained from the Onsite Engineering Report, E. I . du Pont de Nemours, Table 6-14.
2 - Obtained from the Onsite Engineering Report, E. I . du Pont de Nemours, Table 7-12.
3 - Accuracy Correction Factor = 100 / Percent Recovery.
4 - Corrected Concentration = Effluent Concentration X Accuracy Correction Factor.
5 - Log Transform using the natural logarithm. In, of the Corrected Concentration.
Treatment Standard = Corrected Effluent Mean X VF
Calculation of Variability Factor (VF):
c = exp
where
y = the mean of the log transforms
s = the standard deviation of the log transforms.
Therefore, C = exp (-3.938 + 2.33(0.867))
= exp (-1.918)
= 0.147
and VF = C / x
99
where
x = the mean of the corrected effluent concentrations.
Therefore, VF = C / x
= 0?147 / 0.026
= 5.654
Treatment Standard = Corrected Effluent Mean X VF
= 0.026 X 5.654
= 0.147 mg/l
Appendix D - 1
-------
APPENDIX D Calculation of Treatment Standards
Constituent: Aniline
Sample Set
Effluent 1
Concentration
(ing/ 1)
I
Percent 2
Recovery
Accuracy 3
Correction
Factor
Corrected 4
Concentration
(mg/l)
Log 5
Transform
0.030
0.030
0.030
0.960
91
91
91
91
1.10
1.10
1.10
1.10
0.033
0.033
0.033
1.056
-3.411
-3.411
-3.411
0.054
x =
0.289 y =
s =
-2.545
1.733
1 - Obtained from the Onsite Engineering Report, E. J . du Pont de Nemours, Table 6-14.
2 - Obtained from the Onsite Engineering Report, E. I. du Pont de Nemours, Table 7-13.
3 - Accuracy Correction Factor = 100 / Percent Recovery.
4 - Corrected Concentration = Effluent Concentration X Accuracy Correction Factor.
5 - Log Transform using the natural logarithm, In, of the Corrected Concentration.
Treatment Standard = Corrected Effluent Mean X VF
Calculation of Variability Factor (VF):
C = exp (y * 2-33s)
where
y = the mean of the log transforms
s = the standard deviation of the log transforms.
Therefore, C = exp (-2.545 + 2.33(1.733))
= exp (1.493)
= 4.450
and VF = C / x
where
x = the mean of the corrected effluent concentrations.
Therefore, VF = C / x
= 4?450 / 0.289
= 15.398
Treatment Standard = Corrected Effluent Mean X VF
= 0.289 X 15.398
= 4.450 mg/t
Appendix D - 2
-------
APPENDIX P Calculation of Treatment Standards
Constituent: 2,4-Dinitrophenol
Effluent
Sample Set Concentration
(mg/l)
1 0.380
2 0.320
4 0.260
5 0.230
I
Percent 2*
Recovery
80
80
80
80
Accuracy 3
Correction
Factor
1.25
1.25
1.25
1.25
X
Corrected 4
Concentration
(mg/l)
0.475
0.400
0.325
0.288
0.372 y
s
Log 5
Transform
-0.744
-0.916
-1.124
-1.245
= -1.007
= 0.222
1 - Obtained from the Onsite Engineering Report, E. I. du Pont de Nemours, Table 6-14.
2 - Obtained from the Onsite Engineering Report, E. I. du Pont de Nemours, Table 7-13.
* - Average of Percent Recovery for Semivolatiles with greater than or equal to
20% recovery as listed in Table 7-13.
3 - Accuracy Correction Factor = 100 / Percent Recovery.
4 - Corrected Concentration = Effluent Concentration X Accuracy Correction Factor.
5 - Log Transform using the natural logarithm, In, of the Corrected Concentration.
Treatment Standard = Corrected Effluent Mean X VF
Calculation of Variability Factor (VF):
C = exp (y + 2.33s)
where
y = the mean of the log transforms
s = the standard deviation of the log transforms.
Therefore, C = exp (-1.007 + 2.33(0.222))
= exp (-0.490)
= 0.613
and VF = C / x
where
x = the mean of the corrected effluent concentrations.
Therefore, VF = C / x
= 0.613 / 0.372
= 1.648
Treatment Standard = Corrected Effluent Mean X VF
= 0.372 X 1.648
= 0.613 mg/l
Appendix D - 3
-------
APPENDIX D Calculation of Treatment Standards
Constituent: Nitrobenzene
Effluent 1 Accuracy 3 Corrected 4
Sample Set Concentration Percent 2 Correction Concentration Log 5
(mg/l) Recovery Factor (ing/ 1) Transform
1 0.03 115 0.87 0.026
2 0.03 115 0.87 0.026
4 0.03 115 0.87 0.026
5 0.03 115 0.87 0.026
x = 0.026 y =
s =
-3.650
-3.650
-3.650
-3.650
-3.650
0.000
1 - Obtained from the Onsite Engineering Report, E. I. du Pont de Nemours, Table 6-H.
2 - Obtained from the Onsite Engineering Report, E. I. du Pont de Nemours, Table 7-13.
3 - Accuracy Correction Factor = 100 / Percent Recovery.
4 - Corrected Concentration = Effluent Concentration X Accuracy Correction Factor.
5 - Log Transform using the natural logarithm. In, of the Corrected Concentration.
Treatment Standard = Corrected Effluent Mean X VF
Calculation of Variability Factor (VF):
C = exp (y + 2.33s)
where
y = the mean of the log transforms
s = the standard deviation of the log transforms.
Therefore,
99
= exp (-3.650 + 2.33(0))
= exp (-3.650)
= 0.026
and VF = C / x
where
x = the mean of the corrected effluent concentrations.
Therefore, VF = C / x
= 0?026 / 0.026
= 1
A variability factor of one was not used in calculating the treatment standards.
The variability factor of 2.80 was substituted for the value 1.
VF = 2.80
Treatment Standard
Corrected Effluent Mean X VF
= 0.026 X 2.80
= 0.073 mg/t
Appendix D - 4
-------
APPENDIX 0
Calculation of Treatment Standards
Constituent: Phenol
Sample Set
Effluent 1
Concentration
(mg/l)
Percent 2
Recovery
Accuracy 3
Correction
Factor
Corrected 4
Concentration
(mg/D
Log 5
Transform
0.030
0.030
0.030
0.150
21
21
21
21
4.76
4.76
4.76
4.76
0.143
0.143
0.143
0.714
-1.945
-1.945
-1.945
-0.337
0.286 y =
s =
-1.543
0.804
1 - Obtained from the Onsite Engineering Report, E. I. du Pont de Nemours, Table 6-14.
2 - Obtained from the Onsite Engineering Report, E. I. du Pont de Nemours, Table 7-13.
3 - Accuracy Correction Factor = 100 / Percent Recovery.
4 - Corrected Concentration = Effluent Concentration X Accuracy Correction Factor.
5 - Log Transform using the natural logarithm. In, of the Corrected Concentration.
Treatment Standard = Corrected Effluent Mean X VF
Calculation of Variability Factor (VF):
C = exp (y + 2.33s)
where
y = the mean of the log transforms
s = the standard deviation of the log transforms.
Therefore, C = exp (-1.543 + 2.33(0.804))
= exp (0.330)
= 1.391
and VF = C / x
where
x = the mean of the corrected effluent concentrations.
Therefore, VF = C / x
= 1?391 / 0.286
= 4.864
Treatment Standard = Corrected Effluent Mean X VF
= 0.286 X 4.864
= 1.391 mg/l
Appendix D - 5
-------
APPENDIX D Calculation of Treatment Standards
Constituent: Total Cyanides
Sample Set
Effluent
Concentration
(mg/l)
1
Percent 2
Recovery
Accuracy 3
Correction
Factor
Corrected 4
Concentration
(mg/l)
Log 5
Transform
0.565
0.597
0.156
0.129
72
72
72
72
1.39
1.39
1.39
1.39
0.785
0.830
0.217
0.179
-0.242
-0.186
-1.528
-1.720
0.503 y =
s =
-0.919
0.818
1 - Obtained from the Onsite Engineering Report, E. I. du Pont de Nemours, Table 6-K.
2 - Obtained from the Onsite Engineering Report, E. I. du Pont de Nemours, Table 7-14.
3 - Accuracy Correction Factor = 100 / Percent Recovery.
4 - Corrected Concentration = Effluent Concentration X Accuracy Correction Factor.
5 - Log Transform using the natural logarithm, In, of the Corrected Concentration.
Treatment Standard = Corrected Effluent Mean X VF
Calculation of Variability Factor (VF):
C = exp (y + 2.33s)
where
y = the mean of the log transforms
s = the standard deviation of the log transforms.
Therefore, C = exp (-0.919 + 2.33(0.818))
= exp (0.987)
= 2.683
and VF = C / x
where
x = the mean of the corrected effluent concentrations.
Therefore,
VF - C / x
= 2.683 / 0.503
= 5.334
Treatment Standard = Corrected Effluent Mean X VF
= 0.503 X 5.334
= 2.683 mg/l
Appendix D - 6
-------
APPENDIX E - ANALYTICAL QA/QC
The analytical methods used for analysis of the regulated
constituents identified in Section 5 are listed in Table E-l.
SW-846 methods (EPA's Test Methods for Evaluating Solid Waste;
Physical/Chemical Methods. SW-846. Third Edition, November 1986)
are used in most cases for determining total waste
concentrations.
Deviations from SW-846 methods required to analyze the
sample matrix are listed in Table E-2. These deviations are
approved methods for determining constituent concentrations.
SW-846 also allows for the use of alternative or equivalent
procedures or equipment; these are described in Tables E-3
through E-5. These alternatives or equivalents included use of
alternative sample preparation methods and/or use of different
extraction techniques to reduce sample matrix interferences.
The accuracy determination for a constituent is based on the
matrix spike recovery values. Table E-6 present the matrix spike
recovery values for total waste concentrations of benzene,
aniline, nitrobenzene, and phenol for K103/K104 and for total
cyanides for K104 for the EPA-collected data. Because
2,4-dinitrophenol matrix spike recoveries were not collected, the
average of the percent recoveries equal' to or greater than 20%
for all semivolatiles was used as the percent recovery for
2,4-dinitrophenol.
Appendix E-l
-------
The accuracy correction factors for the regulated
constituents for the treatment residuals are presented in Table
E-6. The accuracy correction factors were determined in
accordance with the general methodology presented in the
Introduction. For example, for benzene, actual spike recovery
data were obtained for analysis of liquid matrices and the lowest
percent recovery value was used to calculate the accuracy
correction factor. An example of the calculation of the
corrected concentration value for benzene is shown below.
Analytical Correction Corrected
Value % Recovery Factor Value
0.042 mg/1 76 100 =1.32 1.32 x 0.042 = 0.055 mg/1
76
Appendix E - 2
-------
Table E-1 Analytical Methods for Regulated Constituents
Regulated Constituent
Analytical Method
Method Number
Volatiles
Benzene
Purge and Trap 5030
Gas Chromatography/Mass 8240
Spectrometry for Volatile
Organics
Semivolatiles
Aniline
2,4-Dinitrophenol
Nitrobenzene
Phenol
Continuous Liquid/Liquid 3520
Extraction
Gas Chromatography/Mass 8270
Spectrometry Column
Technique
Inorganics
Cyanides
Total and Amenable Cyanides 9012
a - Environmental Protection Agency. 1986. Test Methods for
Evaluating Solid Waste. Third Edition. U. S. EPA. Office of
Solid Waste and Emergency Response. November 1986.
Appendix E - 3
-------
Table E-2 Deviations from SW-846
a
Ana l>s is
Method
SW 846 specificat ion
Deviation from SW B46
Rationale for deviation
1 Con! muous tiquid/
L iquul f xt ract ion
•d
(D
3
H-
X
M
I
^
35?0 A The internal standards are prepared
by dissolving them in carbon
bisulfide and then diluting to
volume so that the final solvent is
20V, carlinn disulfide and 80/
methytene chlor ide
B The extracts are concentrated to a
final volume of 1-2 ml
C The samples are extracted initially
(base/neutral) extracted at pH >11
and the secondary (acid) extraction
is at pH <2
The preparation of the internal
standards was changed to eliminate the
use of carbon disulfide The internal
standards were prepared in methylene
chloride only
Due to the high organic content in
many samples, the extracts could not
be reduced to the 1-2 ml final
volume The increased sample volume
in the extract was taken into account
when the dilutions were made and when
the concentrations values were
calculated. Final sample volume
varied depending upon the sample
However, for most samples the final
volume was 6-7 ml For sample point
1. the final volume was 7S-100 ml.
For samples from SD3. SD4, and S010,
the acid extraction was completed
first, followed by the base/neutral
extraction.
Final volume of sample extracts
was increased to keep all organic
material in solution. When the
final volume was decreased, the
samples crystallized
The acid extraction was completed
first due to the acidity of the
samples. The pHs for these
samples were between 0 and 2.
Therefore, to prevent potential
sample contamination and to
prevent adding large volumes of
acid and base solution to change
the pH to basic and then back to
acidic, the acid extraction was
completed first. The pH of
samples from Sample Point 11
could not be raised to pH 11
(200 ml of NaOH were added to the
-------
Table E-2 (Continued)
Ana lysis
Method
SW-846 specification
Oeviat ion from SW-846
Rationale for deviation
'O
(D
3
a
H-
x
w
I
01
1 Continuous Liquid/
L iquid Extract ion
(Continued)
0 The samples are extracted for
base/neutral and for acid
extractables
For SO 10. the one sample taken was
extracted for the acid extraction only
1'iter sample and the pH did not
change from the initial pH of
zero.)
The sample contained about 60X
nitrobenzene, therefore, to
obtain information on the
presence of the acid extractable
compounds, the analysis was
completed only on the acid
extractables. The high quantity
of nitrobenzene in the
base/neutral fraction would have
required extremely high dilution
of the material to prevent column
saturation and to bring the
concentration level into the ppb
linear range of the Method.
Therefore, only the level of
nitrobenzene could have been
quantified.
a - Onsite Engineering Report of Treatment Technology Performance for E. I. duPont
de Nemours, Inc., Beaumont, Texas. Table 7-4.
-------
Table E-3 Specific Procedures or Equipment Used in Extraction of Organic Compounds When
Alternatives or Equivalents are Allowed in the SW-846 Methods
Ana l
SW-846 Method
Sample Aliquot
Alternatives or Equivalents Allowed
by SW-846 Methods
Specific Procedures or
Equipment Used
Purge and Trap
5030
5 mi 1li liters of liquid
V
ID
3
H-
X
w
I
o\
Continuous Liquid-
Liquid Extraction
3520
1 liter of liquid
The purge and trap device to be
used is specified in the method in
Figure 1, the desorber to be used
is described in Figures 2 and 3.
and the packing materials are
described in Section 4.10.2 The
method allows equivalents of this
equipment or materials to be used.
The method specifies that the
trap must be at least 25 cm long
and have an inside diameter of at
least 0.105 in.
The surrogates recommended are
toIuene-d8,4-bromofluorobenzene.
and l,2-dichloroethane-d4. The
recommended concentration level is
50 ug/1.
Acid and base/neutral extracts
are usually combined before
analysis by GC/MS. However,
under some situations, they may
be extracted and analyzed
separately.
The purge and trap equipment and
the desorber used were as specified
in SW-846. The purge and trap
equipment is a Teckmar ISC-2 with
standard purging chambers (Supelco
cat. 2-0293). The packing materials
for the traps were 1/3 silica gel
and 2/3 2,6-diphenylene.
The length of the trap was 30 cm
and the diameter was 0.105 cm.
The surrogates were added as
specified in SW-846.
Acid and base/neutral extracts
were combined.
The base/neutral surrogates
recommended are 2-fluorobiphenyl,
nitrobenzene-dS, terphenyl-d!4.
The acid surrogates recommended
are 2-fluorophenol,
2,4,6-tribromophenol, and
phenol-d6. Additional compounds
Surrogates were the same as those
recommended by SW-846. The volume
of the surrogates added was
increased due to the sample matrix.
All samples except, the one sample
from Sample Point 10 had 3 ml of the
surrogates containing 100 ppm of the
-------
Table E-3 (Continued)
I
-o
Ana lysis
SW-846 Method
Sample Al iquot
Alternatives or Equivalents Allowed
by SW-846 Methods
Specific Procedures or
Equipment Used
Continuous L iqu id-
Liquid Extract ion
(Continued)
may be used for surrogates The
recommended concentrations for
low-medium concentration level
samples are 100 ppm for acid
surrogates and 200 ppm for
base/neutral surrogates. Volume
of surrogate may be adjusted
base neutral surrogate and 200 ppm
of the acid surrogates added To
the one sample from Sample Point
10, 10 ml of the surrogates were
added.
tJ
V
ro
a
H-
X
a - Onsite Engineering Report of Treatment Technology Performance for E. I. duPont
de Nemours, Inc., Beaumont, Texas. Table 7-5.
-------
Table E-4 Special Procedures or Equipment Used for Analysis of Organic Compounds When
Alternatives or Equivalents are Allowed in the SW-846 Methods
Analys is
SW-846
Method
Sample
Preparation
Method
Alternatives or Equivalents
Allowed in SW-846 for
fquipment or in Procedure
Specific Equipment or Procedures Used
Recommended GC/MS operating conditions
Actual GC/MS operating conditions.
Gas Chro'tiatography/
Mass Spectromet ry
for volatile
01 cjan ics
8240
5030
3
I-1-
X
I
co
E lectron enerqy
Mass range
Scan time
Initial column temperature
Initial column holding time
Column temperature piogram
Final column temperature
Final column holding time'
Injector temperature-
Source temperature
Transfer line temperature'
Carrier gas
70 vols (nominal)
35-260 amu
To give 5 scans/peak but
not to exceed 7 sec/scan
45'C
3 mm
8'C/m\n
200"C
15 mm
200-225'C
According to manufacturer's
specification
250-300'C
Hydrogen at 50 cm/sec or
hellum at 30 cm/sec
• The column should be 6-ft x 0.1 in 1.0. glass,
packed with I'/ SP-1000 on Carbopaclj B (60/80 mesh) or
an equivalent
• Samples may be analyzed by purge and trap technique
or by direct injection
I lectron energy:
Mass range-
Scan time.
Initial column temperature:
Initial column holding time:
Column temperature program:
Final column temperature:
Final column holding time:
Injector temperature:
Source temperature:
Transfer line temperature:
Carrier gas:
70 ev
35 - 260 amu
2.5 sec/scan
38'C
2 mm
10'C/min
225'C
30 mm or xylene elutes
225'C
lOO'C
275'C
Helium * 30 ml/mm.
•Additional Information on Actual System Used
Equipment: Finnegan model 5100 6C/MS/OS system
Data system: SUPER1NCOS Autoquan
Mode: Electron impact
N6S library available
Interface to MS - Jet separator
• The column used was an 8-ft. x 0 1 in. 1.0. glass.
packed with IX SP-1000 on Carbopack B (60/80 mesh).
• All samples were analyzed using the purge and trap
technique.
-------
Table E-4 (Continued)
Analys is
SW-846
Method
Sample
Preparation
Method
Alternatives or Equivalents
Allowed in SW-846 for
Equipment or in Procedure
Specific Equipment or Procedures Used
Recommended GC/MS operating conditions
Gas Chromatogrttph)/
Mass Speci ro'iet ry
for semivolat i le
organ ics capi1 lai v
column technique
«270 3520-Liquids
tJ
•a
(D
3
a
Mass range
Scan time
Initial column temperature
Initial column holding time
Column temperature program-
Final column temperature hold
Injector temperature
Transfer line temperature-
Source temperature.
In lector
Sample volume
Carrier gas.
3b-500 amu
1 sec/scan
40'C
4 mm
40-270'C at
ICTC/min
270"C (unt)l
benzo[g,h.i,]perylene has
eluted)
250-300'C
250-300"C
According to
manufacturer's
specification
Grob-type, split less
1-2 uL
Hydrogen at 50 cm/sec or
helturn at 30 cm/sec
The column should be 30 m by 0 25 mm I.D.. 1-um film
thickness silicon-coated fused silica capillary column
(J6W Scientific DB-5 or equivalent).
Actual GC/MS operating conditions
Mass range:
Scan time:
Initial column temperature:
Initial column holding time:
Column temperature program:
Final column temperature hold
Injector temperature:
Transfer line temperature
Source temperature:
Injector:
Sample volume
Carrier gas.
35 - 500 amu
1 sec/scan
30'C
4 mm
8'C/min to 275'
and 10'C/min until
305'C
305'C
240-260'C
300'C
Non-heated
Grob-type. spitless
1 uL of sample extract
Helium 9 40 cm/sec.
•Additional Information on Actual System Used
Equipment: Finnegan model 5100 GC/MS/DS system
Software Package: SUPER I NCOS AUTOQUAH
The column used was a 30 m x 0 32 mm I D.
RTx -5 (5% phenyl methyl silicone) FSCC
a - Onsite Engineering Report of Treatment Technology Performance for E. I. doPont
de Nemours, Inc., Beaumont, Texas. Table 7-6.
-------
Table E-5 Specific Procedures or Equipment Used for Analysis of
Cyanides When Alternatives or Equivalents are Allowed
in the SW-846 Methods
Analysis
Total and
amenable
cyanide
SU-846 Sample
Method Aliquot
9012 500 ml
Alternatives or Equivalent
Allowed by SW-846 Methods
Hydrogen sulfide treatment
may be required.
Specific
Procedures Used
Hydrogen sulfide
treatment was not
requ i red .
A Fisher-Mulligan absorber
or equivalent should be used.
A Wheaton Distilling
Apparatus absorber was
used.
a - Onsite Engineering Report of Treatment Technology Performance for E. I. duPont
de Nemours, Inc., Beaumont, Texas. Table 7-8.
Appendix E - 10
-------
Table E-6 Matrix Spike Recoveries for Treated Waste
TJ
a
\->-
X
BOAT Constituent
Volatile
4 . Benzene
Semivolati le
56. Aniline
+ +
Original Amount Sample Set Sample Set Duplicate
Found Spike Added Spike Result Percent Spike Added Spike Result Percent Accuracy
(ug/L) (ug/L) (ug/L) Recovery* (ug/L) (ug/L) Recovery* Factor**
18 50 56 76 50 65 94 1.32
NO 200 194 97 200 182 91 1.10
101. 2,4-Dinitrophenol***
126. Nitrobenzene
142. Phenol
Inorganics
++
169. Total Cyanides
129
200
200
100
232
63
201
85
116
21
72
200
200
229
51
80
115
26
1.25
0.87
4.76
1.39
a = From Onsite Engineering Report of Treatment Technology Performance for E. I. du Pont de Nemours, Inc., Beaumont, Texas. Tables 7-12 through 7-14.
'Percent Recovery = [(Spike Result - Original Amount)/Spike Amount)] x 100.
"Accuracy Correction Factor = 100/(Percent Recovery), using the lower of the two percent recovery values.
ND = Not detected. Value assumed to be zero in calculation for percent recovery.
*** = The matrix spike recovery values presented for 2,4-Dinitrophenol are actually the average of the percent recoveries greater than 20% for all semivolatiles.
+ « For the matrix spike recoveries presented: Volatiles from Sample Set 3(even though this sample set was deleted from the final development of treatment standards,
the matrix spike recoveries were not affected.), Semivolatiles from Sample Set 1, and Inorganics from Sample Set 4.
= Total cyanides are regulated for K104 only.
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The comparative method of measuring thermal
conductivity has been proposed as an ASTM test method under
the name "Guarded, Comparative, Longitudinal Heat Flow
Technique". A thermal heat flow circuit is used which is
the analog of an electrical circuit with resistances in
series. A reference material is chosen to have a thermal
conductivity close to that estimated for the sample.
Reference standards (also known as heat meters) having the
same cross-sectional dimensions as the sample are placed
above and below the sample. An upper heater, a lower
heater, and a heat sink are added to the "stack" to complete
the heat flow circuit. See Figure 1.
Appendix F - 1
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GUARD
GRADIENT
STACK
GRADIENT"
THERMOCOUPLE
UPPER
HEATER
STACK
CLAMP
BOTTOM
REEER-ENCE
SAMPLE
LOWER; STACK
HEATER
LIQUID
HEAT
:OOLED
SINK
HEAT ELOW
DIRECTION
^ — -
UPPER
GUARD
HEATER
X
K
/v
/
K
LOWER
GUARD
HEATER
FIGURE 1 SCHEMATIC DIAGRAM OF THE COMPARATIVE METHOD
Appendix F - 2
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The temperature gradients (analogous to potential
differences) along the stack are measured with type K
(chromel/alumel) thermocouples placed at known separations.
The thermocouples are placed into holes or grooves in the
references and also in the sample whenever the sample is
thick enough to accommodate them.
For molten samples, pastes, greases, and other
materials that must be contained, the material is placed
into a cell consisting of a top and bottom of Pyrex 7740 and
a containment ring of marinite. The sample is 2 inch in
diameter and .5 inch thick. Thermocouples are not placed
into the sample but rather the temperatures measured in the
Pyrex are extrapolated to give the temperature at the top
and bottom surfaces of the sample material. The Pyrex disks
also serve as the thermal conductivity reference material.
The stack is clamped with a reproducible load to
insure intimate contact between the components. In order to
produce a linear flow of heat down the stack and reduce the
amount of heat that flows radially, a guard tube is placed
around the stack and the intervening space is filled with
insulating grains or powder. The temperature gradient in
the guard is matched to that in the stack to further reduce
radial heat flow.
The comparative method is a steady state method of
V-
measuring thermal conductivity. When equilibrium is reached
the heat flux (analogous to current flow) down the stack can
be determined from the references. The heat into the sample
is given by
Appendix F - 3 January 1988
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>WdT/dx)top
and the heat out of the sample is given by
Qout ~ xbottom(dT/dx) bottom
where
X = thermal conductivity
dT/dx = temperature gradient
and top refers to the upper reference while bottom refers to
the lower reference. If the heat was confined to flow just
down the stack, then Q^n and Qout would be equal. If Q^n
and Qout are in reasonable agreement, the average heat flow
is calculated from
The sample thermal conductivity is then found from
Appendix F - 4
** January 1988
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^sample = Q/(dT/dx)sample
The result for the K102 Activated Charcoal Waste
tested here is given in Table 1. The sample was held at an
average temperature of 42C with a 53C temperature drop
across the sample for approximately 20 hours before the
temperature profile became steady and the conductivity
measured. At the conclusion of the test it appeared that
some "drying" of the sample had occurred.
Appendix F - 5
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