United States
Environmental Protection
Agency
Office of
Solid Waste
EPA/530-SW-85-003
April 1985
Solid Waste
Petitions to Deiist
Hazardous Wastes
A Guidance Manua!
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This report has been reviewed by the Office of Solid
Waste, U.S. Environmental Protection Agency, and approved
for publication. Mention of trade names or commercial
products does not constitute endorsement or recommendation
for use.
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PETITIONS TO DELIST HAZARDOUS WASTES;
A GUIDANCE MANUAL
April 1985
Prepared for:
Waste Identification Branch
Office of Solid Waste and Emergency Response
U.S. Environmental Protection Agency
by:
The Cadmus Group, Inc.
375 Concord Avenue
Belmont, MA 02178
Under subcontract to
Industrial Economics, Inc
Contract No. 68-01-6892
Work Assignment No. 3
U S Environmental Protection Agency
Region 5, Library (PL-12J)
77 West Jackson Boulevard, 12th hoof
Chicago, IL 60604-3590
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00
ACKNOWLEDGEMENTS
The authors are grateful to the following individuals and
organizations for their assistance in the writing of this
manual: Mr. William Sproat, Jr., of the U.S. EPA°s Office
of Solid Waste (OSW), who managed the Work Assignment and
who provided the necessary leadership, guidance and en-
couragement; Messrs. James Poppiti and Myles Morse, also
of OSW, who supplied us with information and advice at
critical points; and Ms. Nancy Hammett, of Industrial Eco-
nomics, Inc., who managed the contract under which this
Work Assignment was performed and who greatly eased the
administrative aspects of the task. In addition, the
following people and firms contributed draft materials
that formed the basis for some of the sections. Their
assistance is sincerely appreciated.
Ms. Janie Harris
JRB Associates
Mr. Calvin Spencer
Ms Karen Christensen
Radian Corporation
Mr. George Parris
Dynamac Corporation
Mr. Michael Pich
Industrial Economics, Inc.
Mr. Mark Wagner
Geraghty & Miller, Inc.
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TABLE OF CONTENTS
Page
1.0 INTRODUCTION 1
1.1 Purpose of This Manual 1
1.2 How Wastes are Listed as Hazardous 2
1.3 The Rationale for the Delisting Procedure 3
1.4 The Guidance Manual: Contents and 5
Organization
2.0 THE ELEMENTS OF THE DELISTING PROCESS 9
2.1 Submitting the Petition 9
2.2 Review of the Petition 11
2.3 Decision to Grant or Deny 11
3.0 ADMINISTRATIVE INFORMATION AND SUMMARY 13
4.0 PRODUCTION PROCESSES 15
4.1 General Process Information 15
4.2 Assessment of Hazardousness 16
4.3 Special Procedures for Certain Industries 18
5.0 THE WASTE STREAM 23
5.1 Description of the Waste Stream 23
5.2 Description of Waste Management Methods 24
6.0 SELECTING CONSTITUENTS FOR WHICH TO TEST 25
6.1 General Considerations 25
6.2 Engineering' Analysis to Determine What is 26
Likely to be Present in the Waste
6.3 Supporting Your Selection of Constituents 27
7.0 SAMPLING THE WASTE STREAM 29
7.1 Representative Sampling 30
7.2 Sampling Equipment 31
7.3 Sampling Techniques fpr Specific Forms 38
of Waste
7.4 Sample Handling, Storage, and Documentation 43
7.5 The Written Sampling Plan 46
8.0 SELECTION OF WASTE ANALYSIS METHODS 47
8.1 Tests for Characteristics 47
8.2 Tests for Constituents 49
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9.0 PRESENTATION OF ANALYTICAL DATA 51
9.1 General Information 51
9.2 Sampling Information 51
9.3 Test Results . 52
9.4 Quality Assurance and Quality Control 53
APPENDIXES
A. Optional Form for Delisting Petitions
B. Hazardous Waste Delisting Regulations (40 CFR 260 Subpart C)
C. State Hazardous Waste Agencies and Delisting Contacts
D. Hazardous Waste Characteristics (40 CFR 261 Subpart C)
5. Lists of Hazardous Wastes (40 CFR Subpart D)
F. Hazardous Constituents (40 CFR 261, Appendix VIII)
G. How to Use a Random Number Table
H. Typical Prices for Hazardous Waste Test Procedures
I. Examples of Delisting Petitions:
Inorganic Wastes
Organic wastes
J. Test Methods Not Available in SW-S46:
Extraction procedure for Oily Wastes
Total Organic Carbon
Total Oil and Grease
Determination of Reactive Cyanide and Sulfide
Determination of Photodegradable Cyanide
Explosive Hazard
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1.0 INTRODUCTION
1.1 Purpose of This Manual
Under Part 261 of the hazardous waste regulations, the Envi-
ronmental Protection Agency has listed approximately 90 industrial
waste streams as hazardous.* These wastes were listed because
they typically and frequently exhibit one or more of the charac-
teristics of hazardous wastes, or they typically and frequently
contain certain specific constituents that are known to be toxic
or otherwise hazardous at levels of regulatory concern. A waste
stream from any facility which qualifies as one of the streams
listed in Subpart' D of the regulations is regulated as hazardous;
the Agency does not need to show for any particular plant that the
hazardous constituents are actually present.
EPA has recognized, however, that a listed waste from a
particular facility may not actually be hazardous. This could be
the case if the waste (a) does not exhibit the characteristics or
contain the constituents for which it was originally listed, or
(b) because it contains these constituents at relatively low
concentrations, or (c) although the waste contains the listed
constituents, they are present in an immobile form.** These
situations could occur, for example, if a facility uses different
processes or raw materials than were assumed when the regulations
were written. The regulations (in Sections 260.20 and 260.22),
therefore, contain a procedure for anyone to petition the Agency
to exclude, or "delist," s-uch waste streams from regulation.
The purpose of this manual is, to assist persons who gene-
rate or manage listed wastes to submit delisting petitions. Due
to the need to ensure that hazardous wastes do not reach the
environment, the delisting procedure requires you to submit infor-
*The Agency also has listed approximately 360 commercial
chemical products as hazardous when they are discarded or intended
for discard.
**The delisting criteria were recently modified by the Hazar-
dous and Solid Waste Amendments of 1984 to require the Agency to
consider any factors (including additional constituents) other
than those for which the waste was listed, if there is a reason-
able basis to believe that such factors could cause the waste to
be hazardous.
^References to Section numbers in this manual are current as
of March of 1985 . Amendments to the delisting procedures after
this date may result in the renumbering of some Sections.
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mation on the processes and chemicals used., the results of tests
for hazardous constituents and hazardous waste characteristics,
the waste management practices currently in.effect, and other,
related topics. Due to the large amount of information required,
many petitions have contained errors and omissions. This manual
is intended to address this need, and thus to avoid the costs and
delays that have frequently resulted.
In the remainder of this Introduction, we address some topics
that will help petitioners understand the background of the list-
ing and delisting processes.
1.2 How Wastes are Listed as Hazardous
It is useful to understand how EPA. lists wastes as hazardous,
because that process forms the basis for the delisting procedure.
Subpart B of Part 261 of the hazardous waste regulations directs
EPA to list any waste as hazardous if it meets one or more of the
following criteria:
1. It exhibits any one of four hazardous waste
characteristics;
Ignitability
Corrosivity
Reactivity, or
Extraction procedure (EP) toxicity.
(The definitions of these terms are given in Chapter 8 of
this manual.)
2. It has been found to be fatal to humans in low doses; or,
in the absence of human toxicity data, it has any of the
following properties:
• an oral LD50 (rat) less than 50 mg/kg,
• an inhalation LC^Q (rat) less than 2 mg/1, or
• a dermal LDcQ (rabbit) less than 200 mg/kg;
or it has been found to otherwise cause or contribute to
serious irreversible or incapacitating illness. Such a
waste is called an acutely hazardous waste, and is sub-
ject to control at smaller quantities than other hazar-
dous wastes.
3. It contains one or more of approximately 350 hazardous
constituents listed in Appendix VIII of Part 261 unless,
after considering certain relevant factors, the Adminis-
trator concludes that the waste cannot pose a substantial
threat to human health or the environment when improperly
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managed or disposed of. Many of these constituents
have been shown to cause cancer, genetic mutation, or
embryonic damage in humans or other animals.
Using these three criteria, EPA produced three lists of haz-
ardous wastes, which are given in Subpart D of the regulations.
The first two lists are based primarily on the third criterion
(i.e., presence of hazardous constituents). The lists are:
1. Hazardous waste from non-specific sources. (Section
261.31) These consist mainly of spent solvents and elec-
troplating wastes.
2. Hazardous waste from 'specific sources. (Section 261.32)
These are mostly residues from manufacturing and waste-
water treatment processes.
The third list contains specific commercial chemical products and
is based on all three criteria: the four hazardous waste charac-
teristics, the definition of "acutely" hazardous, and the presence
of hazardous constituents. Specifically, it includes:
3. Discarded commercial chemical products, off-specifica-
tion species, containers, and spill residues thereof.
(Section 261.33) This list is divided into two parts:
acute hazardous wastes and other hazardous wastes.
1.3 The Rationale for the Delisting Procedure
As we mentioned above,- EPA included in its regulations (in
Sections 260.20 and 260.22) a procedure for delisting a waste from
an individual facility if it can be shown that the waste does not
meet any of the criteria for which the waste was listed. Until
recently, EPA required petitioners to demonstrate only that the
waste was not hazardous based on the criteria used by the Adminis-
trator in listing it. Since the petitioner was not? required to
test for other hazardous properties, wastes containing hazardous
constituents at significant levels,still could be delisted. Like-
wise, wastes that exhibited one or more of the hazardous waste
characteristics still could be delisted. In several cases, EPA
found that wastewater treatment sludges from electroplating opera-
tions, although non-hazardous by virtue of their low heavy metal
content, contained high concentrations of several toxic solvents.-
The delisting procedures (as revised by the recently enacted
Hazardous and Solid Waste Amendments of 1984, Section 222) require
you to provide a more comprehensive description of the waste so
that EPA can judge whether factors other than those for which the
waste was originally listed may cause the waste to be hazardous.
To characterize the waste adequately, four additional types of
information should be provided:
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1A. A complete listing of raw materials, intermediate pro-
ducts, by-products and final products, divided into three
separate lists:
• all those materials that are used or produced in the
processes at the plant or facility generating the
waste;
• of those materials identified above, those that are
discharged into or likely to be present in the waste,
as well as the approximate quantities used or pro-
duced; and
• of those materials identified above, those that you
do not believe are discharged into or likely to be
present in the waste, and the basis for this belief?
or
IB. Representative analytical data for all hazardous waste
constituents (as listed in Part 261, Appendix VIII) that
are likely to be present in the waste at significant
levels. For all other hazardous constituents in Appendix
VIII, provide your rationale for why they are not expect-
ed to be present at significant levels;
and all of the following:
2. Test results on representative samples showing whether
the waste exhibits any of the four hazardous waste char-
acteristics (as given in Subpart C of Part 261). Alter-
natively, if you can explain why the waste cannot exhibit
one or more of the four characteristics, you may submit
your rationale in- lieu of test results for those charac-
teristics .
3. Test results on representative samples for total organic
carbon (TOC).
4. Test results on representative samples for total oil and
grease.*
In addition, we shall collect ground-water monitoring data, if
available, from the states and regional offices for consideration
in our petition review process.
While this may seem like a lot of information for us to
request, it is justified by the seriousness of the harm that could
result if wastes that are still hazardous are delisted and escape
into the environment.
*Data on total oil and grease have been requested of peti-
tioners since before the passage of the RCRA amendments of 1984
We list these items here for completeness.
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1.4 The Guidance Manual; Contents and Organization
This manual is intended to be a complete guide on how to
satisfy the delisting petition requirements. It is intended to be
used by plant managers, operators, and engineers. In order to
keep it concise, we have not described the details of the various
waste testing procedures. Most of the necessary information may
be found in the following EPA publication:
"Test Methods for Evaluating Solid Waste: Physical/Chemical
Methods," U.S. EPA Office of Solid Waste and Emergency Re-
sponse, Publication SW-846 (second edition), July 1982.
This document and its supplements and revisions are available from
the Government Printing Office. (Its order number is 055-002-
81001-2.) You need to acquire it, however, only if you plan to do
the waste sampling and testing yourself.
Many of the required procedures — particularly those re-
lating to the sampling and analysis of wastes — are complex and
must be performed by qualified personnel. While some facilities
may have the required staff in house, others may need help from
consultants or commercial testing laboratories. If you decide to
get outside help, you should make sure that the consultant or
laboratory is familiar with the procedures in the publication
cited above.
The rest of this manual is divided into the following
sections:
2.0 The Elements of the Delisting Procedure
3.0 Administrative Information and Summary
4.0 Processes and Materials
5.0 The Waste Stream
6.0 Selecting Constituents for which to Test
7.0 Sampling the Waste Stream
8.0 Waste Analysis Methods
9.0 Presentation of Analytical Data
Appendices are also provided on the following subjects:
A. Optional Petition Form
B. Delisting Procedures (Section 260.22)
C. State Hazardous Waste Agencies
D. Hazardous Waste Characteristics (Sections 261.21,
261.22, 261.23, 261.24)
E. Listed Waste Streams (Sections 261.31, 261.32,
261.33)
F. Hazardous Constituents (Part 261, Appendix VIII)
G. Use of a Random Number Table
H. Price Ranges for Hazardous Waste Test Procedures
I. Examples of Petitions for Organic wastes and
Inorganic wastes
J. Test Methods Not Available in Other References
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The optional petition form in Appendix A is intended to assist you
in reporting the required information. You may substitute your
own reporting format as appropriate, provided that it is clear and
complete. In particular, facilities having special petitioning
requirements as described in Section 4.3 will need to adapt the
optional form to suit their needs.
A summary of the information required in most petitions is
given below.
Administrative Information:
Name, Address, Contact Person, Telephone Number,
RCRA ID number
Statement of Interest.
Description of Proposed Action
Certification Statement
Detailed Description of the Manufacturing Process
(Including Schematic Diagrams)
Waste Stream Information:
EPA Hazardous Waste Number
Description of the Waste
Estimate of Average and Maximum Monthly and Yearly
Quantities Generated
Waste Management Information: Current and Proposed
Sampling and Testing Information:
Name and Address of Laboratories Used
Names and Qualifications of Persons Performing the
Sampling and Analysis
Dates of Sampling and Analysis
Names and Model Numbers of the Testing Equipment Used
Detailed Description of Methods Used to Obtain
Representative Samples
Description of Sample Handling and Preparation
Description of Chain of Custody Procedures
A Statement and Evaluation of the Representativeness of
the Samples
Identification or Description of the Tests Performed
Quality Control and Quality Assurance Measures Taken
Data on Representative Samples for the Listed Constituents
and a Discussion of Why the Waste is Non-Hazardous
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Data to Determine Whether Other Hazardous Constituents May
Reasonably be Present:
Listing of All Raw Materials Used in the Process
Generating the Waste; of Those Materials, a Listing
of Those Expected to be Present in the Waste as
well as Approximate Quantities Used or Produced;
and of Those Materials Used in the Process, a
Listing of Those Not Expected in the Waste and the
Basis for this Judgment; or
Representative Test Data for All Hazardous Constituents
Expected in the Waste and an Explanation of Why
Those Not Tested For can be Excluded
Data on Representative Samples for Total Organic Carbon (TOC)
Data on Representative Samples for Oil and Grease
Data on Representative Samples for the Hazardous Waste
Characteristics
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2.0 THE ELEMENTS OF THE DELISTING PROCESS
This section summarizes the delisting process. There are
three major steps:
A. !fou submit the petition.
B. The Agency reviews the petition. If it is incom-
plete, we request the missing information. When all
of the information is complete, we review the peti-
tion and make a tentative decision whether to grant
or deny the request.
C. We then publish a proposed decision in the Federal
Register and request comments. If there are no
comments, and if no new significant information
comes to light, the Agency then publishes a final
decision. If new facts are brought forward, the
Agency re-evaluates its tentative (proposed) deci-
sion.
Below, we describe your responsibilities in each of these steps,
and what you should expect from us.
2.1 Submitting the Petition
Before you submit a petition, there are several preliminary
issues that you should consider.
Determining why your waste is hazardous. You should review
the reasons why your waste was determined to be hazardous. The
regulations issued on May 19, 1980 required all generators of
solid waste to determine whether their waste was hazardous (Sec-
tion 262.11). Hazardous wastes were defined as those that are
either: (a) listed in Subpart D of Part 261 or (b) exhibit one of
the four characteristics (ignitability, corrosivity, reactivity,
or EP toxicity) described in Subpart C of Part 261. If your waste
was listed, then it is possible that it can be delisted (assuming
the appropriate conditions are met). If it exhibits one of the
four characteristics, however, it cannot be delisted and there is
no point in submitting a delisting petition.
Determining whom to petition. Both the Federal government
and the individual State governments have jurisdiction over haz-
ardous wastes. In general, States whose hazardous waste programs
have been authorized by EPA to make delisting decisions can pro-
cess oetitions without EPA review. (Note that delisting by a
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State does not exempt the waste from the Federal hazardous waste
program or from regulation in other States.) Under the new RCRA
amendments, however, States will need to have their delisting
programs re-authorized to reflect the changes required by the
amendments in order to continue to delist wastes. These changes
include the consideration of "other factors" (including additional
constituents) in evaluating the hazardousness of the waste and the
requirement for notice and comment. Therefore, you should contact
either the Federal Regional Office or the State hazardous waste
agency to determine who administers the delisting program for your
State. A list of Regional delisting contacts and State hazardous
waste agencies is included in Appendix C.
Content of the petition. The elements of the petition are as
follows:
A. Administrative information and summary
B. Description of_the manufacturing processes, including
schematic diagrams
C. Description of the waste stream and management methods
D. The rationale for selecting the hazardous constituents
for testing
E. Development of the sampling plan
F. Selection of waste analysis methods
G. Presentation of analytical data
The following chapters describe in detail what you are to report
within each topic heading. In addition, two Appendixes are pro-
vided to assist you in writing your petition:
• Appendix A presents a form that you may use as a guide.
You may adapt it or use your own format if you wish,
provided that the submission is complete and clear.
• Appendix I gives examples, drawn from petitions received
by EPA in the past, that illustrate the content and
level of detail that we look for.
Petitions are to be submitted to:
The Administrator
U.S. Environmental Protection Agency
401 M Street, S.W.
Washington, D.C. 20460
A copy of the petition should also be submitted to:
Chief, Waste Identification Branch
Office of Solid Waste (WH-562B)
U.S. Environmental Protection Agency
401 M Street, S.W.
Washington, D.G. 20460
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2.2 Review of the Petition
The petition review process is represented schematically in
Exhibit 2.1. Petitions that are received are logged in and filed
with the Public Docket and with the Waste Identification Branch of
the Office of Solid Waste. A person from the delisting staff is
assigned to review the petition and to handle correspondence with
the petitioner. Notices of all petitions received are period-
ically published in the Federal Register.
We then conduct an initial review to determine:
• Whether the waste is eligible for exclusion, i.e., that it
is a currently listed waste and
• Whether the petition is complete and the analytical data
are representative of the waste stream.
If the information submitted is judged to be incomplete, addi-
tional data are requested. Once a petition is judged to be com-
plete, the reviewer makes a tentative decision to grant or deny
the petition. If the tentative decision is to deny it, then you
are notified of this by letter and you are offered the opportunity
to withdraw the petition. If you decline to withdraw it, a draft
Federal Register notice is prepared that proposes to deny the
petition. TT, however, the decision is to grant the petition, a
draft Federal Register notice is prepared announcing that deci-
sion. We also may recommend that the petition be granted on
condition that certain measures (for example, monitoring) be in-
stituted .
The draft notices are then sent to a workgroup consisting of
representatives from OSW and other Offices within EPA. The work-
group carefully evaluates the quality and representativeness of
the supporting data, and submits comments to OSW. When all of the
comments raised by the workgroup have been addressed, the notice
is sent to the Office of the General Counsel for its concurrence.
If that Office concurs, the final recommendation is sent to the
Assistant Administrator for Solid Waste and Emergency Response for
his final review and decision.
2.3 Decision to Grant or Deny
The Assistant Administrator decides whether to approve the
Office's recommendation. A notice of his proposed decision is
published in the Federal Register, along with a request for com-
ments on the action. When the comment period closes, the Office
reviews the information received in response to the Notice, and
the proposed decision is again reviewed by the workgroup and the
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EXHIBIT 2.1: PETITION REVIEW PROCESS
Log In
Reviewer Assigned
I
Reviewer Checks For
Complete Petition
• Representative Samples
• Complete Process Description
• Waste Quantity, Etc.
Reviewer Makes Preliminary
Assessment Of Whether
Petition Can Be Denied
Letter Sent
Informing Petitioner
Deny/Withdrawal Option
Additional Information
Required
Petitioner
Responds
i
Letter Sent
Requesting Additional
Information
Reviewer Recommends To
Grant Or Deny Petition
Reviewer Prepares
Proposal And All
Associated Documentation
Reviewer Prepares
Final Notice And
Associated Documentation
Takes Comments
and Evaluates
process described above is repeated. The Assistant Administrator
then makes a final decision, which is published in the Federal Re-
gister as a final rule.
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3.0 ADMINISTRATIVE INFORMATION AND SUMMARY
In this section, we describe the administrative information
that you are required to provide in your petition. We also
suggest you provide a summary of the technical information; this
will assist us in our review. The material in this section cor-
responds to Section A of the optional petition form in Appendix A.
The following information should be included at the beginning
of your petition. Items that are required by the regulations are
indicated by the appropriate Section number. The other items are
not required, but make it easier for us to review the petition.
o The name and address of the individual or firm submitting
the petition. (Section 260.20(b)(1))
o The name, address, and RCRA identification number of the
specific facility to which the petition applies. (Section
260.22(1)(4))
o The names, titles and telephone numbers of people to
contact for additional information.
o A brief description of the requested delisting action and
a summary of your justification for the action (Section
260.20(b) (2), (3), and (4)). (A detailed justification,
along with supporting data, should be furnished in later
parts of the petition.)
o The following statement signed by you, as generator of the
waste, or by your authorized representative (Section
260.22(i)(12)):
I certify under penalty of law that I have person-
ally examined and am familiar with the information
submitted in this demonstration and all attached
documents, and that, based on my inquiry of those
individuals immediately responsible for obtaining
the information, I believe that the submitted in-
formation is true, accurate, and complete. I am
aware that there are significant penalties for
submitting false information, including the possi-
bility of fine and imprisonment.
An "authorized representative" is a person responsible for
the overall operation of a facility or an operational unit
(for example, a plant manager, superintendent, or person
of equivalent responsibility). Consultants or other out-
side parties may not sign the certification statement.
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4.0 PRODUCTION PROCESSES
This section requests information on the manufacturing opera-
tions or other processes which generate the waste. We require you
to submit sufficient information for us to determine what hazar-
dous waste characteristics and toxic constituents may be present
in the waste. You must submit a description of the manufacturing
or other process that generates the waste. You may choose either
to furnish a list of raw materials or to test for Appendix VIII
constituents; these options are described in greater detail below.
Special data requirements for petroleum refineries and multiple
waste treatment facilities are also described.
This chapter corresponds to Section B of the optional peti-
tion form in Appendix A. (Facilities having special petition
requirements should adapt the optional petition form as appro-
priate. )
4.1 General Process Information
Please provide a description of the manufacturing processes
or other operations that produce the listed waste. Examples may
include, as appropriate, the following items:
• Descriptions of production lines and major items of
equipment. Also describe the stages of the typical oper-
ating cycle (e.g., startup, steady-state operation, clean-
ing and maintenance) on a daily, weekly, or other basis as
appropriate.
• A description of any surface and equipment preparation,
cleaning, degreasing, coating or painting processes used
in the facility that you have not included in the
description of the production lines.
• A schematic diagram of all manufacturing processes, sur-
face preparation, cleaning, and other operations that may
provide influent to the waste stream.
You do not need to provide an exhaustive description of the pro-
cess. Rather, you need only provide sufficient information to
allow us to understand your process, how and where the waste is
formed, and how the toxic constituents may end up in the waste.
The regulatory requirement for the information requested in
this section may be found in Section 260.22 ( i)(5).
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4.2 Assessment of Hazardousness
You may use either of the two approaches described below to
provide information on those constituents that may be present
in the waste.
Approach A;
Please provide the following information:
• Test results on representative samples for the following:
- The specific hazardous constituents for which the
waste was listed (i.e., total concentration of each
listed constituent found in Appendix VII of Part
261) ;
The four hazardous waste characteristics;*
- Appropriate leachate tests for the EP toxic metals,
nickel, and cyanide;
Total concentrations of the EP toxic metals and
nickel;
Total organic carbon (TOG); and
Total oil and grease.
• A list of all materials used in the manufacturing or
other operations that produce the waste. To the extent
possible, use the chemical name rather than the generic
name (e.g., "sodium hydroxide" instead of "caustic
cleaner"). Specify the approximate quantities used annu-
ally. Examples of materials to be included are:
Raw materials
Intermediate products
By-products
Products
Oils and hydraulic fluids
Surface preparation materials (solvents,
acids, cleaners, surface preparation
agents, paints, etc.)
*Note that you may provide an explanation of why the waste
does not exhibit a particular characteristic, in lieu of testing
for that characteristic.
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• An indication of which materials on the above list are
either discharged into the waste or are likely to be
present in the waste. For each material so indicated,
provide an estimate of the amount that enters the waste
stream annually. (Please specify kilograms, pounds, or
similar units.) For any of these materials that is speci-
fied only in terms of a generic or trade name, please
furnish a Materials Safety Data Sheet.
• From the above list of all materials that are used or
produced at the plant or facility, an indication of which
ones are not discharged into or likely to be present in
the waste. Also give the basis for this belief.
• Your assessment of the likelihood that these processes,
operations, or feed materials might produce a waste stream
that is not included in this petition. Include considera-
tions such as startup and shutdown operations, mainte-
nance, spills, leaks, and other accidents.
Approach B;
If you decline to furnish the information requested in Ap-
proach A above, then you should furnish the following information
instead:
• Test results on representative samples for the following:
The specific hazardous constituents for which the
waste was listed (i.e., total concentration of each
constituent found in Appendix VII of Part 261);
All other constituents listed in Appendix VIII of Part
261 that are likely to be present in the waste at
significant levels;
- The four hazardous waste characteristics;
Appropriate leachate tests for EP toxic metals,
nickel, and cyanide;
Total organic carbon; and
Total oil and grease.
• For those constituents listed in Appendix VIII of Part 261
that the petitioner does not expect to find (and thus does
not analyze for), an explanation of why this is reason-
able. Your explanation may be presented on a substance-
by-substance basis or for a group of substances. If the
Agency does not find your explanation satisfactory, we
shall either ask that you analyze for the additional
constituents or ask that a better explanation be provided.
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4.3 Special Procedures for Certain Industries
Certain industries generate wastes whose constituents vary
widely, and for which raw materials data cannot generally be
provided. Therefore, we require petitioners in these industries
to perform testing for certain constituents that we feel can
reasonably be expected to be present in the waste streams. Also,
we request additional information on manufacturing and waste
treatment processes beyond that which was requested in Section 4.1
above. The industries covered by these special procedures are
Petroleum Refining and Multiple Waste Treatment (i.e., commercial
offsite waste treatment facilities that accept waste from a vari-
ety of generators).
Petroleum Refining Wastes
In lieu of Approaches A or B above, please furnish the
following information:
• Test results on a representative number of samples for
each of the following:
The four hazardous waste characteristics. If your
waste contains greater than 1 percent oil and grease,
use both the extraction procedure from Section 261.24
and the extraction procedure for oily waste when test-
ing for EP toxicity. (The oily waste procedure is
required for all wastes that have an oil and grease
content greater than 1 percent.)
Total organic carbon (if total oil and grease is less
than 1,percent).
Total oil and grease.
Weigh»t of the solid residue remaining after Step 9 of
the EP toxicity test for oily waste.
Total concentrations of EP toxic metals in the waste.
Total concentration of each of the constituents shown
in Exhibit 4.1 (some of these will already have been
included in the tests for EP toxic metals).
• Your assessment of the likelihood that these processes,
operations, or feed materials might produce a waste stream
that is not included in this petition. Include considera-
tions such as startup and shutdown operations, mainte-
nance, spills, leaks, and other accidents.
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EXHIBIT 4.1: CONSTITUENTS OF PETROLEUM REFINING WASTES
1 . Metals
Antimony
Arsenic
Barium
Beryllium
Cadmium
Chromium
Cobalt
Lead
Mercury
Nickel
Selenium
Vanadium
2. Volatiles
Benzene
Carbon disulfide
Chlorobenzene
Chloroform
1,2-Dichloroethane
1,4-Dioxane
Ethyl benzene
Ethylene dibromide
Methyl ethyl ketone
Styrene
Toluene
Xylene
3. Semivolatile Base/Neutral
Extractable Compounds
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Bis(2-ethylhexyl) phthalate
Butyl benzyl phthalate
Chrysene
Dibenz(a,h)acridine
Dibenz(a,h)anthracene
Dichlorobenzenes
Diethyl phthalate
7 ,1 2-Diinethylbenz( a)anthracene
Dimethyl phthalate
Di(n)butyl phthalate
Di(n)octyl phthalate
Fluoranthene
Indene
Methyl chrysene
1-Methyl naphthalene
Naphthalene
Phenanthrene
Pyrene
Pyridine
Quinoline
4. Semivolatile Acid-Extractable
Compounds
Benzenethiol
Cresols
2,4-Dimethylphenol
2,4-Dinitrophenol
4-Nitrophenol
Phenol
Anthracene
Benzo(a)anthracene
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Wastes from Multiple Waste Treatment Facilities
Multiple Waste Treatment Facilities (MWTFs) typically receive
large numbers of individual waste shipments having a wide variety
of compositions. Therefore, MWTFs cannot describe adequately the
"raw materials" for the treatment process or use a mass balance to
demonstrate the presence or absence of a constituent in the treat-
ment residue. In addition, it is more difficult for them to
demonstrate that waste samples are representative.
Due to the differences between this hazardous waste category
and others, we have specified a more rigorous sampling and testing
strategy than is otherwise required. In addition, petitioners
must submit a plan for testing each batch of treated sludge before
it is disposed of, for as long as the facility is in operation.
This plan is referred to as the "contingency plan" and is de-
scribed in more detail below.
In lieu of Approaches A or B, please submit the following
information:
• A description of your procedure for prescreening clients
and wastes;
• Test results, on a representative number of samples (but
no fewer than eight) taken over a two-month period, for
each of the following:
The four hazardous waste characteristics. For the EP
toxicity test, use the extraction procedure for oily
wastes in addition to the extraction procedure in
Section 261.24 as appropriate.
Total concentrations of the EP toxic metals and nickel.
Appropriate leachate tests for the EP toxic metals,
nickel, and cyanide.
- Total organic carbon. *
Total oil and grease.
Long-term stability, using the Multiple Extraction
Procedure (see SW-846). This tes't is required only for
stabilized wastes, and only four samples are required
if these will be representative.
Cyanide: total, free, and leachable.
Appendix VIII constituents. Test for all constituents
that can reasonably be expected to be present in the
treatment residue. At a minimum, these should include
the 129 Priority Pollutants.
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• The percentage of the total number of waste types received
during the year that are represented by the wastes sampled
and tested for in this petition.
• For those Appendix VIII constituents for which you do not
analyze, your basis for not analyzing them (i.e., why it
is reasonable that these constituents are not expected to
be present in the treatment residue at significant levels)
• Your contingency plan for continuous testing of the
treated sludge. The following tests will be required for
each batch of treatment residue that is disposed of:
Appropriate leachate tests for the EP toxic metals,
Representative organic toxicants as determined from the
test results for Appendix VIII constituents, and
General screening tests such as TOX and TOC.
In addition, composite samples must be tested periodically
for the 129 Priority Pollutants. Monthly composites must
be tested for base-neutral compounds, and biweekly compo-
sites must be tested for volatiles. Contact the delisting
staff of the Waste Identification Branch for guidance in
developing this plan.
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5.0 THE WASTE STREAM
In this section, you are asked to describe the waste stream
that you request be delisted and to give its hazardous waste
number. The regulatory requirement for this information is found
in Section 260.22( i)(6). You also are asked for information on
how the waste is managed, and how it will be managed if your
petition is granted. The material in this section corresponds to
Section C of the optional petition form in Appendix A.
5.1 Description of the Waste Stream
The lists of regulated wastes are found in Sections 261.31,
261.32, and 261.33. From those lists, please furnish the follow-
ing information regarding the waste that is the subject of your
petition:
• Its EPA'hazardous waste number. If several wastes are
combined or mixed, please provide the hazardous waste
numbers for all listed wastes.
•
• Its common name (e.g., electroplating sludges, spent
xylene, dissolved air flotation (DAF) float from the pet-
roleum refining industry).
• Its physical form (i.e., aqueous stream, sludge, dry
solid; for sludges, please indicate the percentage of
solids).
From your operating records, please estimate the following amounts;
• Average amount generated monthly
• Maximum amount generated monthly
• Average amount generated annually
• Maximum amount generated annually
Please state clearly the units of measurement. Avoid using vague
units (such as "truckloads" or "barrels").
• Examples: kilograms, pounds, English tons, metric tons,
gallons
In addition, please specify which of these descriptions applies to
the waste stream:
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• It is presently being generated.
• It will be generated in the future.
• It has been generated in the past and is presently being
treated or stored on-site.
5.2 Description of Waste Management Methods
Briefly describe how you treat or dispose of the waste at
present. Include the following items:
• A paragraph describing the waste management techniques
currently used (e.g., landfill, lime treatment, etc.)
Please indicate whether the waste is managed on-site or
off-site.
• A schematic flow diagram (if appropriate) of the waste
treatment system, showing the processes, equipment, and
storage methods used.
• The names and locations of any commercial treatment, stor-
age, or disposal facilities that are used.
Describe, in a paragraph, the following as appropriate:
• How you treated or disposed of the waste before November
19, 1980 (when EPA's Hazardous Waste Management System
became effective), and
• How you will treat' or dispose of it if your delisting
petition is granted.
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6.0 SELECTING CONSTITUENTS FOR WHICH TO TEST
This chapter is intended to guide you in determining the
constituents for which you should test. The actual sampling and
testing procedures ar.e described in the following chapters. The
material in this chapter corresponds to Section D of the optional
petition form in Appendix A.
6.1 General Considerations
As we have already stated in previous chapters, the revised
delisting procedures suggest that you submit either;
1A. A complete listing of raw materials, intermediate pro-
ducts, by-products and final products, divided into three
separate lists:
• all those materials that are used or produced in the
processes at the plant or facility generating the
waste;
• of those materials identified above, those that are
discharged into or likely to be present in the waste,
as well as the approximate quantities used or pro-
duced; and
• of those materials identified above, those that you
do not believe are discharged into or likely to be
present in the waste, and the basis for this belief
(Approach A);
or
B. Representative analytical data for all constituents
listed in Appendix VIII of Part 261 that are likely to be
present in the waste at significant levels, as well as
your basis for not analyzing for the other Appendix VIII
toxic constituents (Approach B).
If you have elected to take Approach A, then you need to test
a representative number of samples of the waste for the following:
• The specific hazardous constituents for which the waste
was listed (i.e., total concentration of each listed con-
stituent found in Appendix VII of Part 261);
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• The four hazardous waste characteristics;
• Appropriate leachate tests for the EP toxic metals,
nickel, and cyanide;
• Total concentrations of the EP toxic metals and nickel;
,• Total organic carbon (TOG); and
• Total oil and grease.
After examining the data on raw materials, we may request further
analytical testing for those constituents that are likely to be
present in the waste at levels of regulatory concern. The rele-
vant test procedures are discussed in Chapter 8 of this manual.
If you have chosen this option, you may omit the rest of this
chapter.
If you have chosen Approach B, then you should perform all of
the tests specified above — i.e., listed Appendix VII constit-
uents, total oil and grease, TOG, and hazardous waste characteris-
tics — on representative samples of the waste. You must also
test representative samples for all Appendix VIII constituents
that may "reasonably be expected" to be present in the waste,
whether or not they were used as a basis for listing. In the
remainder of this chapter, we describe engineering analysis me-
thods that can assist you in determining which constituents are
likely to be in the waste.
Note that in selecting constituents for testing, you must
specifically consider each item on the list in Appendix VIII of
Part 261, and either test for its presence or state why it is not
likely to be present. This subject is discussed further in Sec-
t ion 6.3 be low.
6.2 Engineering Analysis to Determine What is Likely to be
Present in the Waste
The list of likely hazardous constituents usually can be
reduced to a reasonable number by specifying the chemicals going.
into a process, the products coming out, and an understanding of
the chemical and physical attributes of the process. This type of
approach involves:
• A mass balance to allow calculation of the total amount
of constituents in the wastes, and
• An examination of the chemical reactions occurring in the
process to identify' other likely constituents in the waste
stream.
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A mass balance for the process will show what raw materials are
used, their use rates, and whether they are likely to be present
in the waste at significant concentrations. For example, consider
a process involving the production of aniline by the reduction of
nitrobenzene. Based on plant data, for each 100 Ib of nitroben-
zene used, 72 Ib of aniline is formed, which indicates that 5 Ib
of nitrobenzene is lost in the process per 100 Ib used. Further-
more, it is known that 2000 gal of wastewater results from the
production of each 72 Ib of aniline. Therefore, one can estimate
that the maximum concentration of nitrobenzene in the wastewater
is about 300 ppm, assuming that all of the nitrobenzene is in the
wastewater. Based on this calculation, the generator would likely
test the wastewater treatment sludge for nitrobenzene.
The area of by-products is the most difficult to consider,
because expert chemical judgment (supported by appropriate exam-
ples from the literature) must be applied to predict the types and
relative amounts of by-products expected from a reaction. Unfor-
tunately, demonstrating that a chemical reaction does not actually
produce traces of hazardous substances also can be inconclusive.
For example, any reaction involving chlorinated phenols might
produce some chlorinated dibenzodioxins, which are considered to
be hazardous at trace levels, although it is not a very probable
reaction in most circumstances. In such cases, you should include
the substance as a constituent for testing.
The more detail that is provided by the engineering analysis,
the more likely our reviewers are to accept your judgment on which
constituents are likely to be present. For example, if a reactant
is described as "technical benzene," questions about the presence
of toluene and other aromatics (and their by-products) in the
waste stream may be raised. On the other hand, identification of
the reactant as "90% benzene, 9% toluene, 1% xylenes and less than
10 ppm sulfur" limits the likely composition of the waste stream.
You may not wish to disclose some items of process informa-
tion, even under the protection of the confidential business
information (CBI) restrictions. In such cases, a greater burden
is placed on the analytical chemist as discussed below. Every
attempt should be made to exclude possibilities from consideration
even when the process itself cannot be discussed. For example, if
none of the starting materials, solvents, or catalysts contain
halogens, the waste stream probably does not contain halogenated
constituents.
In some instances — for example, chemical mixtures used in
maintenance, cleanup, and other non-process applications — it may
not be possible to construct a mass balance. In such cases, you
should list the known constituents in each mixture and estimate
the amounts disposed of based on usage rates.
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6.3 Supporting Your Selection of Constituents
In your petition, you should describe how you selected the
constituents for which you will test. In addition, we shall
require you to give your basis for not analyzing any particular
constituent or group of constituents listed in Appendix VIII of
Part 261. You should state, for each hazardous waste constituent
(or group of constituents) for which you do not test, why you do
not believe it may "reasonably be expected to be present in the
waste." Substances on the list that may be found in your indus-
try°s wastes (although not in your particular facility°s wastes)
should be addressed individually. The remaining constituents may
be addressed as,a group by stating that your facility neither uses
nor produces any of the substances in question, nor any chemicals
that could form the substances in question.
The mass balance approach described above can be quite useful
for eliminating or identifying those constituents that are present
or absent from the waste. If you use this approach, however, you
should describe how it affected your choice of constituents.
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7.0 SAMPLING THE WASTE STREAM
Your delisting petition must be supported by analytical data
for samples of the waste in question. It is particularly im-
portant for you to demonstrate in the petition that the samples
are representative of the waste and that their integrity was
preserved until the required analyses were performed. Specific
reporting procedures are described in Chapter 9 of this manual.
The specific regulatory requirement for this information may be
found in Section 260.22(h).
Information to evaluate whether the collected samples are
representative of the waste is inadequate or totally lacking in
many delisting petitions. A simple statement that the samples are
representative is not sufficient for the Agency to conclude that
the waste has, in fact, been adequately characterized. In order
for us to make a finding of representativeness, you must provide a
detailed rationale as to why the samples that were collected do
represent the waste's composition as it varies in time and space.
This rationale should be based in part on considerations of how
the waste-generating process itself varies.
This chapter of the manual summarizes the elements that must
be considered in the development of a good sampling program. (A
detailed discussion of sampling methods may be found in EPA Publi-
cation SW-846.) In the first section (7.1), the concept of repre-
sentative sampling is discussed, especially with respect to het-
erogeneous wastes. Two basic strategies for obtaining represen-
tative samples of heterogeneous waste are described: time compo-
site sampling and two-dimensional random sampling. In Section
7.2, the most common sampling equipment is briefly described. In
Section 7.3, sampling techniques are described for process dis-
charges, drums, landfills, lagoons, and waste piles. In each
case, specific techniques are presented for obtaining representa-
tive samples, and suitable equipment from Section 7.2 is suggest-
ed. Section 7.4 discusses sample handling and storage, as well as
documentation of the sampling effort. Finally, Section 7.5 de-
scribes how your sampling effort should be documented in the
petition. The material in this manual corresponds to Section E of
the optional petition form in Appendix A.
Sampling is a complex procedure and the representativeness of
the sample is critical to the acceptability of your petition.
Therefore, we strongly recommend that you contact the delisting
staff of the Waste Identification Branch for guidance before you
actually draw the samples.
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7.1 Representative Sampling
The waste to be sampled may be homogeneous, or it may vary in
time or space. The selection of a sampling strategy depends on
what type of variability the waste exhibits.
Time Variability
Time variability is most often encountered when point dis-
charges are sampled, such as flow from pipes. Time composite
sampling usually is used in such cases. In this method, a number
of grab samples of equal volume are taken at regular time inter-
vals. These intervals must adequately characterize the variations
in process flow over time. The individual samples then are com-
bined into a series of composite samples, which are analyzed for
the various constituents.
You must collect and analyze enough composite samples to
characterize the variability of the waste stream over time. The
frequency of collection and the number of samples to be taken from
a production process depend on the process and its operating
schedule, and on the schedule of variation of the waste composi-
tion, if that is known. The greater the variability, the more
composite samples must be taken. The volume of waste required
also must be determined beforehand, and usually is dictated by the
analyses to be performed and the homogeneity of the waste mate-
rial. For example, a one-liter daily composite could consist of
five 200-ml samples taken at two-hour intervals throughout the
day; a weekly composite could consist of seven samples taken on
seven consecutive days and then combined. The schedule for a
composite sample is process-dependent and should be decided upon
by someone who is familiar with the process and who understands
the need for a representative sample.
Spatial Variability
Spatial variability within a container, pile, landfill, or
lagoon may be vertical or horizontal. Contained wastes have a
much greater tendency to vary in a vertical rather than a hori-
zontal direction because of (1) the settling of solids and the
denser phases of liquids and (2) variations in the composition of
the waste as it entered the container.
It is necessary to characterize the waste's variability in
both the horizontal and vertical dimensions. This usually means
collecting a complete vertical sample of the waste at each of
several randomly selected points on a horizontal grid. Appro-
priate methods for accomplishing this are described in Section
7.3. The number of samples to be taken will vary with the size of
the containment area and the degree of spatial variability. A
minimum of four samples should be drawn from each storage location
- 30 -
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or container, even if the waste appears to be homogeneous. In
many cases, however, more than four samples will be required to
adequately characterize the waste. (Drums form a partial excep-
tion to this rule, as described below; one sample per drum will
usually suffice.)
An Example
To illustrate the application of the above principles, we
consider the case of an electroplating line that generates sludge
continuously from rinsing operations (Waste No. F006). Once every
six weeks, however, the plating baths themselves are dumped into
the waste stream. The waste is held in a tank with a residence
time of about two days, and neutralized before being discharged to
a surface impoundment via a pipe. The plating process used in the
plant was implemented two years ago, prior to which a different
process was used.
First, let us assume that the delisting petition applies only
to the currently discharged waste stream. On the basis of the
above information, the Agency would expect the generator to sample
the waste stream over at least a six-week period. In particular,
samples should be taken during the two days in which the plating
baths themselves are resident in the sludge, to demonstrate the
variability of the neutralized sludge due to discharge of the
plating baths.
If the petition includes the sludge stored in the surface
impoundment in addition to the current discharge, then the genera-
tor must take representative samples of the sludge in the impound-
ment as well. Because the waste-generating process was changed
two years ago, there will most likely be vertical non-homogeneity
in the stored sludge. Therefore, full-core samples of the im-
pounded sludge would be necessary. In addition, it is likely that
horizontal variability will occur in the impoundment because the
sludge is discharged into it at a fixed point. Therefore, samples
should be collected at randomly spaced points on a horizontal
grid.
7.2 Sampling Equipment
This section contains a brief description of the most common
sampling devices: dippers, weighted bottles, COLIWASAs, thiefs,
triers, and augers. Detailed descriptions and directions for
obtaining or constructing the equipment can be found in EPA Publi-
cation No. SW-846, "Test Methods for Evaluating Solid Waste,"
second edition.
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Dipper
A dipper consists of a glass or nonreactive plastic beaker
clamped to the end of a pole, which serves as the handle (see
Figure 7.1). It is used to sample flowing liquids and slurries.
The dipper can be varied in size depending on the flow rate of the
waste stream.
Weighted Bottle
This sampling device consists of a glass or nonreactive
plastic bottle with an attached sinker or weight, stopper, and a
line which is .used to lower, raise, and open the bottle. It is
used to sample liquids and slurries. Figure 7.2 depicts a weight-
ed bottle sampler.
COLIWASA
A COLIWASA (composite ^Liquid waste s_ampler) is a glass,
plastic, or metal tube with an end closure that can be opened and
closed while the tube is submerged (see Figure 7.3). This sam-
pling device is useful for free-flowing liquids and slurries
contained in drums, shallow open-top tanks, pits, and similar
containers. It is especially useful for sampling wastes that
consist of several immiscible liquid phases. The COLIWASA is
lowered into the waste at a rate slow enough to permit the level
of liquid inside and outside the sampler to remain the same. When
the sampler hits the bottom, the stopper is closed. In this
manner, a sample is obtained that is representative of the entire
depth of the waste.
Thief
A thief consists of two slotted concentric tubes usually made
of stainless steel or brass (see Figure 7.4). The outer tube has
a conical pointed top- which permits the sampler to penetrate the
material being sampled. The inner tube is rotated to open and
close the sampler. A thief is used to sample dry granules or
powdered wastes whose particle diameter is less than one-third the
width of the slots. A thief is available at laboratory supply
stores.
Trier
A trier consists of a tube cut in half lengthwise with a
sharpened tip that allows the sampler to cut into sticky solids
and loose soil (see Figure 7.5). The trier is then rotated to cut
a core of the waste. A trier samples moist or sticky solids
having a particle diameter less than one-half the diameter of the
trier. Triers can be found at laboratory supply stores, or they
can be fabricated.
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FIGURE 7.1: DIPPER SAMPLER
(Source: Test Methods for Evaluating Solid Wastes, 2nd Edition,
U.S. EPA, SW-846, July 1982)
Varigrip Clamp
Telescoping Aluminum Pole
2.S to 4.5 Meters (8 to IS ft.)
Beaker
150lo600ml
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FIGURE 7.2: WEIGHTED BOTTLE SAMPLER
(Source: Test Methods' for Evaluating Solid Wastes, 2nd Edition,
U.S. EPA, SW-846, July 1982)
Washer
Nut
- 34 -
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FIGURE 7.3: COMPOSITE LIQUID WASTE SAMPLER
(Source: Test Methods for Evaluating Solid Wastes, 2nd Edition,
U.S. EPA, SW-846, July 1982)
2.86cm (1 1/8")
c
Tapered v
Stopper 1
f
II
II
II
II
II
1
I 1
1!
II
II
II
1 1
II
II
II
II
II
II
II
II
ii
II
II
II
II
II
II
II
II
II
II
35
13
i
T-Handle fr
6.35 cm (2 Vt Locking J
Slock H
1
1
1
1
1
I
1
1
1
1
1
1
1.52m (S'-O") 1
1
1
I
1
1
1
1
1
|
~y _, 1
1
1
1
1
r |
IT
IT
17.8 em (7")
4,
1
| Stopper Rod. PVC
0.95cm (3/8") 0. D.
I
1
1 Pipe, PVC. 4.13 cm (1 5/8") I D.
I ^ 4.26cm (1 7/8") 0. D.
I
I
I
I
I
I
I
I
I
I
I
I
I
J ., Stopper, Neoprene. No. 9 with
-1 ' 3/8" S. S. or PVC Nut and Watfier
SAMPLING POSITION
CLOSE POSITION
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FIGURE 7.4: THIEF SAMPLER
(Source: Test Methods for Evaluating Solid Wastes, 2nd Edition,
U.S. EPA, SW-846, July 1982)
60-100 cm
V
1.27-2.54 cm
36 -
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FIGURE 7.5: SAMPLING TRIERS
(Source: Test Methods for Evaluating Solid Wastes
U.S. EPA, SW-846, July 1982)
2nd Edition,
-^ ,___.. 122-183 cm _.
(48-72")
^\
T
5.08-7.32 cm
60— 100cm
\
\
1.27-2.54 cm
- 37 -
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An auger consists of sharpened spiral blades attached to a
•hard metal central shaft. Augers sample hard or packed solid
wastes or soil. They are available at hardware stores or labora-
tory supply stores.
7.3 Sampling Techniques for Specific Forms of Waste
In this section, sampling techniques are presented for va-
rious sampling situations: sampling from pipes and other process
discharges; drums; landfills; lagoons; and waste piles. We also
describe an approach for taking samples at multiple waste treat-
ment facilities.
•The variety of physical forms of waste and the uniqueness of
each sampling situation necessitates a flexible approach to ac-
quiring samples. The procedures discussed here are believed to
represent the best approaches to sampling different forms of
waste; however, the technique that you select should be devised in
each case by a person familiar with the process and with general
principles of sampling.
Pipes and Other Process Discharges
Representative samples from pipes and other process dis-
charges are best obtained through time composite sampling, which
was described in section 7.1 of this chapter. Composite sampling
may be performed through the use of automatic compositers, or it
may be done manually. This discussion assumes that manual sam-
pling is performed.
There are two general types of process discharges: liquid or
slurry discharges, and solid or semi-solid discharges. Liquids or
slurries generally will be sampled from pipes, valves, or sluice-
ways. Solid process discharges are often sampled from conveyor
belts or filter presses.
For slurry and liquid discharges, a dipper-type sampler
should be used. The dipper can be easily constructed out of
materials on hand at the plant. The dipper bucket should be of an
appropriate non-reactive material, similar to the sample contain-
ers. The size of the bucket used should increase with increasing
stream flow rate. A dipper should be used to sample only one
waste stream and it should be cleaned aftuer each sample is
collected.
Each time a grab sample is taken, the dipper is first rinsed
in the sampled stream. Then the dipper is passed in one sweeping
motion through the discharge stream so that the dipper is filled
- 38 -
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in one pass. Do not sample from the edge of the stream only. , If
the cross-sectional area of the stream is large in comparison with
the size of the dipper, more than one pass may be necessary to
sweep the entire cross-sectional area of the stream. Each grab
sample should be emptied into the composite container and the
entire contents mixed well.
Solid or semi-solid discharges on a belt should be sampled
with a scoop or a shovel. The shovel should be chosen or fabri-
cated to match the width and general contour of the belt as close-
ly as possible. The grab samples can be taken at any convenient
point along the belt, as long as the entire width of the belt is
sampled. Any fines or liquid present on the belt at the sampling
point should be included in the sample.
Another common type of solid discharge is filter cake. If
samples are taken as the material is produced, then a trowel or
shovel may be useful, depending on the type of filter. Care
should be taken so that the entire waste stream is represented by
the sample
In each case, the frequency of sampling and the number of
individual grab samples that are combined to form a composite
depends on the variability of the waste over time and on the time
span which the sample is to represent. For sampling point dis-
charges as they are generated, samples can be taken every hour for
eight to 24 hours, depending on the process schedule, and combined
to form a daily composite. As an alternative, samples can be
taken daily for a week, and the daily samples combined into a
weekly composite. Again, the sampling period and number of sam-
ples will vary for each petitioner. Therefore, it is important
that whoever takes the sample be familiar with the spatial and
temporal variability of the waste stream.
Often solid discharges, such as filter cakes, fall from the
press or plate-and-frame filter into a hopper or storage area.
In this case, a more long-term composite may be obtained by samp-
ling the material after it has accumulated for a period of time.
For example, filter cake can be allowed to accumulate in a hopper
for 24 hours, and then random core samples can be taken using a
simple two-dimensional random sampling strategy. (If separation
of the waste — such as by the expression of liquids — appears to
have occurred in the storage container, mix the waste well before
drawing the samples.) The samples would be combined to form a 24-
hour composite. The process would be repeated enough times to
obtain the number of samples required for analysis. Sampling
filter cake from a hopper would require the use of a thief or a
trier, depending on the water content of the material. In each
case, the composite should be mixed until it is homogeneous before
sub-samples are split for analysis.
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Drums
If the waste is contained in drums, then ideally each drum
should be sampled. If there are too many drums for this to be
practical, then a representative number of individual drums must
be randomly selected. This is easily done by assigning a number
to each drum consecutively and then using a random number table to
choose the sample. A detailed method for selecting drums for
sampling may be found in the following publication:
"Waste Analysis Plans: A Guidance Manual," U.S. EPA Office
of Solid Waste, Publication EPA/530-SW-84-012, October 1984.
For each drum, a single sample that samples the entire depth
of the drum along its axis is sufficient. Equipment used for sam-
pling waste in drums includes weighted bottles (for heterogeneous
wastes), COLIWASAs, thiefs, and triers. COLIWASAs and weighted
bottles are best suited to sampling liquids and slurries; if the
sample is dry granules or a powder, a drum thief should be used.
A trier should be used to sample moist or sticky solids.
Landfills
Wastes contained in landfills are primarily solids or moist
solids. These wastes are best sampled using a two-dimensional
random sampling strategy as described below. (The procedure is
also illustrated in Figure 7.6).
(1) On a dia.gram, divide the landfill to be sampled into
sections of equal area. If the area is under 40,000
square feet, then it should be divided into four equal
quadrants. If the area is over 40,000 square feet, then
it should be divided into equal sections of not more
than 10,000 square feet each.
(2) Divide each quadrant or section into an imaginary 10x10
grid to get 100 squares (or rectangles) of equal size.
Number the grid lines in each dimension from 1 to 9.
(3) For each section, determine the number of sampling
points necessary to characterize the waste. This number
will depend on the degree of spatial variability within
the landfill.
(4) Select a two-digit number using a random number table.
Repeat this procedure until you have one two-digit num-
ber for each sampling point in the section. (Random
number tables are available in any introductory statis-
tics text or handbook. Their use is explained in.Appen-
dix G. )
(5) Locate the grid intersections whose coordinates corres-
pond to each of the two-digit random numbers. These
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FIGURE 7.6: SCHEMATIC DIAGRAM OF SAMPLING GRID FOR A LANDFILL
The Figure shows a 30,000 sq ft landfill (150 ft x 200 ft)
divided into four 7,500 sq ft quadrants.
i
2
3
4
S
6
7
8
9
Quadrant 1
Sampling point (corresponds
to randoa nuaber 82)
Quadrant 2
Quadrant 4
I Z
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intersections are the locations of the randomly selected
sampling points.
(6) Sample each selected grid point vertically along the
entire distance from the top to the bottom of the land-
fill.
(7) Combine the samples for each section and mix them well
to form a homogeneous composite sample. Do not, how-
ever, combine samples from different sections.
For example, a landfill of 10,000 square feet would be divided
into four quadrants of 2,500 square feet each. In each quadrant,
a sufficient number of core samples would be taken and combined.
The result would be four homogeneous composite samples, one from
each quadrant. Similarly, a landfill of 60,000 square feet would
be divided into six sections of 10,000 square feet each, yielding
six homogeneous composite samples.
It is particularly important to obtain vertical samples along
the entire depth, including the bottom. Hollow-stem augers com-
bined with split-spoon samplers are frequently useful for sampling
landfills. Triers or modified triers also may be used.
Lagoons
Lagoons are similar to landfills in that they cover a large
area and stratification and settling are likely to occur. The
same two-dimensional randomized sampling strategy therefore may be
used. Again, it is important that each sample include material
from the entire depth of the lagoon, including the bottom.* This
can be done by using a COLIWASA.
Waste Piles
Ideally, waste piles should be divided into quadrants (in a
similar fashion to landfills), and each quadrant sampled using a
two-dimensional grid and random vertical core samples. Equipment
commonly used to sample piles includes thiefs, triers, and shovels.
Multiple Waste Treatment Facilities
The variety and number of incoming wastes accepted at mul-
tiple waste treatment facilities (MWTFs) result in less control
over the variability of constituent concentrations. Since -
inherent variability makes it difficult to collect representative
*Note that if the listed waste is a sludge (e.g., Waste No,
F006), the liquid above the sludge, if any, need not be sampled.
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samples, the MWTF petitioner has fewer options available to demon-
strate the non-hazardousness of his waste. To obtain representa-
tive samples, the following guidelines are suggested:
• Analyze as many samples as necessary to represent varia-
bility in toxicant concentrations in the treatment residue
generated annually. (The Agency believes that a minimum
of eight weekly composite samples should be collected over
a minimum period of two months.)
• Determine what percentage of waste treated annually is
treated during the sampling period.
• Explain why the remaining percentage of the waste would not
be expected to contain any hazardous constituents; dif-
ferent levels of these constituents; or different charac-
teristics than the waste sampled.
7.4 Sample Handling, Storage, and Documentation
Samples collected must be handled, labeled, and stored so
that sample integrity is preserved. In addition, proper documen-
tation of sample collection, preservation, and custody is essen-
tial.
Handling and Storage
Containers. Samples should be collected and composited in
glass, polytetrafluoroethylene (PTFE), or plastic containers with
tight, screw-type lids. PTFE lid liners should be used if organic
analyses are to be performed on the sample. Containers made of
plastic other than PTFE should not be used if organic analyses are
to be performed.
On-Site Preservation. Once a sample has been collected,
steps must be taken to preserve the physical and chemical integri-
ty of the sample during transport and analysis. Sample preserva-
tion and storage requirements vary according to the analysis to be
performed. Therefore, it may be necessary to prepare more than
one container of the waste material to accommodate the different
analyses. Again, refer to EPA Publication SW-846 for detailed
preservation procedures.
Identification and Labeling. Each container should be as-
signed a unique sample identification number. An indelible label
should be secured to the container that identifies the sample.
The label should contain the following information:
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Sample identification number
Name of collector
Date and time of collection
Place of collection
The label should be filled out after the container is filled to
avoid spilling the sample onto the label. Finally, the label
should be completely covered with wide cellophane tape to ensure
that the labels remain attached and dry throughout shipping and
analysis.
Shipping. After the samples have been preserved, labeled,
and sealed, they are ready for shipping. Samples should be ship-
ped and analyzed as rapidly as possible to ensure that the most
accurate and reliable data can be obtained.
There are four areas of concern: 1) protection of carriers
and receivers, 2) preservation of samples, 3) rapid and efficient
transit, and 4) compliance with DOT regulations.
Specific DOT requirements for the packaging of hazardous
environmental laboratory samples can be found in 49 CFR 173.24 and
173.6. In general, these requirements state that hazardous sam-
ples must be packaged in such a way that under normal conditions
of transportation, no significant release of hazardous materials
to the environment will occur due to breakage, leakage, or reac-
tion with packing materials.
The following recommendations are patterned after EPA-recom-
mended procedures which are designed to comply with DOT regula-
tions.
• Shipping containers must be designed such that they will
withstand a four-foot drop on solid concrete in the posi-
tion most likely to cause damage. A good example is a
metal clad cooler lined with plastic. The container
should be taped shut and the drain plug at the bottom
secured to prevent leakage. The container should be
marked "THIS END UP" in proper position.
• Glass containers must be packed in a shipping container in
a manner that minimizes the possibility of breakage or
leakage. Screw-type lids should be securely tightened.
Large glass bottles should be separated by cushioning
material. Containers should be sealed in plastic bags or
packed in absorbent material in case breakage does occur.
• Plastic- containers, though not requiring packaging to
prevent breakage, are packed with a cushioning material to
prevent leakage by puncture. Screw-type lids should be
tightened securely.
• If the sample is to be analyzed for volatile organics, it
should be packed in a cooler and maintained at 4°C.
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Documentation
In addition to labels and seals, there are three types of
documentation necessary to ensure the integrity of the sample: a
chain-of-custody record, a field log book, and a sample analysis
request sheet.
A chain-of-custody record should be filled out and should
accompany every sample. The record should contain the following
information: sample identification number, signature of collect-
or, date and time of collection, place and address of collection,
and waste type. A place also should be provided for the signature
of each person who has the samples in their possession, along with
the inclusive.dates of possession.
In addition, all information pertinent to a field survey or
sampling must be recorded in a log book. Entries in the log book
should include the following items:
Date and time of sampling
Collector's name and affiliation
Process sampled
Type of waste (e.g., sludge, wastewater)
Exact location of all sampling points (drawings
may be helpful)
Description of sampling methodology
Number, volume, and appearance of samples
Any field measurements made
Field observations
Any deviations from the sample plan or any problems should be
noted. In general, sufficient information should be recorded so
that the sampling can be entirely reconstructed without reliance
on the collector's memory.
Finally, a sample analysis request sheet should accompany the
sample to the laboratory. The sheet should specify the following
items:
Sample identification number
Description of sample
Date
Analyses to be performed
On-site preservation
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You should preserve all chain-of-custody documents, log
books, and similar records in case a question arises regarding the
sampling portion of your petition.
7.5 The Written Sampling Plan
A written sampling plan should be prepared for even the
simplest sampling efforts. This will ensure that proper planning
has taken place and that planned procedures are followed. The
sampling plan .also will serve as the basis for demonstrating the
representativeness of your samples in the petition. A good sam-
pling plan should contain the following information:
• Purpose of the sampling effort
• List of the waste stream or streams to be sampled
• Name of the sampler (or sampling crew for larger efforts)
• Professional qualifications of the samplers
• Sampling strategy, e.g., time composite
• Detailed sampling procedures, including location of sam-
pling points, equipment needed, and sample containers
• Safety procedures, including safety equipment
• Any on-site preservation that will be performed
• Analytical lab to be used and method of transport
• Analyses to be performed
• Plans for documentation of the sampling effort
Instructions for reporting your sampling procedures are given in
Section 9 below.
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8.0 SELECTION OF WASTE ANALYSIS METHODS
In this section, we describe briefly the methods to be used
to analyze the waste for the hazardous characteristics and con-
stituents. The methods themselves are complex and require fairly
elaborate laboratory facilities. Most of the methods specified
for these tests may be found in the following EPA Publication:
"Test Methods for Evaluating Solid Waste: Physical/Chemical
Methods," and its supplements and revisions, SW-846 (second
edition), June 1982. Referred to here as "SW-S46".
Additional methods ara contained in Appendix J of this Manual.
The design and execution of the testing program should be
done by an analytical chemist with the proper qualifications. If
you do not have the necessary personnel or laboratory resources
in-house, you should contract with a commercial testing laboratory
or a consulting analytical chemist with experience in hazardous
waste. A list of typical 1984 prices for the tests described in
this section is included in Appendix H.
8.1 Tests for Characteristics
You must determine whether the waste exhibits one of the four
characteristics (ignitability, corrosivity, reactivity, and EP
toxicity). This determination may take the form of an explanation
of why the waste cannot exhibit one or more of the characteris-
tics. (For example, a waste stream composed entirely of organic
solvents would not contain any of the EP toxicants listed in
Section 261.24.) If you cannot explain conclusively a character-
istic's absence, you must test for it instead. If you test for a
characteristic, any analyses must be performed on as many samples
as are necessary to be representative of the waste (see Chapter 7
above), but on no fewer than four samples.
1. Ignitability. (See Section 261.21) This characteristic
identifies wastes that either present fire hazards under routine
storage, disposal, and transportation or are capable of severely
exacerbating a fire once it is started. Ignitability for a liquid
is defined in terms of its flash point. For a non-liquid, it is
the ability to cause fire through friction, absorption, moisture,
or spontaneous chemical change. The most common test for ignita-
ble liquids, the Pensky-Martens Closed-Cup method, involves heat-
ing a sample slowly and determining the minimum temperature at
which a small flame ignites the vapor above the sample (see SW-
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346). The ignitability characteristic for non-liquids is a de-
scriptive standard, and does not specify a test procedure.
2. Corrosivity. (See Section 261.22} This characteristic
identifies wastes which might pose a hazard to human health or the
environment due to their ability to:
• Mobilize toxic metals;
• Corrode handling, storage, transportation, and management
equipment; or
• Destroy human or animal tissue in the event of inadvertent
contact.
A waste is defined as corrosive if: (a) it is aqueous and has a pH
of less than or equal to 2 or greater than or equal to 12.5, or
(b) it is a liquid and corrodes a specific grade of steel at a
rate greater than 6.35 mm per year under standardized test con-
ditions. Test methods are given in SW-346.
3. Reactivity. (See Section 261.23) This characteristic
identifies wastes which, because of their extreme instability and
tendency to react violently or to explode, pose problems at all
stages of the waste management process. In particular, such
wastes have any of the following properties:
• They readily undergo violent chemical change;
• They react violently OT form potentially explosive
mixtures with water;
•> They generate toxic fumes when mixed with water or, in the
case of cyanide or sulfide-bearing wastes, when exposed
to acidic or basic conditions;
• They explode when subjected to a strong initiating force;
• They explode at normal temperatures and pressures; or
• They fit within the Department of Transportation^
forbidden explosives classifications.
Several methods for testing for reactivity are available,
although none are comprehensive. The Defense Logistics Agency°s
Explosives Hazard Classification Procedures (DLAR 8220.1) pre-
scribe a blasting-cap test (see Appendix J). Methods 9010 and
9030 in SW-846 measure cyanide and sulfides, respectively. In
addition, a gas-generation test for reactive cyanide and sulfides
in waste is contained in Appendix J, as is a test for photo-
degradable cyanide. Descriptions of reactive wastes may be found
in SW-846. In general, if you are dealing with an explosive
waste, please contact EPA°s Waste Identification Branch at (202)
475-8551 for further guidance on test methods.
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4. Extraction Procedure (EP) Toxicity. (See Section 261.24)
The Extraction Procedure is designed to simulate the leaching that
a waste will undergo if it is disposed of in a sanitary landfill.
In a laboratory, a representative sample of a waste is extracted
with deionized water maintained at a pH of 5 using acetic acid.
The extract obtained from the procedure (the "EP extract") is
analyzed to determine if any of the thresholds for the eight
metals, four pesticides, and two herbicides specified in the
regulations have been exceeded.* At least one EP toxicity test
for each EP metal should be run using the method of standard
additions. Spike and recovery concentrations and recovery effi-
ciency should be reported.
8.2 Tests for Constituents
In addition to testing for the characteristics as described
above, the following tests should be conducted as appropriate for
the waste stream.
• If cyanide was a constituent for which the waste was
listed, or if it is expected to be present in the waste,
analyze for total cyanide (see SW-846). If the total
concentration recorded is greater than 1 ppm, test for
free cyanide (see SW-846). If the concentration of total
cyanide is greater than 10 ppm, perform the photoconver-
sion test for photodegradable cyanide (see Appendix J).
• If the cyanide analysis indicates the presence of an
interference in the waste that produces non-representa-
tive concentrations, note and explain the interference.
In addition, perform the following test (see Appendix J):
"Test Method for the Determination of Reactive Cya-
nide and Sulfide Containing Wastes, Final Method".
• Perform a total constituent analysis by complete acid
digestion for all the EP metals and nickel (if nickel is
a constituent for which the waste was listed). See SW-
846 for a description of the method.
• Perform the Total Oil and Grease analysis to determine
the percent of total mass that is oil and grease. The
*Note that if the total constituent analysis described below
shows that one or more of the EP metals is not present or is
present at concentrations of less than regulatory concern, then
you may not have to test for those metals in the SP Toxicity Test.
Contact the Waste Identification Branch for guidance on specific
cases.
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method involves drying the waste and then extracting the
constituent oil and grease with an organic solvent such
as freon.
• If the Total Oil and Grease analysis shows that the total
oil and grease content of the waste is 1 percent or more,
the EP Toxicity Test for Oily Wastes should be used (see
Appendix J).
• Analyze,for Total Organic Carbon (see Appendix J). In
this test, organic carbon is converted to carbon dioxide
by analytic combustion or wet chemical oxidation. The
COo formed can be measured or converted to methane (CH4)
and measured. The amount of C02 or CH^ is directly
proportional to the concentration of carbonaceous mater-
ial in the sample.
• Identify and quantify individual organic constituents.
This must usually be done using gas chromatography-mass
spectrometry (GC-MS) methods. Applicable methods are
contained in SW-846.
If chromium, cyanide, and nickel are listed constituents,
tests for them may be combined with the EP toxicity test. For the
first two compounds, the following special procedures apply:
• Analyze the EP.extract for total chromium and hexavalent
chromium separately. Report initial and final pH data on
the hexavalent chromium EP analysis. If the pH drops
from an alkaline or neutral value to ah acidic pH, then
alkaline digestion of the waste is required before ana-
lyzing for hexavalent chromium (Method 3060 in SW-846).
• Test for extractable cyanide using the EP procedure,
using distilled water only (instead of acetic acid) as
the extract medium.
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9.0 PRESENTATION OF ANALYTICAL DATA
The data from the analytical tests should be presented in a
format that supports your contention that the waste:
a. Does not exhibit any of the hazardous waste characteris-
tics, and
b. Is not hazardous based on the constituents for which it
was listed.
In addition, you must provide the necessary information on other
hazardous constituents so that the Agency can determine whether
the waste may reasonably be hazardous for any other reason. We
also request data on other topics such as quality control proce-
dure. This chapter corresponds to Part S of the optional petition
form in Appendix A.
9 .1 General Information
Please provide the names and addresses of the consultants or
laboratory•facilities that
(a) sampled the waste, and
(b) tested the samples.
If sampling or testing were performed using in-house staff and
equipment, indicate that fact. In addition, please provide the
names and qualifications of the persons who designed the sampling
plan, drew samples, designed the test plan and performed the
analytical tests (Section 260.22(i)(l) and (2)).
9.2 Sampling Information
Demonstrating that the waste samples are representative is a
particularly important requirement of the delisting process. Many
of the petitions we receive are deficient in this area. There-
fore, please submit:
• A detailed description of your sampling strategy. The
description should state why you believe the samples
tested are representative of the waste stream, including
any variations in the waste's properties over time and
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space. In the case of process buttlows, state whether all
major equipment items, raw materials, and operating condi-
tions are represented. In the oUsJ) of storage locations,
describe how sampling points werV^elected and how samples
were drawn. Note that each outflow and storage loca-
tion included in this petition must be sampled in a rep-
resentative manner.
• A description of the documentation system used to track
the samples; or, a statement that the Chain-of-Custody
system specified in Section 1.3 of' SW-846 was used.
In addition, please furnish the following information for
each sample:
• The sample number, as it appears in your logbook or other
record.
• The location where the sample was taken. Specify the
general location (e.g., the outflow, lagoon, pile, etc.)
and the specific point of sampling (e.g., quadrant and
depth in a lagoon). Include a diagram.
• The equipment used for drawing the sample (Section
260.22(i)(8)).
• The date on which it was drawn (Section 260.22(i)(3)).
• The time of day when it was drawn.
• The handling and preparation techniques used, including
techniques for extraction, containerization, and preserva-
tion (Section 260.'22(i) (9) ) .
9.3 Test Results
For each test performed on each sample, please report the
following information:
• The hazard being tested for;
• The specific substance or parameter being tested for;
• The date the test was performed (Section 260.22(i)(3));
• The test method used (Section 260.22(i)(10));
• The source of the test method used. Sources for methods
are:
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- "Test Methods for Evaluating Solid Waste: Physical/
Chemical Methods," and its supplements and revisions,
SW-846 (second edition), June, 1982, and
- Appendix J of this manual.
• The sample workup or preparation method.
• The names and model numbers of all equipment used in the
tests (Section 260.22(i)(11)).
• The test results, expressing concentrations in common
units such as mg/1, ppm, etc. (Section 260.22(i)(10)).
• Quality control procedures.
• Any supplementary information needed to interpret the
test procedures or results.
Append a discussion explaining any inconsistencies or deviations
among the analytical results presented.
9.4 Quality Assurance and Quality Control
It is important to report the methods taken to insure the
quality of the sampling and testing procedure, so that our review-
ers will know how much confidence to place in the results. In the
case of inorganic substances, Standards Addition Analysis can be
used for this purpose. In this method, a sample of the waste is
"spiked" with a known concentration of the substance in question
prior to being analyzed. 'The spike concentration should be ap-
proximately the same as the anticipated level of the constituent
in the waste. If the concentration of the constituent is below
the detection limit, then the spike concentration should be be-
tween three and ten times the detection limit. At least one test
should be run for each substance. You should report:
• The spike concentration,
• The recovery concentration, and
• The recovery efficiency.
In the case of organic constituents, you should spike the
sample with the substance of interest if possible. It may be
necessary, however, to use a surrogate substance. This may be the
case because a standard is not otherwise available, or because of
interferences from other substances in the waste. Surrogates
should be chosen on the basis of similar chemical structure to the
substance of interest; similarity of physical properties such as
boiling and melting points may also be considered. The spike
concentration for the substance or its surrogate should be as
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described above. Methods for calibrating the gas chromatography
apparatus when using internal or external standards are described
in SW-846 (see, for example, Section 7.2 of Method 8020).
When reporting the results of the spike analysis for or-
ganics, give the spike concentration, recovery concentration, and
recovery efficiency as specified above. In addition, please spe-
cify which substance, if any, was used as a surrogate for the
compound of interest, and provide details of the method used to
calibrate the analytical equipment.
Describe any other quality control measures taken as well.
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APPENDIX A
OPTIONAL FORM FOR DELISTING PETITIONS
-------
OPTIONAL FORM:
DELISTING PETITION FOR WASTE STREAM
Submitted by:
Date:
A-3
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INSTRUCTIONS
1. This form is meant to assist you in submitting a petition to
delist a RCRA hazardous waste under the provisions of Section
260.22 of the hazardous waste regulations. Its use is option-
al. Any part of the form may be changed or adapted to your
circumstance, provided that all information submitted is
clear, complete, and conforms to the regulatory requirements.
2. Instructions for completing this petition form are contained
in the document entitled, "Petitions to Delist Hazardous
Wastes: A Guidance Manual," EPA/530-SW-85-003, April 1935.
The manual is available from the National Technical Informa-
tion Service. Please review the manual thoroughly before
attempting to develop your petition. Should you need further
assistance, it may be obtained by calling the Environmental
Protection Agency's RCRA Hotline, at (800) 424-9346 (in the
Washington, D.C. area, 382-3000).
3. Certain types of facilities, such as petroleum refineries and
multiple waste treatment facilities, are required to submit
information in addition to or in lieu of the information
specified in this form. Petitioners for such facilities
should refer to Section 4.3 of the Guidance Manual and adapt
this form as appropriate.
4. Items that you are required to submit are designated by refer-
ences to the appropriate parts of the hazardous waste regula-
tions .
5. If insufficient space is provided for your answers, attach
extra sheets as necessary.
6. Please submit completed petitions to:
The Administrator
US Environmental Protection Agency
401 M Street SW
Washington, D.C. 20460
In addition, send a copy to:
Chief, Waste Identification Branch
Office of Solid Waste (WH-562B)
US Environmental Protection Agency
401 M Street, SW
Washington, D.C. 20460
A-5
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7. Please be sure to provide the following items, which are often
omitted. Their omission will delay the review process and may
cause extra work for you and for EPA.
RCRA ID Numbers
Facility contact(s) and telephone numbers
Material safety data sheets, where requested
Waste generation quantities
Signed certification statement
Statement of sample representativeness
Statement of waste's ignitibility/reactivity/corrosivity
A-6
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SECTION A: Administrative Data and Summary
1. Name [260.20(b)(1)]
a. Name of firm:
b. Address of firm: Street:
City:
State: Zip:
c. RCRA Generator ID number:
2. Facility Location [260.20(b)(1)]
a. Name of facility:
b. Location of facility: Street:
City:
State: Zip:
3. Name(s) of personnel to be contacted for additional informa-
tion pertaining to this petition:
Name Title Telephone
A-7
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4. Description and Justification for the Proposed Action
Please describe briefly the proposed delisting action, why it
is needed, and how it will affect your operation. Describe
why you believe that the waste stream of concern (a) is not
hazardous for the reasons it was originally listed and (b)
contains no other constituents or characteristics that render
it hazardous as defined in 40 CFR 261. [ 260.20(b) (2), (3) and
(4)]
5. Certification of Accuracy and Responsibility [260.22(i) (12)]
I certify under penalty of law that I have personally examined
and am familiar with the information submitted in this demon-
stration and all attached documents, and that based on my
inquiry of those individuals immediately responsible for ob-
taining the information, I believe that the submitted informa-
tion is true, accurate, and complete. I am aware that there
are significant penalties for submitting false information,
including the possibility of fine and imprisonment.
Signed,>
Waste Generator, Title or
Authorized Representative*
of Waste Generator, Title
*Note: An "authorized representative" is a person respon-
sible for the overall operation of a facility or an opera-
tional unit (for example, a plant manager, superintendent,
or person of equivalent responsibility). Consultants or
other outside parties may not sign the certification state-
ment .
A-8
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SECTION B: Production Processes
1. Description of Manufacturing Processes and Other Operations
C260.22(i)(5)].
a. Please provide a brief description of the on-site
manufacturing/generating process(es) that produce the
waste stream. Include descriptions of major equipment
items .and production lines. Also, describe the stages of
the typical operating cycle (e.g., startup, steady-state
operation, cleaning and maintenance) on a daily, weekly,
or other basis as appropriate.
b. Please provide a description of all surface and equipment
preparation, cleaning, degreasing, coating or painting
processes used in your facility that you have not
described in (a) above.
Attach a schematic diagram of all manufacturing processes,
surface preparation, cleaning, and other operations that
may provide influent into the waste stream.
A-9
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2. Materials Used or Produced
You may comply with the requirements for additional
information in either of two ways; see Section 4 of the
Guidance Manual for a detailed description of the two
approaches.
Approach A;
a. List all materials used or produced in the manufacturing
or other process generating the waste stream(s). Use the
correct chemical name wherever possible. Include mate-
rials such as:
Raw materials
Intermediate products
By-products
Products
Oils and hydraulic fluids
Surface preparation materials
(solvents, acids, cleaners, surface
preparation agents, paints, etc.)
Also:
• For each material on the list, indicate whether it is
discharged to or likely to be present in the waste, and
the estimated amount entering the waste stream annual-
ly. (Specify kilograms, pounds, or similar units.)
Describe your estimation method.
• For each material on the list that you do not expect to
be present in the waste, give supporting reasons for
this expectation. Supporting reasons may include mass
balance and process information.
• Attach Materials Safety Data Sheets (MSDS) for all
materials that are identified by trade or generic name
only and that are discharged into or likely to be
present in the waste stream.
Estimated Amount
Material Entering the Waste
Stream Annually
(Continue on additional sheets as necessary)
A-10
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b. Please give your assessment of the likelihood that the
processes, operations, or feed materials described above
might produce a waste stream that is not included in this
petition.
Approach B;
You need not furnish any other information regarding your
facility's processes and materials. You must, however, test
your waste for additional constituents as described in Chap-
ters 4 and 6 of the Guidance Manual.
A-ll
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SECTION C: The Waste Stream
1. EPA hazardous waste number and description of waste stream
(from 261.31 or 261.32):
No. Description
Form of the waste (e.g., aqueous solution, sludge, dry solids):
If the waste is a sludge, give the percent solids:
2. Estimated average and maximum monthly and annual quantities
generated: (Please use consistent units of measurement.)
Average Maximum
Monthly
Annually
3. This waste stream: (check all that apply)
Is currently being generated.
Will be generated in the future.
Has been generated in the past and is currently
being treated/stored on-site.
Has been generated in the past and is currently
being treated/stored off-site.
A-12
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4. Present methods of on-site storage, and amounts being stored:
Amount
Surface impoundment,
Evaporation pond
Percolation bed
Waste pile(s)
Tank(s)
Containers
Landfill
Drums
Other (please specify)
5. Waste Management Methods:
Briefly describe:
(a) how the waste is currently managed;
(b) how it was managed before November 19, 1980; and
(c) how it will be managed if this petition is approved,
As appropriate, provide names and locations of off-site treat-
ment, storage or disposal facilities, and names and addresses
of waste transportation firms.
If the waste is treated prior to disposal, please attach a
schematic flow diagram of your present waste treatment system,
showing the processes and equipment used.
A-13
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SECTION D: Selection of Constituents for Testing
The procedures described below apply to all types of wastes
other than those from petroleum refineries and multiple waste
treatment facilities. Petitioners for these facilities should
refer to Section 4 of the Guidance Manual and adapt this
section of the petition appropriately.
1. If you have followed Approach A in Section B above, please
submit test results on representative samples for the follow-
ing:
• The specific hazardous constituents for which the
waste was listed (i.e., total concentration of each
listed constituent found in Appendix VII of Part
261) ;
• The four hazardous waste characteristics (but see the
Note immediately below);
• Appropriate leachate tests for the EP toxic metals,
nickel, and cyanide;
• Total concentrations of the EP toxic metals and
nickel;
• Total organic carbon (TOC); and
• Total oil and grease.
Note; If you can explain why the waste cannot exhibit one or
more of the four hazardous waste characteristics, you may
submit your rationale in lieu of test results for those char-
acteristics. For example, if the waste is composed exclusive-
ly of organic solvents and there is no chance (on the basis of
process considerations) that it contains any of the EP toxi-
cants, you need not test for the EP Toxicity characteristic.
You may omit the rest of this section and go to Part E.
2. If you have opted for Approach 3 in Section B above, then you
must perform the tests specified in the above paragraph, and
you should test for all hazardous constituents that may "rea-
sonably be expected" to be in the waste, whether or not they
were used as a basis for listing.
The remainder of this section is to be used to support your
decision regarding which constituents to test for.
A-14
-------
List the constituents (from Appendix VIII to Part 261)
that may reasonably be expected to be in the waste. De-
scribe the engineering, chemical, or other considerations
that support your choice.
Constituent:
Reasons for Selection:
(Repeat as necessary.)
For each of the remaining hazardous constituents (or
groups of constituents) in Appendix VIII of Part 261,
specify why it may not reasonably be expected to occur in
the waste stream. Base your reasoning on process, engi-
neering, mass balance or other considerations as appro-
priate.
Constituent (or group of constituents):
Reasons for non-occurence:
(Repeat as necessary.)
A-15
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SECTION £: Sampling and Testing the Waste
The purpose of the data requested below is to demonstrate that
representative samples of the waste stream:
a. Do not exhibit any of the criteria (e.g., hazardous waste
characteristics or constituents) for which the waste was
listed, and
b. Do not exhibit any other criteria that could cause it to
be listed.
Additional information is also requested as a check on the test
results. Refer to the accompanying Guidance Manual for instruc-
tions on developing a sampling plan (Chapter 7), selecting proper
test methods, (Chapter 8) and presenting the test results (Chapter
9).
1. General Information
Name and address of the laboratory facility performing the
sampling [260.22(i)(1)]:
Name
Street
City State Zip _
Telephone: ( ) -
If sampling was done by in-house staff, check here:
For each individual person who (a) designed the sampling
plan or (b~)collected samples, please provide the follow-
ing information and attach a resume or other statement of
qualifications [260.22(i)(2)].
Name ;
Affiliation _^^
Title
(Repeat as necessary.)
A-16
-------
b. Name and address of the laboratory facility performing the
testing, if different from the sampling laboratory
[260.22(1)(1)]:
Name
Street
City State Zip
Telephone: ( ) -
If testing was done by in-house staff, check here:
For each individual person who (a) designed the testing
plan or (b) performed tests, please provide the following
information and attach a resume or other statement of
qualifications [260.22(i)(2)] .
Name
Affiliation
Title
(Repeat as necessary.)
A-17
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Describe the sampling strategy you followed to insure that
the samples were representative [260.22(i)(8)] . Please
address specifically:
the variation of the waste stream over time; and
the variation of the waste stream in space.
All waste stream outflows or storage locations to which
this petition applies must be sampled. The Delisting
Petition Guidance Manual (see Instructions to this form)
gives .directions for developing a sampling plan.
d. State whether the Chain of Custody procedures in Section
1.3 of SV/-846 were followed. Please describe any devia-
tions from those procedures and the reasons for them.
A-18
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2. Sample-Specific Information
For each individual sample, please furnish the'information
requested in the form on the following page. The notes below
refer to those items on the form that are not self-explana-
tory. The Guidance Manual contains additional instructions.
Notes
Item f, "Parameter/Constituent Tested For": Enter the hazardous
waste characteristic or constituent that was the subject
of the test.
Item i, "Test Method and Source": See Chapter 3 of the Guidance
Manual for a listing of applicable test methods. Sources
for test methods may be designated by number, as follows:
1. "Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods," EPA SW-846 (second
edition), July, 1982, and supplements.
2. "Methods for the Evaluation of Water and
Wastewater," EPA _600 14-79-020, March, 1979.
3. "Standard Methods for the Examination of Water
and Wastewater," (14th Edition).
4. Appendix J of the Guidance Manual
Item j, "Sample Workup or Preparation Method": See Section Four
of Reference 1 above.
Item 1, "Test Results": Enter concentrations in mg/1, ppm, etc.
as appropriate.
A-19
-------
Sample Number:
Sampling Information;
a. Sampling location:
b. Person(s) who drew the sample:
c. Equipment used for drawing the sample:
a .m,
d. Date and time when the sample was drawn: / / , p.m.
e. Handling, containerization, and preservation techniques used:
Test Procedures and Results; (Repeat for each test conducted)
f. Parameter/Constituent Tested For:
g. Date Test Performed: / /
h. Person(s) who performed the test:
i. Test Method (or Number) and Source:
j. Sample Workup or Preparation Method:
k. Equipment: Name Model Number
1. Test Results:
A-20
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3. Summary Table of Analytical Results
For each sample, please enter the Test Results from Item 2
above onto the form contained in the following pages.
4. Analytical Discussion
Please furnish explanations or additional information on the
following topics as necessary:
a. Inconsistencies or deviations in the analytical results
presented above.
b. Additional reasons as to why the waste stream should be
delisted.
A-21
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SUMMARY OF TEST RESULTS
Ni
N>
Sample Number :
Sampling Location:
Date Sample Taken:
1 . ignitability
Liquids Flash point
Non- liquids Spontaneous
combustion
Compressed Flammability
Gas
Oxidizer Oxygen yield
2. Corrosivity pH
Corrosivity
towards steel
3. Reactivity Violent chemical
change
Reacts violently
with water
Water-reactive;
explosive
-
-------
SUMMARY OF TEST RESULTS (Continued)
to
LJ
Sample Number:
3. Reactivity Water-reactive;
(Cont.) toxic gases,
vapors , fumes
Cyanide or sulfur-
bearing wastes
which, when exposed
to acidic/basic
conditions, gen-
erate toxic gases,
vapors, or fumes
Explosive when
subjected to
force or heat
Explosive at stan-
dard temperature
and pressure
DOT explosive
4. Total Arsenic
Metals
(Complete Barium
Acid
Digestion) Cadmium
Chromium
-------
SUMMARY OF TEST RESULTS (Continued)
K>
Sample Number :
4. Total Lead
Metals
(cont.) Mercury
Selenium
Silver
Nickel
5. EP Toxicity Arsenic
— Metals
Barium
Cadmium
Chromium
Lead
Mercury
Selenium
Silver
Nickel
-------
SUMMARY OF TEST RESULTS (Continued)
>
NJ
Sample Number:
6. EP Toxicity Arsenic
— Metals;
Oily Waste Barium
Methods*
Cadmium
Chromium
Lead
Mercury
Selenium
Silver
»
Nickel
7. EP Toxicity Endrin
— Pesticides
Lindane
Methoxychlor
Toxaphene
8. EP Toxicity 2,4-D
— Herbicides
2,4,5-TP (Silvex)
*For wastes containing greater than 1% total oil and grease.
-------
SUMMARY OF TEST RESULTS (Continued)
to
Sample Number:
9. EP Toxic ity
— Organics
10. Total Organ-
ic Carbon
11. Oil and
Grease
1 2 . Cyanide Total
Free
Extraction
procedure
Photodegradable
13. Other Appendix VIII
cons ti tuents
(Add sheets as
necessary)
-------
5. Quality Assurance and Quality Control
a. For inorganic substances, describe the procedures used for
Standard Additions Analysis. Provide the following for
each substance tested:
Spike Recovery Percent
Substance Concentration Concentration Recovery
For organic substances, describe the procedures used for
analysis of spiked samples. For each substance tested,
provide the information requested in the following table.
Also, describe in writing the procedures used to cali-
brate the analytical equipment.
Substance Surrogate, Spike Recovery Percent
Tested For if any Cone. Cone. Recovery
Describe any other QA/QC measures followed in regard to
the sampling and analysis procedures.
A-27
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APPENDIX B
HAZARDOUS WASTE DELISTING REGULATIONS (40 CFR 260 Subpart C)
The regulations in this Appendix are current
as of April 1985. Therefore, they do not
reflect forthcoming changes in the delisting
procedures to be issued in accordance with the
Hazardous and Solid Waste Amendments of 1984.
-------
Subpart C—Rulamaking Petition!
§260.20 General.
(a) Any person may petition the Ad-
ministrator to modify or revoke any
provision in Parts 260 through 265 of
this chapter. This section sets forth
general requirements which apply to
all such petitions. Section 260.21 sets
forth additional requirements for peti-
tions to add a testing or analytical
method to Pan 261, 264 or 265. Sec-
tion 260.22 sets forth additional re-
quirements for petitions to exclude a
waste at a particular facility from
S 261.3 of this chapter or the lists ol
hazardous wastes in Subpart D of Part
261.
(b) Each petition must be submitted
to the Administrator by certified mail
and must include:
(1) The petitioner's name and ad-
dress;
(2) A statement of the petitioner's
interest in the proposed action;
(3) A description of the proposed
action, including (where appropriate)
suggested regulatory language; and
(4) A statement of the need and jus-
tification for the proposed action, in-
cluding any supporting tests, studies,
or other information.
B-3
-------
Chapter I—Environmental Protection Agency
1260.22
(c) The Administrator will make a
tentative decision to grant or deny a
petition and will publish notice of
such tentative decision, either in the
form of an advanced notice of pro-
posed rulemaking, a proposed rule, or
a tentative determination to deny the
petition, in the FEDERAL REGISTER for
written public comment.
(d) Upon the written request of any
interested person, the Administrator
may, at his discretion, hold an infor-
mal public hearing to consider oral
comments on the tentative decision. A
person requesting a hearing must state
the issues to be raised and explain
why written comments would not suf-
fice to communicate the person's
views. The Administrator may in any
case decide on his own motion to hold
an informal public hearing.
(e) After evaluating all public com-
ments the Administrator will make a
final decision by publishing in the
FEDERAL REGISTER a regulatory amend-
ment or a denial of the petition.
§ 260.21 Petitions for equivalent testing or
analytical method*.
(a) Any person seeking to add a test-
ing or analytical method to Part 261,
264, or 265 of this chapter may peti-
tion for a regulatory amendment
under this section and J 260.20. To be
successful, the person must demon-
strate to the satisfaction of the Ad-
ministrator that the proposed method
is equal to or superior to the corre-
sponding method prescribed in Part
261. 264. or 265 of this chapter, in
terms of its sensitivity, accuracy, and
precision (i.e., reproducibility).
(b) Each petition must include, in
addition to the information required
by § 260.20(b):
(DA full description of the proposed
method, including all procedural steps
and equipment used in the method;
(2) A description of the types of
wastes or waste matrices for which the
proposed method may be used;
(3) Comparative results obtained
from using the proposed method with
those obtained from using the rele-
vant or corresponding methods pre-
scribed in Part 261. 264. or 265 of this
chapter;
(4) An assessment of any factors
which may interfere with, or limit the
use of, the proposed method; and
(5) A description of the quality con-
trol procedures necessary to ensure
the sensitivity, accuracy and precision
of the proposed method.
(c) After receiving a petition for an
equivalent method, the Administrator
may request any additional informa-
tion on the proposed method which he
may reasonably require to evaluate
the method.
(d) If the Administrator amends the
regulations to permit use of a new
testing method, the method will be in-
corporated In "Test Methods for the
Evaluation of Solid Waste: Physical/
Chemical Methods," SW-846. U.S. En-
vironmental Protection Agency, Office
of Solid Waste, Washington, D.C.
20460.
[Comment This manual will be provided to
any person on request, and will be available
for inspection or copying at EPA headquar-
ters or any EPA Regional Office.]
§260.22 Petitions to amend Part 261 to
exclude a waste produced at a particu-
lar facility.
(a) Any person seeking to exclude a
waste at a particular generating facili-
ty from the lists in Subpart D of Part
261 may petition for a regulatory
amendment under this section and.
! 260.20. To be successful, the petition-
er must demonstrate to the satisfac-
tion of the Administrator that the
waste produced by a particular gener-
ating facility does not meet any of the
criteria under which the waste was
listed as a hazardous waste and, in the
case of an acutely hazardous waste
listed under § 261.11(a)(2). that it also
does not meet the criterion of
§ 261.11(a)(3). A waste which is so ex-
cluded may still, however, be a hazard-
ous waste by operation of Subpart C
of Part 261.
(b) The procedures in this section
and g260.20 may also be used to peti-
tion the Administrator for a regulato-
ry amendment to exclude from
§ 261.3(a)(2)(ii) or (c), a waste which is
described in those sections and is
either a waste listed in Subpart D,
contains a waste listed in Subpart D,
or is derived from a waste listed in
B-4
-------
§ 260.22
Title 40—Protection of Environment
Subpart D. This exclusion may only be
issued for a particular generating,
storage, treatment, or disposal facility.
The petitioner must make the same
demonstration as required by para-
graph (a) of this section, except that
where the waste is a mixture of solid
waste and one or more listed hazard-
ous wastes or is derived from one or
more hazardous wastes, his demon-
stration may be made with respect to
each constituent listed waste or the
waste mixture as a whole. A waste
which is so excluded may still be a
hazardous waste by operation of Sub-
part C of Part 261.
(c) If the waste is listed with codes
"I", "C", "R", or "E" in Subpart D,
the petitioner must show that demon-
stration samples of the waste do not
exhibit the relevant characteristic de-
fined in §261.21, § 261.22, § 261.23, or
5 261.24 using any applicable test
methods prescribed therein.
(d) If the waste is listed with code
"T" in Subpart D, the petitioner must
demonstrate that:
(1) Demonstration samples of the
waste do not contain the constituent
(as defined in Appendix VII) that
caused the Administrator to list the
waste, using the appropriate test
methods prescribed In Appendix III;
or
(2) The waste does not meet the cri-
terion of 5 261.11(a)(3) when consider-
ing the factors in § 261.11(a)(3) (i)
through (xi).
(e) If the waste is listed with the
code "H" in Subpart D, the petitioner
must demonstrate that the waste does
not meet both of the following crite-
ria:
(1) The criterion of § 261.11(a)(2).
(2) The criterion of § 261.11
-------
quest any additional information
which he may reasonably require to
evaluate the petition.
-------
APPENDIX C
STATE HAZARDOUS WASTE AGENCIES
AND DELISTING CONTACTS
-------
STATE HAZARDOUS WASTE AGENCIES
AND DELISTING CONTACTS
(Telephone numbers for delisting contacts are the same
as for the agency, unless otherwise shown.)
Alabama
Alabama Dept. of Environmental
Management
Solid S Hazardous Waste
Management Division
State Capitol
Montgomery,- Alabama 36130
(205) 832-6728
Delisting Contact:
Bill Gallagher, (404) 881-3016
Alaska
Department of Environmental Conservation
Air & Solid waste Management
Pouch 0
Juneau, Alaska 99811
(907) 465-2635
Delisting Contact:
Dave Ditraglia, (907) 465-2666
American Samoa
Environmental Quality Commission
American Samoa Government
Pago Pago, American Samoa 96799
Overseas Operator 633-4116
Delisting Contact:
Lucy Mlenar (EPA Region IX)
(415) 974-7472
California
Department of Health Services
Toxic Substances Control Division
714 P Street
Sacramento, California 95814
(916) 324-1789
Delisting Contact:
Stan Lau, (916) 324-1807
Colorado
Colorado Department of Health
Waste Management Division
4210 E. 11th Avenue
Denver, Colorado 80220
(303) 320-8333
Delisting Contact:
Ken Waesche
Commonwealth of North Mariana Islands
Department of Public Health and
Environmental Services
Division of Environmental Quality
Commonwealth of the North Mariana Islands
Saipan, Mariana Islands 96950
Overseas Operator: 6984
Delisting Contact:
Lucy Mlenar (EPA Region IX)
(415) 974-7472
Arizona
Bureau of Waste Control
Department of Health Services
State Health Building
1740 West Adams Street
Phoenix, Arizona 85007
(602) 255-1170
Delisting Contact:
Sally Mates, (602) 255-1160
Connecticut
Department of Environmental Protection
Hazardous Materials Management Unit
State Office Building
165 Capitol Avenue
Hartford, Connecticut 06115
(203) 549-4924
Delisting Contact:
Barry Giroux, (203) 566-4869
Arkansas
Department of Pollution Control
and Ecology
Solid Waste Management Division
PO Box 9533
8001 National Drive
Little Rock, Arkansas 72219
(501) 562-7444
Delisting Contact:
Jay Justice, x274
Delaware
Department of Natural Resources
and Environmental Control
Solid Waste Management Branch
89 King Highway
PO Box 1401
Dover, Delaware 19901
(302) 736-4781
Delisting Contact:
Alan Simpson
C-3
-------
District of Columbia
Department of Environmental
Services
Division of Pesticides
and Hazardous Materials
5000 Overlook Avenue, S.W.
Washington, D.C. 20032
(202) 767-8422
Delisting Contact:
Angelo Tompros
Florida
Department of Environmental Regulations
Solid Waste Section
Twin Towers Office Building
2600 Blair Stone Road
Tallahassee, Florida 32301
(904) 488-0300
Delisting Contact:
Craig Dieltz
Department of Natural Resources
Environmental Protection Division
270 Washington Street, S.W.
Atlanta, Georgia 30334
(404) 656-2833
Delisting Contact:
Shirley Maxwell
Guam
Environmental Protection Agency'
Government of Guam
PO Box 2999
Agana, Guam 96910
Overseas Operator 646-3863
«
Delisting Contact:
Jim Canto
Hawaii
Department of Health
Environmental Health Division
PO Box 3378
Honolulu, Hawaii 96801
(808) 548-4139
Delisting Contact:
Lucy Mlenar (EPA Region IX)
(415) 974-7472
Idaho
Department of Health and Welfare
Hazardous Materials Bureau
State House
Boise, Idaho 83720
(208) 334-4064
Delisting Contact:
Daryl Koch, (208) 384-4118
Illinois
Environmental Protection Agency
Division of Land Pollution Control
2200 Churchill Road
Springfield, Illinois 62706
(217) 782-0246
Delisting Contact:
Gary King, (217) 782-5544
Indiana
State Board of Health
Land Pollution Control Division
1330 West Michigan Street
Indianapolis, Indiana 46206
(317) 633-0194
Delisting Contact:
Gwyn Doyle, (317) 243-5021
Iowa
Department of Environmental Quality
Hazardous Waste Program
Henry A. Wallace Building
9OO East Grand street
Des Moines, Iowa 50319
(515) 281-8853
Delisting Contact:
Ron Kolpa, (515) 281-8925
Kansas
Department of Health and Environment
Bureau of Environmental Sanitation
Forbes Field, Building 321
Topeka, Kansas 66620
(913) 862-9360
Delisting Contact:
John Mitchell
C-4
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Kentucky
Michigan
Department of Natural Resources
and Environmental Protection
Division of Waste Management
18 Reilly Road
Frankfort, Kentucky 40601
(502) 564-6716
Department of Natural Resources
Environmental Services Division
Office of Hazardous Waste Management
Box 30028
Lansing, Michigan 48909
(517) 373-2730
Delisting Contact:
George Gilbert
Delisting Contact:
Al Howard
Louisiana
Minnesota
Department of Natural Resources
Solid Waste Management Division
PO Box 44066
Baton Rouge, Louisiana 70804
(504) 342-1216
Pollution Control Agency
Solid and Hazardous Waste Division
1935 West County Road, R-2
Roseville, Minnesota 55113
(612) 296-7333
Delisting Contact:
Bill Greenwich, (504) 342-1227
Delisting Contact:
Gordon Myer, (612) 296-7784
Maine
Department of Environmental Protection
Bureau of Oil and Hazardous Materials
State House - Station 17
Augusta, Maine 04333
(207) 289-2651
Delisting Contact:
Dave Boulter, (207)
289-2651
Mississippi
Department of Natural Resources
Division of Solid & Hazardous
Waste Management
PO Box 10385
Jackson, Mississippi 39209
(601) 961-5171
Delisting Contact:
David Lee, (601) 961-5046
Maryland
Department of Health and Mental Hygiene
Waste Management Administration
201 Hast Preston Street
Baltimore, Maryland 21201
(301) 383-5740
Delisting Contact:
Alvin Bowles, (301) 383-5736
Massachusetts
Department of Environmental
Quality Engineering
Division of Hazardous waste
One Winter Street
Boston, Massachusetts 02108
(617) 292-5589
Delisting Contact:
Steve Dreeszen, (617) 292-5832
Missouri
Department of Natural Resources
Solid Haste Management Program
PO BOX 1368
Jefferson City, Missouri 65102
(314) 751-3241
Delisting Contact:
Stan Jorgenaon
Montana
Department of Health and
Environmental Services
Solid Haste Management Bureau
Cogswell Building
Helena, Montana 59602
(406) 444-2821
Delisting Contact:
Roger Thorvilson
C-5
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Nebraska
New York
Department of Environmental Control
Water and Haste Management Division
PO Sox 94877
Lincoln, Nebraska 63509
(402) 471-2186
Delisting Contact:
Mike Steffensmeier
Nevada
Department of Conservation and
Natural Resources
Waste Management. Program
Capitol Complex
Carson City, Nevada 89701
(702) 885-4670
Delisting Contact:
Verne Rosse
New Hampshire
Department of Health and Welfare
Office of Waste Management
Health & welfare Building
Hazen Drive
Concord, New Hampshire 03301
(603) 271-4608
Delisting Contact:
Len Poole, (603) 271-4611
New Jersey
Department of Environmental protection
Solid Waste Administration
32 E. Hanover Street
Trenton, New Jersey 08625
(609) 292-9877
Delisting Contact:
Sonya Shashova, (609) 292-8341
New Mexico
New Mexico Health and Environment
Department
Environmental Improvement Division
PO BOX 968
Santa Fe, New Mexico 87504
(505) 984-0020
Delisting Contacts:
Peter Pache, (SOS) 984-0020, X340
Trent Thomas, (505) 827-5271
Department of Environmental
Conservation
Division of Solid Waste
50 Wolf Road
Albany, New York 12233
(518) 457-6603
Delisting Contact:
Jim Moran, (518) 457-6858
North Carolina
Department of Human Services
Environmental Health Section
Solid s Hazardous Waste
Management Branch
PO Box 2091
Raleigh, North Carolina 27602
(919) 733-2178
Delisting Contact:
Jerry Rhodes, (919) 733-2178
North Dakota
Department of Health
Division of Environmental
Waste Management & Research
1200 Missouri Avenue
Bisnark, North Dakota 58505
(701) 224-2366
Delisting Contact:
Neil Knatterud, (701) 224-2366
Ohio
Ohio Environmental Protection Agency
Office of Land Pollution Control
9O Box 1049
Columbus, Ohio 43216
(614) 466-8934
Delisting Contact:
Tom Carlisle, (614) 462-6735
Oklahoma
Oklahoma State Department of Health
Industrial s solid waste Service
1000 HE 10th Street
Oklahoma City, Oklahoma <73152
(405) 271-5338
Delisting Contact:
Donald A. Hensch,
(405) 271-5338
C-6
-------
South Dakota
Department of Environmental Quality
Solid Waste Management Division
PO Box 1760
522 S.W. Fifth Avenue
Portland, Oregon 97207
(503) 229-5913
Delisting Contact:
Rich Reiter, (503) 229-6434
Pennsylvania,
Department of Environmental Resources
Bureau of Solid Waata Management
Fulton Building
PO Box 2063
Harrisburg, Pennsylvania 17120
(717) 787-9870
Delisting Contact:
David Freedman, (215) 637-7381
Department of Water & Natural Resources
Office of Air Quality & Solid Waste
Joe Foss Building
Pierre, South Dakota 57501
(605) 773-3329
Delisting Contact:
Kevin Tviadt
Tennessee
Department of Public Health
Bureau of Environmental Services
Division of Solid waste Management
150 9th Avenue, North
Nashville, Tennessee 37203
(615) 741-3424
Delisting Contact:
Shirley Dunn
Puerto Rico
Environmental Quality Board
Solid, Toxics, S Hazardous Waste Program
Box 11488
Santurce, Puerto Rico 00910-1488
(809) 725-8992
Delisting Contact:
Yacnan Lopez
Rhode Island
Department of Environmental Management
Solid Haste Management Program
Cannon Building
75 Davis Street
Providence, Rhode Island 02908
(401) 277-2797
Delisting Contact:
Steve Majkut
South Carolina
South Carolina Department of
Health £ Environmental Control
Bureau of Solid 4 Hazardous Waste
Management
J. Marion Siam* Building
2600 Bull Street
Columbia, South Carolina 29201
(803) 758-5681
Texas
Texas Department of Health
Bureau of Solid Waste Management
1100 west 49th Street, T-602
Austin, Texas 78756
(512) 458-7271
Delisting Contact:
Dick Martin (TDWR), (512) 475-2041
Utah
Bureau of Solid s Hazardous Waste
Waste Management Division
PO Box 2500
ISO West North Temple
Salt Lake City, Utah 34110
(301) 533-4145
Delisting Contact:
Kent Gray
Vermont
Agency of Environmental Conservation
Air £ Solid waste Programs
State Office Building
Montpeliar, Vermont 05602
(802) 328-3395
Delisting Contact:
John Miller
Delisting Contacts:
Lynn Martin, Rick Grant
C-7
-------
Virgin Islands
Department of Conservation and
Cultural Affairs
Division of Natural Resources
Hazardous Waste Program
PO Box 4340, Charlotte Amalie
St. Thomas, Virgin Islands 00801
(809) 774-6420
Delisting Contact:
Roger Van Eepoel
Virginia
Virginia Department of Health
Division of Solid and Hazardous
Haste Management
Madison Building
109 Governor Street
Richmond, Virginia 23219
(304) 786-5271
West Virginia
Department of Natural Resources
1201 Greenbrier Street
East Charleston, West Virginia 25311
(304) 348-5935
Deliating Contact:
Robert Jelacic
Wisconsin
Department of Natural Resources
Bureau of Solid Waste Management
PO Box 7921
Madison, Wisconsin 53707
(608) 266-1327
Delisting Contact:
Richard O'Hara, (608) 266-0833
Delisting Contact:
Walt Gulovich, (804) 225-2667
Washington
Department of Ecology
Solid waste Management Division
Olympia, Washington 98504
(206) 459-6317
Delisting Contact:
Tom Cook, (206) 459-6301
State of Wyoming Department of Environ-
mental Quality
Solid waste Management Program
Equality State Bank Building
401 West 19th Street
Cheyenne, Wyoming 32002
(307) 777-7752
Delisting Contact:
Dave Finley
C-8
-------
APPENDIX D
HAZARDOUS WASTE CHARACTERISTICS (40 CFR 261 Subpart C)
The content of this Appendix was reproduced
from the Code of Federal Regulations of July
1, 1984. Users should check the current ver-
sion of the Code of Federal Regulations and
more recent issues of the Fe3era^T~Register for
amendments.
-------
Subpart C—Characteristics of
Hazardous Wast*
3 281.20 General.
(a) A solid waste, as defined in
9 261.2. which is not excluded from
regulation as a hazardous waste under
§ 261.4(b), is a hazardous waste if it ex-
hibits any of the characteristics identi-
fied in this Subpart.
[Comment: 5 2S2.11 of this chapter sets
forth the generator's responsibility to deter-
mine whether his waste exhibits one or
more of the characteristics Identified In this
Subpart] .
(b) A hazardous waste which is iden-
tified by a characteristic in this sub-
part, but is not listed as a hazardous
D-3
-------
§ 261.21
Till* 40—Protection of Environment
waste in Subpart O, is assigned the
EPA Hazardous Waste Number set
forth in the respective characteristic
in this Subpart. This number must be
used in complying with the notifica-
tion requirements of Section 3010 of
the Act and certain recordkeeping and
reporting requirements under Parts
262 through 265 and Part 270 of this
chapter.
(c) For purposes of this Subpart, the
Administrator will consider a sample
obtained using any of the applicable
sampling methods specified in Appen-
dix I to be a representative sample
within the meaning of Part 260 of this
chapter.
[Comment Since the Appendix I sampling
methods are not being formally adopted by
the Administrator, a person who desires to
employ an alternative sampling method is
not required to demonstrate the equivalency
of his method under the procedures set
forth in Si 280.20 and 260.21.]
(45 PR 33119. May 19. 1980. a» amended at
48 PR 14294. Apr. 1. 19831
9 261.21 CharmctcriaUe of ignitability.
(a) A solid waste exhibits the charac-
teristic of ignitability if a representa-
tive sample of the waste has any of
the following properties:
(1) It is a liquid, other than an aque-
ous solution containing less than 24
percent alcohol by volume and has
flash point less than 60*C (140'P). as
determined by a Pensky-Martens
Closed Cup Tester, using -the test
method specified in ASTM Standard
D-93-79 or D-93-80 (incorporated by
reference, see 5 260.11). or a Setaflash
Closed Cup Tester, using the test
method specified in ASTM Standard
D-3278-78 (incorporated by reference,
see i 260.11), or as determined by an
equivalent test method approved by
the Administrator under procedures
set forth in 35 260.20 and 260.21.
(2) It is not a liquid and is capable,
under standard temperature and pres-
sure, of causing fire through friction.
absorption of moisture or spontaneous
chemical changes and. when ignited.
burns so vigorously and persistently
that is creates a hazard.
(3) It is an ignitable compressed gas
as defined in 49 CPR 173.300 and as
determined by the test methods de-
scribed in that regulation or equiva-
lent test methods approved by the Ad-
ministrator under § § 260.20 and 260.21.
(4) It is an oxidizer as defined in 49
CFR 173.151.
(b) A solid waste that exhibits the
characteristic of ignitability, but is not
listed as a hazardous waste in Subpart
D, has the EPA Hazardous Waste
Number of D001.
[45 PR 33119. May 19, 1980, a* amended at
46 PR 35247. July 7. 1981]
9 261.22 Characteristic of corrosivity.
(a) A solid waste exhibits the charac-
teristic of corrosivity if a representa-
tive sample of the waste has either of
the following properties:
(1) It is aqueous and has a pH less
than or equal to 2 or greater than or
equal to 12.5. as determined by a pH
meter using either an EPA test
method or an equivalent test method
approved by the Administrator under
the procedures set forth in §§ 260.20
and 260.21. The EPA test method for
pH is specified as Method 5.2 in "Test
Methods for the Evaluation of Solid
Waste, Physical/Chemical Methods"
(incorporated by reference, see
J 260.11).
(2) It is a liquid and corrodes steel
(SAE 1020) at a rate greater than 6.35
mm (0.250 inch) per year at a test tem-
perature of 55'C (130'P) as determined
by the test method specified in NACE
(National Association of Corrosion En-
gineers) Standard TM-01-69 as stand-
ardized in "Test Methods for the Eval-
uation of Solid Waste. Physical/
Chemical Methods" (incorporated by
reference, see § 260.11) or an equiva-
lent test method approved by the Ad-
ministrator under the procedures set
forth in §5 260.20 and 260.21.
(b) A solid waste that exhibits the
characteristic of corrosivity, but is not
listed as a hazardous waste in Subpart
D, has the EPA Hazardous Waste
Number of O002.
[45 FR 33119, May 19. 1980. as amended at
46 PR 35247, July 7, 1981]
9 261.23 Characteristic of reactivity.
(a) A solid waste exhibits the charac-
teristic of reactivity if a representative
sample of the waste has any of the fol-
lowing properties:
D-4
-------
Chapter I—Environmental Protection Agency
§261.30
(1) It is normally unstable and read-
ily undergoes violent change without
detonating.
(2) It reacts violently with water.
(3) It forms potentially explosive
mixtures with water.
(4) When mixed with water, it gener-
ates toxic gases, vapors or fumes in a
quantity sufficient to present a danger
to human health or the environment.
(5) It is a cyanide or sulfide bearing
waste which, when exposed to pH con-
ditions between 2 and 12.5, can gener-
ate toxic gases, vapors or fumes in a
quantity sufficient to present a danger
to human health or the environment.
(6) It is capable of detonation or ex-
plosive reaction if it is subjected to a
strong initiating source or if heated
under confinement.
(7) It is readily capable of detona-
tion or explosive decomposition or re-
action at standard temperature and
pressure.
(8) It is a forbidden explosive as de-
fined in 49 CFR 173.51. or a Class A
explosive as defined in 49 CFR 173.53
or a Class B explosive as defined in 49
CPR 173.88.
(b) A solid waste that exhibits the
characteristic of reactivity, but is not
listed as a hazardous waste in Subpart
D. has the EPA Hazardous Waste
Number of O003.
9 261.24 Characteristic of EP toxicity.
(a) A solid waste exhibits the charac-
teristic of EP toxicity if, using the test
methods described in Appendix II or
equivalent methods approved by the
Administrator under the procedures
set forth in 55 260.20 and 260.21. the
extract from a representative sample
of the waste contains any of the con-
taminants listed in Table I at a con-
centration equal to or greater than the
respective value given in that Table.
Where the waste contains less than 0.5
percent filterable solids, the waste
Itself, after filtering, is considered to
be the extract for the purposes of this
section.
(b) A solid waste that exhibits the
characteristic of EP toxicity. but is not
listed as a hazardous waste in Subpart
O, has the EPA Hazardous Waste
Number specified in Table I which cor-
responds to the toxic contaminant
causing it to be hazardous.
TABLE I—MAXIMUM CONCENTRATION OF CON-
TAMINANTS FOR CHARACTERISTIC OF EP
TOXICITY
EPA
nazarooua
wuia
numMr
0004
0005
0008
0007
0008
0009
0010
0011
0012
0013
0014
0015
0016
0017
Contaminant
Araanic ...
Swum
Cadmium
Cnromum
Laad
Mwcury
SaMnum . .. .
Si(v«r . . ...
EnOnn (1.2.3,4.10,10-hKiicn.
ion>l.7-apo»y-
i .4,4a.5.6.7.8.8a-aciaflydro-
i ,4-
-------
APPENDIX E
LISTS OF HAZARDOUS WASTES (40 CFR 261 Subpart D)
The content of this Appendix was reproduced
from the Code of Federal Regulations of July
1, 1984. Users should check the current ver-
sion of the Code of Federal Regulations and
more recent issues of the Federal Register for
amendments.
-------
Subpart 0—Lists of Hazardous
Wastes
§ 261.30 General.
(a) A solid waste is a hazardous
waste if it is listed in this subpart,
unless it has been excluded from this
list under !§ 260.20 and 260.22.
(b) The Administrator will indicate
his basis for listing the classes or types
of wastes listed in this Subpart by em-
ploying one or more of the following
Hazard Codes:
(I)
COT09M W«M (Q
RMCM WMW (R)
EPTonqWaiw (&
Acun Hfivaaut w«w. . .... (H)
Tone WMM (T)
Appendix VII identifies the constitu-
ent which caused the Administrator to
list the waste as an EP Toxic Waste
(E) or Toxic Waste (T) in {$261.31
and 261.32.
(c) Each hazardous waste listed in
this subpart is assigned an EPA Haz-
E-3
-------
§ 261.31
Title 40—Protection of Environment
ardous Waste Number which precedes
the name of the waste. This number
must be used in complying with the
notification requirements of Section
3010 of the Act and certain record-
keeping and reporting requirements
under Parts 262 through 265 and Part
270 of this chapter.
(d) The following hazardous wastes
listed in § 261.31 or § 261.32 are subject
to the exclusion limits for acutely haz-
ardous wastes established in § 261.5:
[Reserved]
[45 FR 33119. May 19. 1980. as amended at
45 FR 74892. Nov. 12. 1980: 48 FR 14294.
Apr. 1. 1983]
9 261.31 Hazardous wattes from non-specific sources.
mduMry and EPA hazardous)
Generic
F001
F002
F003
FOO4
FOOS
FOOS
F019
FOOT
FOOS..
Fono>
F010
PQ11
F01Z_
F024.... _
Hazardoua wane
tncNoroemylene, memytens chloride. 1,1,1-lncnioroethane. caroon tetracltionda.
and cnkxinaiad fluorocarbons. and sludge* from the recovery of mese solvents m
degreaamg operations.
The louowmg spent halogenated solvents. latracntoroetnyMne methyiene chloride
incnioroetnvlena. t.i.i-incnuxoetnane. ctuorobenzene. 1.t.2-tnchloro-1.2.2-tnfluor-
oemane, orfftodicMorooenzene. and tnchlorofkjoromemane; and the sou bottoms
from me recovery ol these solvents.
Benzene. »myl ether, metnyl isoDulyl kalone. n-outyl alcohol, cydohexanone. and
memanot and the sun bonoms from ihe recovery at mese solvents.
nitrobenzene: and the still bonoms from the recovery at these solvents.
solvents.
loHowng processes: (1) suttunc aod anodomg ol Hummunr (2) tn plating on
carbon suet (3) one plating (segregated Oaaisl on carbon steel: (4) akjmmum or
anc-akimnum platng on caroon siaeh (5) cleaning/ skipping asaoaaMd witti bn.
aluminum.
wnere cyanides are used m me process (eicept lor preoous metals eMctropMlng
pMang bam skidgesl.
stripping and cleaning bam solutions).
cyandea are used n the process (except tor precious mataia heeltfeeeng
quenenjng bam sludges).
operations (except tor precious metals fteat treeing spent cyanide solutions from
sad bath pot cleaning).
cyarades are used m me process (except lor preoous metal* heat treating
rMCtor ctMfroui wawtM from the production ol cnkmnateW attpnatic hydrocar*
bons, hemng cartton conrtnt from ona to fiv*. uotemg fr*M radical catalyzad
procaaiai. [This Imtmg do»M not inchxJ* Itgm ends, soatit ftttart and ftltar aida.
wa«aa(mad«$26l.3Z]
Hazard
coda
CO
(I Tl
(Q T\
(R T)
(R T)
[48 FR 4617. Jan. 16. 1981. as amended at 46 FR 27477. May 20, 1981; 49 FR 5312. Feb. 10,
1984]
EJTECTIVS DATS NOTE: At 49 FR 5312, Feb. 10. 1984. the waste stream Identified by EPA
hazardous waste no. P024 was added to the table In 5 261.31. eHecttve August 10, 1984.
E-4
-------
Chapter I—Environmental Protection Agency
§261.32
S 261.32 Hazardous wastes from specific sources.
industry and EPA hazardous
waste No.
Hazardous waste
Hazard
code
Wood preservation. KOOI
Inorganic pigments:
K002
Bottom sediment sludge Irom the treatment ol wasiewaters trom wood preserving
processes mat use creosote and/ or pentaehforopnenol.
Wastewsier treatment sludge
the production of chrome yellow and orange
(T)
m
K003 Wastewater treatment sludge from the production of motybdate orange pigment* (T)
KOXM Wastewaler treatment sludge from the production of zinc yellow pigments (T)
KOOS Wastewaler treatment sludge from the production of chrome green pigment* . . . (T)
KOM Wastewaler treatment sludge from me production ol chrome oxide green pigments (T)
(anhydrous and hydralad)
K007 Wastawater treatment sludge from the production of iron blue pigments (T)
KOOS Oven residue from me production of chrome and* green pigments (T)
Organic cnemcalK
KOM OtsliUalion bottoms from me production of acelaldenyde from elhyiene . ... (T)
K010 OistHlation side cuts from the production of acetaldenyae from einylene. .CO
KO11 Bottom stream from the wastewater stnpper n me production of acrylonilnta. j (H. '
K013 Bottom stream trom the aceioramie column in the production ol acryiontnle ! (R. T)
K014 Bottoms Irom me acatomtnle punficauon column in the production'of acryKxiunle. , (T)
KOIS Sod bottoms Irom the distillation ol benzyl cnionde .. . . . . | (T)
K016 Heavy ends or datdlation residues Irom the production ol carbon teiracfilonoe j (T)
KOI 7 Heavy ends HUH bottoms) Irom the purification column in the production of (T)
epicnioronydnn
K018 Heavy ends from me fractionation column m ethyl cnionde production (T)
K019 Heavy ends from the duttUanon of afhvtene dtttvonde m ediytene demand* (T)
Production.
K020 - Heevy ends from the Asouanon of vinyl cnionde m vmyl cnionde monomer (T)
production.
K021 Aqueous spent antimony catalyst waste Irom lluoromemanes production (T)
K022 Otsouaoon bottom tars from the production of phenol/acetone from cumene (T)
KOM ttsMlaBon bgm end* from the production of pmnakc anhydride from naphthalen* (T)
K024 ... emulation bottoms from me production ol pmnakc anhydride from naphthalene (T)
KOM - Distillation light ends from the production of pntnakc anhydride trom orthc-ryMne (T)
KOM — OmNakon bottom* from me production of phtnakc anhydride Irom onno-iyMne (T)
K02S OMkatnn bottoms trom me production of nitrobenzene by me nitration ol benzene... (T)
KOM Snipping sun tans trom me production of methy ethyl pyndxes (T)
K027 Centrifuge and dnaUalnn residue* from toluene dnocyenate production (R. T)
K02S Spent catalyst from the hydrochtonnator reactor « the production of 1.1.1-mentor- (T)
oethane.
KOM Waste trom the product steem sinpper m me production ol t.i.l-mcfiloroetnane (D
KOM— Otwutation bottoms from me production of 1.1.1-tnchtoroeinane (T)
KOM Heavy end* from the heavy end* column from the production of 1.1.1-tnchloroetn- (T)
K030.
KOS3..
K103..
K104..
KOM.
K105..
I percMofoemylene.
i front •VMetfw production
production ol tncMoroediylene
K071.
K073..
K10S.
K031
K032..
K033..
KQ34
K097
Process residuee trom amkne extraction from me production of antne —
Combined westewster stream* generated from rairooenzene/anien* production
Oeunation or trac»onat>on column bottom* from m* production of cntorooenzene*
Separated aqueous stream trom the reactor product washing step in me production
ol cMorooeraene*.
Brine purification mud* trom the mercury eel proceas n cnkmne producBon. where
ieperaiel» prepunfied bnne i* not used.
CMomatto: hydrocarbon waste from the purification step ol the diaphragm cell
pfOCVM UflMQ QTBpfMW •nOOJeM M cMOfUW pTOdUeileiHi.
Waeteweler Ireetmenl sludge from the mercury cell precise in cMame production.—
ay-product sun generated In the production ol MSMA and ocodykc sod
Wastewaler treatment sludge from m* production ol chtoraene.
and scruo water from me chkmmnon of
production of cfttoroane.
RNar soed* from the fWraoon of heieOiWrocvciopentaaene n the producton al
Vacuum stnpper atecnarge from the cNordane cnwonaior n the produoon ol
K03S...
K036
K037 .
K038...
Wsiiewsier treatment sludge* generated m the production of creoaote
Son bottom* from toluene reclamation dlstManon in me production of dauttoton.
Wastewaler treatment sludges from the production of Asuncion
Wasiewaler from the wesfung and stripping of phoral* production
(T)
(T)
m
(T)
(T)
(T)
m
m
(T)
m
m
(T)
E-5
-------
§261.33
Title 40—Protection of Environment
Industry and EPA nsramoim
•MM No
K039
K040 .
K041
KMS
K042
KIMS
Ci plenum.
K044
KO45
K044
K047
PMroMufli rafinmg:
K048
K048
K050
K051
KOS2
Iran and suat
K061
K082
Svcondafy l*adr
KOW
K100
Vciamavy pfiaffnscauttcals?
K084
K101
K102
Ink MnnuMaore KOM
CMung:
Koeo
KM7
Hazardous waste
pnoraia
production ol 2.4.5-T
2.6-acnkxopn*nol vnsu Irom tn» production ol 2.4-O
Pmft/r«d water from TNT operations
Tank bottoms (leaded) from me petroleum refining industry .. .
furnace*.
Spent pickle hquor from steel (trashing operations
Wast* leaching lobbon from acx) leaching of emission conttol dust/sludge from
secondary lead smelong.
CMOcata from arasnc or organo-anMnc compounds.
Oitttaaon tar rmduaa from aw dnudmon of antm-busd compounds n m*
pounds.
vetennary prtamiacauocais from arsenic or organo-arsanic compounds.
Solvent wasrtaa and s*xidg*n, caustic washes and sludge* or water washes and
sludge* from ctaanng tubs and equipment used m the formuiabon of mtt from
AmmonM MH time studge from coking operation*.
Decanter tank tar ikjdge from coking operations
Hazard
code
cn
rn
m
m
ia\
(T)
(C T)
(T)
(n
m
(T)
(T)
C46 FR 4618, Jan. 16,1981, u amended at 46 FR 27476-27477, May 20. 1981]
9261.33 Discarded commercial chemical
product!, off'tpeeification apeciea, con-
tminer residues, and ipill residue*
thereof.
The following materials or Items are
hazardous wastes if and when they are
discarded or intended to be discarded:
(a) Any commercial chemical prod-
uct, or manufacturing chemical inter-
mediate having the generic name
listed In paragraph (e) or (f) of this
section.
(b) Any off-specification commercial
chemical product or manufacturing
chemical intermediate which, if It met
specifications, would have the generic
name listed in paragraph (e) or (f) of
this section.
(c) Any container or inner liner re-
moved from a container that has been
used to hold any commercial chemical
product or manufacturing chemical in-
termediate having the generic names
listed in paragraph (e) of this section.
or any container or inner liner re-
moved from a container that has been
used to hold any off-specification
chemical product and manufacturing
chemical intermediate which. If it met
specifications, would have the generic
name listed In paragraph (e) of this
section, unless the container is empty
as defined in 5 261.7(b)<3) of this chap-
ter.
[Comment Unless the residue Is being bene-
ficially used or reused, or legitimately recy-
E-6
-------
Chapter I—Environmental Protection Agoncy
§261.33
cled or reclaimed: or being accumulated.
stored, transported or treated prior to such
use. re-use, recycling or reclamation. EPA
considers the residue to be intended for dis-
card, and thus a hazardous waste. An exam-
ple of a legitimate re-use of the residue
would be where the residue remains in the
container and the container is used to hold
the same commericat chemical product or
manufacturing chemical product or manu-
facturing chemical intermediate it previous-
ly held. An example of the discard of the
residue would be where the drum is sent to
a drum reconditioner who reconditions the
drum but discards the residue.]
(d) Any residue or contaminated soil.
water or other debris resulting from
the cleanup of a spill into or on any
land or water of any commercial
chemical product or manufacturing
chemical intermediate having the ge-
neric name listed in paragraph (e) or
(f) of this section, or any residue or
contaminated soil, water or other
debris resulting from the cleanup of a
spill, into or on any land or water, of
any off-specification chemical product
and manufacturing chemical interme-
diate which, if it met specifications,
would have the generic name listed in
paragraph (e) or (f) of this section.
[Comment The phrase "commercial chemi-
cal product or manufacturing chemical in-
termediate having the generic name listed
In ..." refers to a chemical substance
which Is manufactured or formulated for
commercial or manufacturing use which
consists of the commercially pure grade of
the chemical, any technical grades of the
chemical that are produced or marketed.
and all formulations in which the chemical
Is the sole active Ingredient. It does not
refer to a material, such as a manufacturing
process waste, that contains any of the sub-
stances listed in paragraphs (e) or (f).
Where a manufacturing process waste Is
deemed to be a hazardous waste because It
contains a substance listed in paragraphs (e)
or (f). such waste will be listed in either
U 261.31 or M1J3 or will be Identified as a
hazardous waste by the characteristics set
forth in Subpart C of this part.]
(e) The commercial chemical prod-
ucts, manufacturing chemical interme-
diates or off-specification commercial
chemical products or manufacturing
chemical intermediates referred to in
paragraphs (a) through (d) of this sec-
tion, are identified as acute hazardous
wastes (H) and are subject to be the
small quantity exclusion defined in
§ 261.5(e).
[Comment For the convenience of the regu-
lated community the primary hazardous
properties of these materials have been indi-
cated by the letters T (Toxicity), and R (Re-
activity). Absence of a letter indicates that
the compound only is listed for acute toxici-
ty.]
These wastes and their correspond-
ing EPA Hazardous Waste Numbers
are:
Hmzaroou*
WMMNO.
P023.....
POS7
P058
P066.
P001
P002
P003
P070
P004
POOS. .-
P00»
P007
P008
P009
P119
P010
P012
P011 _
P01 1
P012
POM
P054
P013
POZ4
P077
P04Z.
P014
P028
P01S
P016.
P017
P012
POZ1
P123
P022.
P02Z. _.
P023
P024
P026.
P029. „
POM.. „..
P031
P037
P03S
Subatanca
Acauudanyda. cntoro-
AcaunMa. 2-fluoro-
AcaumidK acid. N-l(m«nylc«f-
bamoylK»y]tnio-. mattiyl a*tar
3-(alpn»-Aceuxiy««nry(M-"y<»o«vcoum«nn
and sans, *nan prawM at concantrattora
graalar man 0.3%
l-Acaiyt-2-ttwuraa
Acrotem
AK»cart>
Aldnn
AMyt alcohol
Alumnum pflcapfuda
4-aAmmooyndma
Ammonium (xcrmla (R)
Arcane aod
Araanc (III) oada
Anarac (V) onda
Arsarac pantanda
Anna, dwny-
Annan*
aanzanamina. 4-cftom-
Banzanamna. 4-mtro-
1 2-SanzanadKH. 4-(1-flydroxy-2-
-------
§261.33
Title 40—Protection of Environment
Hazardous
waste No
P039. .
P041 .. . .
P040
P043
POM
P04S
P071
P082 .
P047
POM
P048
P020
P08S
P039.
P049. . . .
P109. . ..
POSO.
POM. .
POSt
P042
P046
P084
P101
POS4
P097
POS6
P057
POM
P06S
POSt
POS1
P037
POM
POM
POBO
P082.
POM. _.._.
P063.._. .
POM
P084
P007
P092,...~
POM.
POH..~
pna
P118.
POS9.
POM.
P087.
POM--
POM.
P071 ..
P07^
P073
P074
Suoslance
0.0-Oiatnyl S-(2-(einylthK»etnylJ phospnoro-
Oiinioaie
Omnyl-p-nitropnenyl phosphate
O.O-Oietnyl O-pyrazmyl pnospnorothioaia
Dusopropyl Huorophosphale
Oimetnoaie
3.3-Oimetnyl-1-(metny«hio»-2.Dutanone. O-
[(mettiylamno(carOonyl] oiirrw
O.O-Onwtnyt 0-p-nlropnenyt pnospnoro-
ihoate
Ornaihylnlrosarnine
4,6-OmKro-o-aesc4 aod salts
4.8-O«nirc-i.4:i.aHinda. endo-dnwm- «n-
onapntnelene
1,2,3 4 10 10-HexecMorc-l 4 4a.5.8 8a-
hexanyiin> 1 ,4-.S.a-endo,eiip.
HyofUHM, fiMtfiyi^
Hydrocyanic add
Hydrogen cyanide
leWcysnic i&A, nwthyl Mivf
Mercury, (aceuic-OKinenyl-
Mercury fuknrats) (R.T)
MMnane, o«yt»a(cnloro-
Memaneanol. tnc«on>
4.7.Memeno-1H»ndene. 1 ,4,5,e,7,8.8-neB-
tacntoro-a«.4,7.7a-la«anydro-
2'Memyl40ndin«
2-Metnylla)Ctonrtrtl«
Methyl paratnion
aipna-Napnmyfmiouree
Nickel carDonyl
Nickel cyenide
Hazardous
waste No.
P074
P073
P075 ....
P078..
P077 ..
P078
P076
P078
P081
P082
POSO
P087
P087
POM. .
P089 .. .
P034
PQ48
P047
P02Q
P009 .
P036 .. ..
P092.
P093
P094
P095
P096
P041
P089
P110
POM
P099
P070 „
*^'^*
poai
P017
P003
POOS
P102
P075
P103
P1Q4
P1QS
pi 06.
P107
P108
PQt8
P108
P11S
P10B
Su&sunce
NickeMM) cyanide
Nicket letracarconyl
Nwoiine and sails
Nitric oxide
p-Nitroanihne
Nilroqan dioxid*
Nitrog«n(ll) o»d«
Nnrog«n(IV) ond*
NMroglycanrw (HI
N-NiUOSodKiwmylamna
acnioro, cyckc sultit*
Osrraum ouM
OiiTHum telronda
7-OnaacycloC2.2.t lheptane-2.3-d>caiooxylic
acid
Paratnion
Phenol. 2-cycloneKyl-4,s-flV«tro-
Phanol, 2.4
eaur
(•ttyltniotmMliyt •««
Phoaolxiroihioa aad. 0 Q dutfuii O-OHHITO
pneoyl) ester
•SMI
>rwinylamnol-iullonyl)pnenylle*ter
PlumbairM, tetfaeihyt-
PotaaMum cyand*
Pousaium mm cyanide
Propanal. 2-m«nyt.2-(memyrtn>o»-. 0-
1 2,3>farepan*Mnot tnnrtraH*> (H)
2-Propanoiw, 1-Oromo-
2-Prapevul
2-Prop«vt-ol
2-Propyn-l-ol
Pyndrw, (3>-3-vnt>t.t»ny1)-l and
uttt
Sannounn
aiver cyanide
Sodumtzide
Sodwmcyarade
Slronoum suKtde
Sttyetirwin-lO^jrw. and satta
Stiycnndm-tO-on*. 2,3-dnwamy-
Strycnrww and salts
Sultwic acid. tn*ttum(l) salt
TetrMtnykMnnoyropnoaptwa)
E-8
-------
Chapter I—Environmental Protection Agency
§ 261.33
Hazardous
wana No.
P110 ..
P111 ...
P112
P062...
P113
P113.
P114
P11S.
P04S.
P049.
P014
P116.
P028
P072
P093
P123
P118
P119
P120
P120
PO01
P121 .
P122,
SuDatanca
TetrMtnyl lead
Tettaeinylpyropnaapnale
Tetrantromatnina (R)
Tatrapnoaononc aad, twuetnyi ester
Thattconde
Tha»um(NI| onde
Thnwaa. (2-cnkmpnanyl)-
Thnuraa. 1-napnmalenyl
Thouraa. pnanyt-
Toxapnane
Tnchtorofliethaneihnl
Vanaacaod. arnmonum salt
Vanadwm pentonde
VanaduiKV) and*
Wanann. often preaent at concentrations
9ieaia> man 03%
Zmccyarade
Zinc pnoapmde. wnen preaent at concentra-
tions greater man 10%
(f) The commercial chemical prod-
ucts, manufacturing chemical interme-
diates, or off-specification commercial
chemical products referred to in para-
graphs (a) through (d) of this section,
are identified as toxic wastes (T)
unless otherwise designated and are
subject to the small quantity exclusion
defined in § 261.5 (a) and (f).
[Comment; For the convenience of the regu-
lated community, the primary hazardous
properties of these materials have been indi-
cated by the letters T (Toxicity). R (Reac-
tivity). I (Ignitamlity) and C (Corrosivity).
Absence of a letter indicates that the com-
pound is only listed for toxicity.]
These wastes and their correspond-
ing EPA Hazardous Waste Numbers
are:
w«
U001
U034
U187
UOOS
U112
U144
UZ14
U002
U003
U248
U004
UOOS
AcaukMhyda (I)
AcataJdaflyda. cicnloro-
N44-e
mathyl-
Senzenanune. 4-cnloro-2-matriy|.
Banzanamna. 4.4'-matnyleneDia(2-cnioro-
Banzenannna. 2-matnyl-. nydrccnkxida
Banzenamna. 2-metHyl-5-nitro
Benzene (I.T)
Senzeneacetic aad. 4-cn4orc-«lqna-(4-cniorc-
pnenyll-alpna-nydroiy, alnyl auar
Benzene, chloro*
1 2-8eniBna<»cart)Oxvtic aad annydnde
1.2-aenzenaacartwxylic aad. [N»<2-«myt-
heiryl)] eMer
l,2-8enzenedicartx)«ylw aad. cnbucyl eater
t.2-8enzenedicaraoiylic aad. dwtriy! eater
< ,2-SenzenaOicarboiyiic aad, amwmyl ester
Seiuene. t.2-dicnlon>
Benzene. t.3-d>cnlorc-
Benzene, 1 ,4^]icftlorc-
Senzene. (dKruoromeinyl)-
8«nz*xw dHTMttiyH' T)
B«nzen«, hwtactiloro-
3eWiZ4W, htnuttvf&o* (I)
BWIZWM, hydroxy*
Benzene. (1-me«iyletnyl)- (1)
Benzene. pantacnldn>nilR>
Benzanaaullonyt ctuonda (C.R)
Benzene. 1 .2.4,S-letraentoro-
Banzane. (tncniOfOmemvl)-(C.H.T)
Benzene. 1.3,5-lnmtro- (R.T)
Bwindma
1,2 8«nnsomcazc*n.3-ona. 1.1-dioiida
BenzoC|.k]lluorana
Banzolajpyrena
3.4-Banzopyrane
p-Sanzoqunona
E-9
-------
§261.33
Title 40—Protection of Environment
Hazardous
Waste No
U023
U050 . .. .
U085
U021
U073
UOfll
U095
U024
U027
U028 .'...
U248 _
U22S
U030
U128
U172 ...
U03S .. . .
U031 .
U159 . .
U160 .
UOS3
U074
U031
U136 ....
U032 . ...
IJ3M
U178
U178..
U177
U219
U097
U21S
U1S«
U033
U211
0033
U034
uo35 :..
U038
U026
U037
U039
U041
U042
U044
U047
U048
J049
U032
UOSO
UOS1 ..._
UOS2
UOS2
UOS3
UOSS
uosa
UOS7
U130
U056
U240
UOS9
UOM
U081
U06Z
U133
U221
Substance
SenzoincniofKM (C.R.T)
1 .2-Benzprienantncene
2.2*-BiO]arane (1 T1
( 1 , V -SipnenylM.*' -diamine
(1,1'-Bipnenyr)-4.4'-n«acnioro-
t-aulannmne. M-Outyl-N-nn/ojo-
Butanoc add. 4.(Bn(2-cnt«oaltvyi)aminol
benzene-
t-Butanol (1)
2-Sulanone (I,T)
2 Sularwne peroxide (R.T)
2-Bulenal
2.8ulene. 1 4^jicnkxo- (I.T)
n-8ulyl alcnonol (0
Cacocrylic acid
Calcium cnromate
CarBunc acid. etOyt mac
Carbarmc acid, mathylnivoso-. etnyt asiar
CarOannda. N-«myt-N-o(f05o-
Cafturmd*. N-mamyl-N.nitroao-
Caroamde. tno-
CarOamoyl cntonOa. dmwtftyt-
Careone aod, dMnaUwm(i) an
CaroonocMondK acid, memyl mar (I.T)
CarBon oxyfluonda (R.T)
Cafoon tanachionila
Carbonyl fluonda (n.T) '
Cnloral
CMonrnoucH
Chkydane, tactvucal
CMofnapnuna
CMoroOanzafta
2OMoro»Mf*y* vmyt eww
Chloroform
oCNorapnanol
4-Cnkxo-o-tok«c*na. nydmcnionda
Cfirorrac aod, calciurn salt
Ctwyiana
Cramota
CraaoM
Craaykcaod
Cumarwd)
CydorMMan* (1)
1,3-CydooMt.idMna. 1,2,3,4,5.5-h*n(.v chtoro-
2.44-0. sail* and attars
Oaunomyon
000
DOT
cydoOuta(c.d)-pantaMn-2^)na
Oiallaia
Ownma (R.T)
Otamnotoluana
Hazardous
Waste No
U063
U063
U064 . .. .
U064
U066
U089
U062
U070
U071
U072
U073
U074
U07S .. .
U192
U060
U081 ..
U078
U079 .. ..
U025
U081 . ..
U082
U240
U083
U084
U085
U108
U086
U088
U089
U148
U090
U091
U092
U093
U094 ... .
U097
U098
U099
U102
U1M
U105
U106
U107
utoa
U109
ui 10
U001
U087
U076
U077
U114 .
U131
U024
U003
UI117
U025
U184
U208
U209
U218
U247
U227
U043
Substance
Oioenzl a.n lanmracane
I 2 5.6-Oioenzantlvacene
1.2 7,S-CNtienzopyrene
Oibenzfa.ilpyrene
1 2-Oibrofno-3-chloropropane
Qoulyl pntnalata
c-Ownkxabanzena
m-Oichlorooenzene
p-Oicniorobenzene
3.3'-Oicnioroeenzidna
1 ,4-OwrUorc-2-bulana (I.T)
Otchloroditiuoromethane
3.5-Oicnl(x o-N-( 1 . 1 -dnwtnyl-2-prooynyl)
benzamda
Oicnioro dipnanyl dunioroetnana
Dicnloro dipnenyl tncMoroathane
t I -Oicnioroetnyiane
i 2-Oicnloroeirtyiene
Oichloroetrtvl etner
2. 4-Oicnioroprienol
2.6-Oicnioropnanol
2.4-Oicnioropnanoi
1 2-EmanarjryiTM<;amamo<*W<4te ac4
Ethane. 1,1,1,2,2,2-neiaenlorc-
Etharw. 1 . 1 '-ImalHytanabuXoicy)lBiat2-chloro-
Etnananiinla (1. T)
Ethane, l.r-oiyon- (I)
Etnana. l.l'4xydi*(2-cniore-
Ethanc. pentacftkxo-
etnana, 1.l.t.2-niracr*orc-
Ethana. V1.2.2.|aliacNorc-
Ethanetmoamida
Ethane, i,l,l.-lncny-
pnanyll.
Ethane. 1,1,2-lncntoro-
Ethana. cnkxo-
E-10
-------
Chapter I—EnvirennMntal Protection Agency
1261.33
Hazardous
Wast* No.
UO42
U078
U079
U210
U173
U004 _.
UOOt
U112
U113
UJ38
UO38 _;..
U114
U087
U077
U11S
U1I7
U078
U118
U119
U139
U120
UI22
UI23
U124 . ...
U125
U147
U213
U125
U124
U206
U128
U183
U127
U128
U129
U130
U131
U132
U243
U133
U088
UOM
UOM
U109
U134 >i_m_
U134
Ut3S
UOM
U136
U116
Ut37
Ut39
U140
U141
U142
U143
U144
U14S
U148
UI29
U147
U148
U149
uiso
U1SI
U152
U092
U029 ..
U045
U048
Sufiattiie* Waste No
Elnana. l.1-dK«oro-
Etnana. trana-i,2
Etnanot 2.2Mn*oaomno)b«>.
Ethanoyl cMond* (CAT)
Ethyl acatau (0
Ethyl aoylM (1)
EtfiyMnt dcMond*
Ethton* onda (I.T)
Ethyl emer (1)
Etnynnetnacrylate
Ethyl rnetnaneauNonatt
Fluor anmana
FofmefdeAyda
Forme aod (C.T1
Furan (1)
2.S-funndnna
Furan. lavanydn-(l)
FuriuraMD
Furfuran (1)
O-Glucooyranoaa. 2-daoxy-2(3-ma
Mainanoill)
Matnapynlana
Mainoxycnkx
Mainyl alcohol (1)
Methyl DrorrMe
I Mainyibuladiene (1)
Matnyl cnionoa (i.T)
Mainyl cniorocaroonate (I.T)
Metnylcniorolorm
3-Mainylcrmaninrene
4.4 -Melhywnacxs<2-cni(XoapiUnal
2.2'-MemyianaO»(3.4,e-tncnloropnanol)
Maihylan* arorrada
Mainyl ethyl kaiona (I.T)
Matnyl ethyl kaiona paronda (R.T)
Matnyl odKJa
Matnyl isodulyl kaiona (1)
Mainyl mamacrylaia (I.T)
4.Mathyi-2-panunona (1)
MainvUNouraol
Mrtofnyctn C
S.12-Napninacamdiona. (8S-osHd-acatyl-tO-
( (3-amno-2,3.B-tndeon;-alpn*-l.-lyxo-
haiopyranoaylKuy'1-7.8.9. 10-latranydro-
8.8. 11 •tnnydroxy- 1 -niamaiy-
Napntnalan*
NapntnaMne, 2-cnloro-
mathyl-( 1 , 1 •-bipnanylM.4'oW]-oia
salt
1.4,Napnmaquinona
1-Napntnylansna
2-Napntnylamina
iipna-Napntnyta/nme
Nitrooanzana (I.T)
p-Nitropnanol
2-NHroprapana (1)
N-Nitrosoawvoulylarrena
N-Niiroaooiatnyiamina
N-Nilroio-N-propylamma
N-Nitro»o-N-amyturaa
N-Nnroso-N-metnyiuraa
N-Nitroao-N-matftyluramana
5-Nnro-o-toiuidina
1.2-Oxainiolane. 2.2-dnnde
2H-i.3.2-O>azapnospnonrw. 2-{bis(2-cnioro-
airtyDammoltairanydro-. ouoa 2-
Oarane (I.T)
E-ll
-------
§261.33
Title 40— Protection of Environment
Hazardous
Wasta No
Suostanca
! Owrana. 2-ene
Phospnonc acid. Lead sail
PN»pnoroditnio« aod, 0,0--, pnoaqnata (3:1)
1-Propano(. Z3-«ooJiy-
t -Propane!, 2-m«myt- (!,T)
2-Propanon* (I)
2* PTOQ^O tttmi9 a
PrepafM. 1.3-dKtNoro-
t-PrapatM. 1.1.2,3.3.3-n«iacfitoro-
2-ProparwiMnM
2-PtapananMiiU). 2-mattiyl- (I.T)
2-Propaooc acid (I)
2-Propano« add. ainyl eslec (I)
2-PrapanoK aoo. 2-m»inyt-. atfiyl mtar
2-Prooanoc aod. 2-m«tny(-, mainyl aaiar (I.T)
Propane aod, 2-R4,5-tncnioropr*anoiy)-
rvPrapylamn* (I.T)
Propytao* acMonaa
Hazardous
Wasta No
U205
U232 .
U207
U208 . .. .
U209
U210
U212
U213
U214
U21S
U21S
UZ17
U218 . .
U153.
U219 . .
U244 ..
U220
U221
U223
Substanca
Sullur salemda (R.T)
2.4.5-T
1 .2.4,S-Tatracniorooanzana
1.1.1 .2-Ta(racnianMtnana
1 . 1 .2.2-Taffacnioroainana
Tavacnioroathylana
2.3.4.8-Talracnioropnanol
Talrarrydrofuran (1)
ThaikurrKI) acatata
ThalkunXO carOonata
ThalaunKl) cfuonda
Thailium
4.4'-SlHb*rwdnt. ajpha.alpna'-dwtnyl-
Streotozotocin
Sulfur hydnda
Sultunc acid, dvnattyl aaiar
Sullur pnoaprwM (H)
[45 PR 78529. 78541. Nov. 25. 1980. as
amended at 48 PR 27477. May 20. 1981: 49
FR 19923. May 10. 1984]
E-12
-------
APPENDIX F
HAZARDOUS CONSTITUENTS (40 CFR 261, APPENDIX VIII)
The content of this Appendix was reproduced
from the Code of Federal Regulations of July
1, 1984. Users should check the current ver-
sion of the Code of Federal Regulations and
more recent issues of the Fe"deral Register for
amendments.
-------
APPENDIX VIII— HAZARDOUS
AcetonitrUe (Ethanenitrile)
Acetophenone (Ethanone, 1-phenyl)
3-< alpha- AcetonyibenzylM-
hydroxycoumarin and salts (Warfarin)
2-Acetylaminofluorene (Acetamide. N-OH-
fluoren-2-yl)-)
Acetyl chloride (Ethanoyl chloride)
l-Acetyl-2-thiourea (Acetamide, N-(amin-
othioxomethyl)-)
Acrolein (2-Propenal)
Acrylamide (2-Propenamide)
Acrylonltrile (2-Propenenitrile>
Aflatoxins
Aldrin ( 1,2,3.4.10.10-Hexachloro-
1.4.4a.5.8.8a.8b-hexahydro-endo,exo-
M:5,8-Dlmethanonaphthalene)
Allyl alcohol (2-Propen-l-ol)
Aluminum phosphide
4-Aminobiphenyl ( C l.l'-Biphenyl]-4-amlne)
S-Amino-l.la,2.8,8tt,8b-hexahydro-a-
( hydroxymethy 1 )-8a-methoxy-5-methyl-
carbamate azirinoC2'.3>:3.41pyrrolo(1.2-
a]lndole-4.7-dlone. (ester) (Mltomycin C)
:3.4]pyrroioU.2-a)lndole-4,7-
dione, 8-amlno-8-C((amino-
carbonyl)oxy imethyU- 1, la.2.8.8a,8b-
hexahydro-8amethoxy-S-methy- )
5-
-------
Part 261, App. VIII
Title 40—Protection of Environment
Arsenic and compounds. N.O.S.*
Arsenic acid (Orthoarsenic acid)
Arsenic pentoxide (Arsenic (V) oxide)
Arsenic trioxide (Arsenic (III) oxide)
Auramme (Benzenamme. 4,4'-
carbonimidoylbislN.N-Dimethyl-, mono-
hydrochloride)
Azaserine ether (Ethane. 1.1'-
oxybis(2-chloro-])
N,N-Bls<2-chloroethyl)-2-naphthylatnine
(Chlomaphazine)
Bis(2-chloroisopropyl> ether (Propane. 2.2'•
oxybist2-chloro-]>
Bls(chloromethyl) ether (Methane.
oxybtstchloro-])
Bls<2-ethylhexyl) phthalate (1,2-Benzenedi-
carboxylic acid. bis(2-ethylhexyl) ester)
Bromoacetone (2-Propanone. 1-bromo-)
Bromomethane (Methyl bromide)
4-Bromophenyl phenyl ether (Benzene. 1-
bromo-4-phenoxy-)
Brucine (Strychnidln-10-one. 2.3-dlmethoxy-
)
2-Butanone peroxide (Methyl ethyl ketone.
peroxide)
Butyl benzyl phthalate (1.2-Benzenedlcar-
boxylic acid, butyl phenylmethyl ester)
2-sec-ButyM,8-dlnitrophenol (ONBP)
(Phenol. 2,4-dlnitro-«-
2-Cyclohexyl-4.6-dinitrophenol (Phenol. 2-
cyclohexy 1-4,8-dinitro-)
Cyclophosphamide (2H-1.3,2. -Oxazaphos-
phorine, Cbis(2-chloroethyl)amlno]-tetra-
hydro-, 2-oxide)
Oaunomycin (S.12-Naphthacenedione, (8S-
cis)-8-acetyl-10-[(3-amino-2.3.S-trideoxy)-
alpha-L-lyxo-hexopyranosy Doxy 1-7.8.9,10-
tetrahydro-6.8,ll-trihydroxy-l-methoxy-)
DDD (Dichlorodiphenyldichloroethane)
(Ethane, l,l-dlchloro-2.2-bis(p-chloro-
phenyl)-)
ODE (Ethylene, l.l-dlchloro-2,2-bls(4-chlor-
ophenyl)-)
DDT (Dlchlorodiphenyltrichloroethane)
(Ethane. l.l.l-trichtoro-2.2-bis(D
-------
Chapter I—Environmental Protection Agency
Part 261, App. VIII
DibenzU.h]anthracene (1,2.5.6-Dibenzanth-
racene)
7H-DibenzoCc,g]carbazole(3.4.5,6-Dibenzcar-
bazole)
DibenzoCa,e]pyrene(1.2,4.5-Dibenzpyrene)
DibenzoCa.h]pyrene (1.2,5,6-Dibenzpyrene)
DibenzoCajlpyrene (1,2,7,8-Dlbenzpyrene)
l,2-Dibromo-3-chloropropane (Propane. 1,2-
dibromo-3-chloro-)
1,2-Dibromoethane (Ethylene dibromide)
Dibromomethane (Methylene bromide)
Di-n-butyl phthalate (1,2-Benzenedicarbox-
yllc acid, dibutyl ester)
o-Dichlorobenzene (Benzene, 1,2-dlchloro-)
m-Dichlorobenzene (Benzene, 1,3-dichloro-)
p-Dlchlorobenzene (Benzene, 1,4-dichloro-)
Dichlorobenzene. N.OJS.* (Benzene,
dichlorc-. N.O.S.')
3,3'-Dichlorobenzidine <[l,l'-Biphenyl]-4,4'-
diamine, 3,3'-dichloro-)
l,4-Dichloro-2-butene (2-Butene, 1,4-dich-
loro-)
Dichlorodinuoromethane (Methane, dich-
lorodifluoro-)
1,1-Dichloroethane (Ethylidene dichloride)
1.2-Dichloroethane (Ethylene dichloride)
trans-1,2-Dichloroethene (1.2-Dtchloroethy-
lene)
Dichloroethylene. N.O.S.* (Ethene, dich-
loro-, N.O.S.')
1,1-Dichloroethylene (Ethene. 1,1-dichJoro-)
Dichloromethane (Methylene chloride)
2,4-Dichlorophenol (Phenol. 2,4-dichloro-)
2,6-Dichlorophenol (Phenol, 2.6-dichloro-)
2,4-Oichlorophenoxyacetic acid (2,4-D), salts
and «sters (Acetic acid, 2,4-dichlorophen-
oxy-, salts and esters)
Dichlorophenylarsine (Phenyl dichloroar-
sine)
Dtchloropropane. N.O.S.* (Propane, dich-
loro-, N.O.S.*)
1,2-Dichloropropane (Propylene dichloride)
Dichloropropanol, N.O.S.* (Propanol, dich-
loro-, N.O.S.*)
Dlchloropropene, N.O.S.' (Propene. dich-
loro-. N.O-S.')
1,3-Dichloropropene (1-Propene. 1,3-dich-
loro-)
Dieldrin (1.2,3,4,10.10-hexachloro-S,7-epoxy-
l,4.4a,5,6,7,8,8a-octa-hydro-endo,exo-
1,4:S,8-Olmethanonaphthalene)
l,2:3,4-Dlepoxybutane <2,2'-Bloxirane>
Dlethylarsine (Arsine, diethyl-)
N,N-Diethylhydrazine (Hydrazine, 1.2-
diethyl)
O,O-Diethyl S-methyl ester of phosphoro-
dithioic acid (Phosphorodithioic acid.
O.O-diethyl S-methyl ester
O.O-Diethylphosphoric acid, O-p-nitro-
phenyl ester (Phosphoric acid, diethyl p-
nitrophenyl ester)
Diethyl phthalate (1,2-Benzenedicarboxylic
acid, diethyl ester)
O.O-Oiethyl O-2-pyrazinyl phosphoroth-
ioate (Phosphorothioic acid, O.O-diethyl
O-pyrazinyl ester
Diethy Istilbesterol (4.4'-Stilbenediol.
alpha.alpha-diethyl, bis(dihydrogen phos-
phate, (E)->
Dihydrosafrole (Benzene, 1,2-methylene-
dioxy-4-propyl-)
3.4-Dihydroxy-alpha-( methy lamino )methyl
benzyl alcohol (1.2-Benzenediol, 4-U-hy-
droxy-2-(methylamino )ethyU-)
Diisopropylfluorophosphate (DPP) (Phos-
phorofluoridic acid, bis(l-methylethyl)
ester)
Dlmethoate (Phosphorodithioic acid, O.O-
dimethyl S-C2-(methylamino)-2-oxoethyU
ester
3.3'-Dimethoxybenzidine (Cl.l'-BlphenyU-
4,4'diamine. 3-3'-dimethoxy-)
p-Oimethylamlnoazobenzene (Benzenamine.
N,N-dimethyl-4-( phenylazo)-)
7.12-DlmethylbenzCalanthracene (1.2-Ben-
zanthracene, 7,12-dimethyl-)
3,3'-Dimethylbenzidine ((l.l'-BlphenylM.^-
diamine. 3,3'-dimethyl->
Dimethylcarbamoyl chloride (Carbamoyl
chloride, dimethyl-)
1.1-Dlmethylhydrazine (Hydrazine. 1.1-di-
methyl-)
1.2-Oimethylhydrazine (Hydrazine. 1,2-di-
methyl-)
3.3-Dimethyl-l-(methylthlo)-2-butanone, O-
[(methylamino) carbonyUoxime (Thio-
fanox)
alpha,alpha-Dlmethylphenethylamine (Eth-
anamine, l.l-dimethyl-2-phenyl-)
2.4-Olmethylphenol (Phenol, 2.4-dimethyl-)
Dimethyl phthalate (1,2-Benzenedicarboxy-
lic acid, dimethyl ester)
Dimethyl sulfate (Sulfuric acid, dimethyl
ester)
Dinitrobenzene, N.O^.* (Benzene, dinitro-,
N.O.S.')
4,6-Dinitro-o-cresol and salts (Phenol, 2,4-
dinitro-6-methyl-, and salts)
2.4-Dlnitrophenol (Phenol, 2,4-dinitro-)
2,4-Dlnitrotoluene (Benzene, l-methyl-2,4-
dinitro-)
2.6-Dinitrotoluene (Benzene, l-methyl-2,8-
dinitro-)
Di-n-octyl phthalate (1,2-Benzenedicarboxy-
lic acid, dloctyl ester)
1.4-Dloxane (1.4-Diethylene oxide)
Diphenylamine (Benzenamine, N-phenyl-)
1,2-Diphenylhydrazine (Hydrazine. 1,2-dl-
phenyl-)
Di-n-propylnitrosamine (N-Nitroso-di-n-pro-
pylamine)
Disulfoton (O.O-diethyl S-C2-
(ethylthio)ethyl] phosphorodithioate)
2.4-Dithiobiuret (Thioimidodicarbonic dia-
mide)
Endosulfan (5-Norbornene, 2,3-dimethanol.
1,4,5,6,7,7-hexochloro-. cyclic sulfite)
Endrin and metabolites (1,2,3,4.10.10-hex-
achloro-6,7-epoxy-l,4.4a,5,6,7,8,8a-
octahydro-endo.endo-1,4:5,8-
dlmethanonaphthalene, and metabolites)
F-5
-------
Part 261, App. VIII
Title 40—Protection of Environment
Ethyl carbamate (Urethan) (Carbamic acid.
ethyl ester)
Ethyl cyanide (propanenitrile)
Ethylenebisdithiocarbamic acid, salts and
esters (1.2-Ethanedlylbiscarbainodithioic
acid, salts and esters
Ethyleneimine (Aziridine)
Ethylene oxide (Oxirane)
Ethylenethiourea (2-Imidazolidinethione)
Ethyl methacrylate (2-Propenoic acid. 2-
methyl-, ethyl ester)
Ethyl methanesulfonate (Methanesullonic
acid, ethyl ester)
Fluoranthene (Benzotj.kJfluorene)
Fluorine
2-Fluoroacetamide (Acetatnide, 2-fluoro->
Fluoroacetic acid, sodium salt (Acetic acid.
fluoro-, sodium salt)
Formaldehyde (Methylene oxide)
Formic acid (Methanoic acid)
Glycidylaldehyde (l-Propanol-2,3-epoxy)
Halomethane, N.O.S.*
Heptachlor (4.7-Methano-lH-indene.
l,4.5,6,7,8,8-heptachloro-3a.4,7,7a-
tetrahydro-)
Heptachlor epoxide (alpha, beta, and
gamma isomers) (4,7-Methano-lH-indene,
l,4.5,6,7.8,8-heptachloro-2,3-epoxy-3a,4,7,7-
tetrahydro-, alpha, beta, and gamma iso-
mers)
Hexachlorobenzene (Benzene, hexachloro-)
Hexachlorobutadiene (1.3-Butadiene,
1,1,2.3.4,4-hexachloro-)
Hexachlorocyclohexane (all isomers) (Lin-
dane and isomers)
Hexachlorocyclopentadiene (1,3-Cyclopen-
tadiene, 1,2,3.4.5.5-hexachloro-)
Hexachloroethane (Ethane. 1,1,1.2.2,2-hex-
achloro-)
1.2,3,4,10,10-Hexachloro-1.4,4a,5,8,8a-
hexahydro-l,4:5,8-endo,endo-
dimethanonaphthalene (Hexachlorohexa-
hydro-endo.endo-dimethanonaph thaiene)
Hexachlorophene (2.2'-Methylenebis(3,4.6-
trichlorophenol))
Hexachloropropene (1-Propene. 1,1,2.3,3.3-
hexachloro-)
Hexaethyl tetraphosphate (Tetraphos-
phoric acid, hexaethyl ester)
Hydrazine (Diamine)
Hydrocyanic acid (Hydrogen cyanide)
Hydrofluoric acid (Hydrogen fluoride)
Hydrogen sulfide (Sulfur hydride)
Hydroxydlmethylarsine oxide (Cacodylic
acid)
Indeno(l;2,3-cd)pyrene (1.KW1.2-
pheny lene )py rene)
lodomethane (Methyl iodide)
Iron dextran (Ferric dextran)
Isocyanic add, methyl ester (Methyl iso-
cyanate)
Isobutyl alcohol (1-Propanol, 2-methyl-)
Isosafrole (Benzene, l,2-methylenedioxy-4-
allyl-)
Kepone (Decachlorooctahydro-1.3,4-Meth-
ano-2H-cyclobuta(cdlpentalen-2-one>
Lasiocarpine (2-Butenoic acid, 2-methyl-. 7-
C(2,3-dihydroxy-2-U-methoxyethyl)-3-
methyl-1 -oxobutoxy )methy 1 ]-2,3,5,7a-
tetrahydro-lH-pyrrolizin-1-yl ester)
Lead and compounds, N.O.S.*
Lead acetate (Acetic acid, lead salt)
Lead phosphate (Phosphoric acid, lead salt)
Lead subacetate (Lead. bis(acetato-
O )tetrahydroxytri-)
Maleic anhydride (2,5-Furandione)
Maleic hydrazide (1.2-Dihydro-3,6-pyridazin-
edione)
Malononitrile (Propanedinitrile)
Melphalan (Alanine, 3-Cp-bis(2-
chloroethyDamlnolphenyl-, L-)
Mercury fulminate (Fulminic acid, mercury
salt)
Mercury and compounds, N.O.S.*
Methacrylonitrile (2-Propenenitrile. 2-
methyl-)
Methanethiol (Thiomethanol)
Methapyrilene (Pyridine, 2-C(2-
dimethylamino)ethyl]-2-thenylamlno-)
Methoimyl (Acetimidic acid, N-
[(methylcarbamoyDoxyHhlo-, methyl
ester
Methoxychlor (Ethane, l,l,l-trichloro-2,2'-
bis( p-methoxy pheny 1)-)
2-Methylaziridine (1.2-Propylenimine)
3-Methylcholanthrene
(Benz[j]aceanthrylene, 1.2-dlhydro-3-
methyl-)
Methyl chlorocarbonate (Carbonochloridlc
acid, methyl ester)
4,4'-Methylenebis(2-chloroaniline) (Benzen-
amine, 4,4'-methylenebis-<2-chloro-)
Methyl ethyl ketone (MEK) (2-Butanone)
Methyl hydrazine (Hydrazine, methyl-)
2-Methyllactonitrile (Propanenitrile, 2-hy-
droxy-2-methyl-)
Methyl methacrylate (2-Propenoic acid, 2-
methyl-, methyl ester)
Methyl methanesulfonate (Methanesulfonic
acid, methyl ester)
2-Methyl-2-(methylthio)proplonaldehyde-o-
(methylcarbonyl) oxime (Propanal, 2-
methyl-2-(methylthio)-, O-
[(methylaminOcarbonynoxime)
N-Methyl-N'-nitro-N-nitrosoguanidine (Gua-
nidine, N-nitroso-N-methyl-N'-nitro-)
Methyl parathlon (O,O-dimethyl O-(4-nltro-
phenyl) phosphorothioate)
MethylthiouracU (4-lH-Pyrimidinone, 2,3-
dihydro-8-methyl-2-thioxo-)
Mustard gas (Sulfide, bis(2-chloroethyl)-)
Naphthalene
1,4-Naphthoquinone (1,4-Naphthalene-
dione)
1-Naphthylamine (alpha-Naphthylamine)
2-Naphthylamine (beta-Naphthylamine)
l-Naphthyl-2-thiourea (Thiourea, 1-naphth-
alenyl-)
Nickel and compounds. N.O.S.*
Nickel carbonyl (Nickel tetracarbonyl)
Nickel cyanide (Nickel (II) cyanide)
P-6
-------
Chapter I—Environmental Protection Agency
Part 261, App. VIII
Nicotine and salts (Pyridine. (S)-3-(l-
methyl-2-pyrrolidinyl)-. and salts)
Nitric oxide (Nitrogen (II) oxide)
p-Nitroaniline (Benzenamine, 4-nitro-)
Nitrobenzine (Benzene, nitro-)
Nitrogen dioxide (Nitrogen (IV) oxide)
Nitrogen mustard and hydrochloride salt
(Ethanamine. 2-chloro-. N-<2-chloroethyD-
N-methyl-. and hydrochloride salt)
Nitrogen mustard N-Oxide and hydrochlo-
ride salt (Ethanamine. 2-chloro-, N-<2-
chloroethyD-N-methyl-, and hydrochlo-
ride salt)
Nitroglycerine (1,2.3-Propanetriol, trini-
trate)
4-Nitrophenol (Phenol, 4-nitro-)
4-Nitroquinoline-l-oxide (Quinoline. 4-nltro-
1-oxide-)
Nltrosamine, N.O.S.*
N-Nitrosodi-n-butylamine (1-Butanamine,
N-buty l-N-nitroso-)
N-Nitrosodiethanolamine (Ethanol. 2,2'-
(nitrosoimino )bis-)
N-Nitrosodiethylamine (Ethanamine, N-
ethy l-N-nitroso-)
N-Nltrosodimethylamine (Dimethylnitrosa-
mine)
N-Nitroso-N-ethylurea (Carbamide, N-ethyl-
N-nltroso-)
N-Nitrosomethylethylamine (Ethanamine,
N-methy l-N-nitroso-)
N-Nltroso-N-methy lurea (Carbamide, N-
methy l-N-nitroso-)
N-Nltroso-N-methy lurethane (Carbamlc
acid, methylnitroso-, ethyl ester)
N-Nitrosomethylvlnylamine (Ethenamine,
N-methy l-N-nitroso-)
N-Nltroaomorphollne (Morpholine, N-nitro-
so-)
N-Nitrosonornlcotine (Nomicotine, N-
nitroso-)
N-Nltrosoplperidine (Pyridine, hexahydro-,
N-nitroso-)
Nitrosopyrrolidine (Pyrrole, tetrahydro-, N-
nitroso-)
N-Nltrososarcosine (Sarcosine, N-nltroso-)
5-Nitro-o-toluldine (Benzenamine, 2-methyl-
5-nitro-)
Octamethylpyrophosphoramide (Diphos-
phoramlde, octamethyl-)
Osmium tetroxide (Osmium (VIII) oxide)
7-OxabicycloC2.2.11heptane-2,3-dlcarboxyUc
acid (Endothal)
Pmraldehyde (1,3,5-Trloxane, 2,4,8-tri-
methyl-)
Parathion (Phosphorothlolc acid, O.O-
dlethyl O-(p-nitrophenyl) ester
Pentachlorobenzene (Benzene, pentachloro-
)
Pentachloroethane (Ethane, pentachloro-)
Pentachloronltrobenzene (PCNB) (Benzene,
pentachloronltro-)
Pentachlorophenol (Phenol, pentachloro-)
Phenacetln (Acetamide. N-<4-ethoxy-
phenyl)-)
Phenol (Benzene, hydroxy-)
Phenylenedlamlne (Benzenediamine)
Phenylmercury acetate (Mercury, acetato-
phenyl-)
N-Phenylthiourea (Thiourea, phenyl-)
Phosgene (Carbonyl chloride)
Phosphine (Hydrogen phosphide)
Phosphorodithioic acid, O.O-diethyl S-
[(ethylthio)methyll ester (Phorate)
Phosphorothioic acid, O.O-dimethyl O-tp-
Udimethylamino)sulfonyl)phenyU ester
(Famphur)
Phthalic acid esters, N.O.S.* (Benzene, 1,2-
dicarboxylic acid, esters. N.O.S.*)
Phthalic anhydride (1,2-Benzenedicarboxy-
lic acid anhydride)
2-Picoline (Pyridine, 2-methyl-)
Polychlorlnated biphenyl, N.O.S.'
Potassium cyanide
Potassium silver cyanide (Argentate(l-), di-
cyano-, potassium)
Pronamide (3,5-Dichloro-N-< 1,1-dimethy 1-2-
propyny 1 )benzamide)
1,3-Propane sultone (1,2-Oxathiolane, 2,2-dl-
oxide)
n-Propylamme (1-Propanamine)
Propy Ithiouracil (Undecamethylenedia-
mine. N,N'-bis(2-chlorobenzyl)-, dlhy-
drochloride)
2-Propyn-l-ol (Propargyl alcohol)
Pyridine
Reserpine (Yohimban-16-carooxylic acid,
11.17-dimethoxy-18-[(3.4,5-
trimethoxybenzoyl>oxy]-, methyl ester)
Resorcinol (1,3-Benzenedlol)
Saccharin and salts U,2-Benzoisothiazolin-3-
one, 1,1-dloxide. and salts)
Saf role (Benzene, 1.2-methylenedloxy-4-
allyl-)
Selenious acid (Selenium dioxide)
Selenium and compounds. N.O.S.*
Selenium sulfide (Sulfur selenide)
Selenourea (Carbamimldoselenoic acid)
Silver and compounds, N.O.S.'
Silver cyanide
Sodium cyanide
Streptozotocln (D-Glucopyranose, 2-deoxy-
2-( 3-methy 1-3-nitrosoureido)-)
Strontium sulfide
Strychnine and salts (Strychnldln-10-one.
and salts)
1,2,4,5-Tetrachlorobenzene (Benzene,
1.2.4.5-tetrachloro-)
2,3,7.8-Tetrachlorodibenzo-p-dioxln (TCDD)
(Dlbenzo-p-dloxin, 2,3,7,a-tetrachloro-)
Tetrachloroethane, N.O.S.* (Ethane, tetra-
chloro-. N.O.S.*)
1,1,1.2-Tetrachlorethane (Ethane. 1.1,1.2-
tetrachloro-)
1,1.2,2-Tetrachlorethane (Ethane. 1.1,2,2-
tetrachloro-)
Tetrachloroethane (Ethene, 1.1.2,2-tetra-
chloro-)
Tetrachloromethane (Carbon tetrachloride)
2,3,4,8,-Tetrachlorophenol (Phenol, 2,3,4.6-
tetrachloro-)
Tetraethyldithiopyrophosphate (Dithiopyr-
ophosphoric acid, tetraethyl-ester)
F-7
-------
Part 261, App. VIII
Title 40—Protection of Environment
Tetraethyl lead (Plumbane, tetraethyl-)
Tetraethylpyrophosphate (Pyrophosphoric
acide, tetraethyl ester)
Tetranitromethane (Methane, tetranitro-)
Thallium and compounds. N.O.S.*
Thallic oxide (Thallium (III) oxide)
Thallium (I) acetate (Acetic acid, thallium
(I) salt)
Thallium (I) carbonate (Carbonic acid, dith-
allium (I) salt)
Thallium (I) chloride
Thallium (I) nitrate (Nitric add. thallium
(I) salt)
Thallium selenite
Thallium (I) sulfate (Sulfuric acid, thallium
(I) salt)
Thloacetamide (Ethanethioamide)
Thiosemlcarbazide (Hydrazinecarbothioa-
mide)
Thlourea (Carbamide thio-)
Thiuram (Bis(dimethylthiocarbamoyl) di-
sulfide)
Toluene (Benzene, methyl-)
Toluenediamine (Oiaminotoiuene)
o-Toluidine hydrochloride (Benzenamine. 2-
methyl-. hydrochloride)
Tolylene diisocyanate (Benzene. 1,3-diiso-
cyanatomethyl-)
Toxaphene (Camphene. octachloro-)
Tribromomethane (Bromoform)
1,2,4-Trichlorooenzene (Benzene, 1.2.4-trich-
loro-)
1.1,1-Trichloroethane (Methyl chloroform)
1.1,2-Trichloroethane (Ethane, 1,1,2-trich-
loro-)
Trichloroethene (Trichloroethylene)
Trichloromethanethiol (Methanethiol.
trichloro-)
Trichloromonofluoromethane (Methane,
trichlorofluoro-)
2,4.5-Trichlorophenol (Phenol. 2.4,5-trtch-
loro-)
2.4.6-Trichlorophenol (Phenol, 2,4.6-trtch-
loro-)
2,4,5-Trichlorophenoxyacetlc acid (2.4.5-T)
(Acetic acid. 2.4,5-trichlorophenoxy-)
2,4,5-Trichlorophenoxyproplonic acid (2,4,5-
TP) (Silvex) (Propionoic acid, 2-(2,4,5-
trichlorophenoxy)-)
Trichloropropane, N.O.S.* (Propane, trich-
loro-, N.O.S.*>
1.2.3-Trichloropropane (Propane, 1,2,3-trich-
loro-)
O.O.O-Triethyl phosphorothioate (Phoo-
phorothioic acid. O.O.O-trlethyl ester)
sym-Trinitrobenzene (Benzene, 1,3.5-trinl-
tro-)
Tris(l-azridinyl) phosphine sulflde (Phos-
phine sulfIde, triad-aziridinyl-)
Tris(2.3-dibromopropyl) phosphate (1-Pro-
panol, 2,3-dibromo-, phosphate)
Trypan blue (2.7-Naphthalenedisulfonic
acid, S.S'-CO.S'-dimethyK l.r-biphenyl)-
4.4<-diyl)bis(azo)]bis(S-amino-4-hydroxy-.
tetrasodium salt)
Uracil mustard (Uracil 5-Cbis(2-
chloroethyDamino]-)
Vanadic acid, ammonium salt (ammonium
vanadate)
Vanadium pentoxide (Vanadium (V) oxide)
Vinyl chloride (Ethene, chloro-)
Zinc cyanide
Zinc phosphide
[46 PR 27477. May 20. 1981; 46 PR 29708.
June 3,1981; 49 PR 5312. Feb. 10.1984]
EFFECTIVE DATE NOTE At 49 PR 5312. Feb.
10, 1984. the entries for 2-Chloro-l, 3-butadi-
ene (cnloroprene), and 3-Chloropropene
(allyl chloride), were added to the table in
Part 261. App. VTII, effective August 10.
1984.
F-8
-------
APPENDIX G
HOW TO USE A RANDOM NUMBER TABLE
-------
How to Use a Random Number Table
The sampling procedure for contained wastes that is .described
in Section 7 of the Manual requires you to select sampling points
using a random number table. This Appendix gives the general
procedure for using such a table, which can be found in almost any
statistical text or handbook.
The general problem is to select a sample of n members (such
as grid points to be sampled) from a population of N members (such
as the total number of points in the grid). Below we present a
"single-stage" method of drawing such a sample. Other methods
provide somewhat greater assurance of randomness, but at the cost
of additional complexity. The method is as follows:
1. Decide upon an arbitrary rule for selecting entries from
the table. You might want to choose the second row in the
first column, the third row in the second column, and so
on, or every kth number.
2. Number your unive'rse from 1 to N. If N has three digits,
the first number in your universe would be 001, and so
forth.
3. The number of digits in each random number in the table
may exceed the number of digits in N. If so, decide upon
an arbitrary rule to select from each random number in the
table another number with the correct number of digits.
For example, if the table is made up of five-digit numbers
and N has three digits, you could use the first three of
each random number, or digits 1-3-5, or 2-3-4, or any
three-digit set.
4. Construct a list of n random numbers using the rules in Steps
1 and 3 above. This list will then constitute a random
sample of the set N.
5. If you exhaust the table before n random numbers have been
drawn, start at a new place near the beginning of the
table and continue as before.
An alternative to the manual process described above is to
use the random number function RANDOM that is contained in the
BASIC software on most microcomputers.
G-3
-------
APPENDIX H
TYPICAL PRICES FOR HAZARDOUS WASTE TEST PROCEDURES
-------
TYPICAL PRICES FOR HAZARDOUS WASTE TEST PROCEDURES
The prices given below are based chiefly on a survey of
testing laboratories that was conducted by Industrial Economics,
Inc. (lEc) in the course of its work for the Office of Solid
Waste. The prices are current as of the spring of 1984. In two
cases (Ignitability and Corrosivity), figures missing from the lEc
survey were supplied by telephone calls to laboratories in the New
England region. The figures are indicative of unit prices charged
for small numbers of samples. Runs involving large numbers of
samples would receive price discounts.
Pr ice
Test Method ($ per sample)
Ignitability 25 - 60
Corrosivity
pH ' 5
Steel corrosion test 75 - 200
EP Toxicity
Extraction procedure . 100 - 150
8 SDWA metals 145 - 475
Pesticides analysis 125 - 215
Herbicides analysis 150 - 270
Cyanide (with separate extraction procedure) 100
Oily Waste EP Toxicity
Extraction procedure plus 8 SDWA metals 750
Total Organic Carbon
Non-standard matrix (solid, sludge) 20 - 65
Standard matrix (wastewater) 20 - 60
Total Oil and Grease
Non-standard matrix 16 - 75
Standard matrix 16 - 70
H-3
-------
Test Method
($ per sample)
Total Metals
Digestion
Non-standard matrix
Standard matrix
Metals analysis
As: furnace
3a: furnace
Cd: furnace
Hex Cr: colorimetric
Cr : furnace
Pb: furnace
Hg : cold-vapor
Ag : furnace
Ni: furnace
8 SDWA metals
13 priority pollutant metals
10 - 25
0-15
10
10
10
15
10
10
15
10
10
20
20
20
30
20
20
30
20
20
200
200 - 250
Organic Analyses
Sample preparation
Solid, sludge
Extraord inary preparation/cleanup
Refinery organics in sludge
Appendix VIII consituents in sludge
0-40
100
100
500
1500
Gas Chromatography
Halogenated volatile organics 80 - 120
Non-halogenated volatile organics 80 - 120
Aromatic volatile organics 80 - 120
Polychlorinated biphenyls 150 - 180
Pesticides and PCBs, including fractionation 175 - 200
Gas Chromatogfaphy/Mass Spectrometry
Volatile organics
Priority pollutants
Appendix VIII constituents
170 - 240
450
H-4
-------
Test Method ($ per sample)
Acid extractables
Priority pollutants 200 - 250
Appendix VIII constituents 500
Base/neutral extractables
Priority pollutants 250 - 400
Appendix VIII constituents 650
H-5
-------
APPENDIX I
EXAMPLES OF DELISTING PETITIONS
The following types of wastes are represented:
• Inorganic wastes
• Organic wastes
A complete petition is presented for the former;
excerpts are given for the latter. For the other
two major types of facilities — petroleum
refineries and multiple waste treatment facilities
— there is too much variability from petition to
petition to construct representative examples.
The information contained in the Inorganics exam-
ple is based on an actual petition submitted by
Texas Instruments, Inc. of Dallas, TX. Names of
people have been altered, and some of the content
has been changed for the purpose of providing a
more general illustration.
-------
INORGANIC WASTESTREAM
OPTIONAL FORM:
DELISTING PETITION FOR WASTE STREAM
F006: Wastewater treatment sludges from electroplating
processes
Submitted by:
ABC INDUSTRIES, INC.
120 Smith Lane
Dallas, TX 75266
Date:
December 12, 1982
1-3
-------
SECTION A: Administrative Data and Summary
1.
2.
3.
Name [260.20(b)(1)]
a. Name of firm:
ABC Industries, Inc.
b. Address of firm: Street:
City:
State:
c. RCRA Generator ID Number:
120 Smith Lane
Dallas
Texas
Zip:
75226
TXD000567890
Facility Location [260.20(b)(1)]
a. Name of facility: Long Horn Avenue Site
b. Location of facility: Street:
City:
State:
5 Long Horn Avenue
Dallas
TX
Zip: 75266
Name(s) of personnel to be contacted for additional informa-
tion pertaining to this petition:
Name
Frederick Lewis
Susan Smith
Thomas Roberts
Joseph Kale
Title
Mgr, Process Eng.
Process Engineer
Engineering Analyst
Mgr, Anal. Svcs Div
Green Laboratories
Telephone
(214) 555-5555
(214) 555-5555
(214) 555-5555
(214) 555-5555
1-5
-------
4. Description and Justification for the Proposed Action
Please describe briefly the proposed delisting action, why it
is needed, and how it will affect your operation. Describe
why you believe that the waste stream of concern (a) is not
hazardous for the reasons it was originally listed and (b)
contains no other constituents or characteristics that render
it hazardous as defined in 40 CFR 261. [260.20(b)(2), (3) and
(4)]
This petition seeks to exclude from regulation under Subpart D of
40 CFR Part 261 a waste stream that is generated at a metal finishing
shop at the ABC Industries Manufacturing Facility at Long Horn Avenue in
Dallas, TX. The waste stream is EPA HW Code F006, Wastewater Treatment
Sludges from Electroplating Operations. This action is needed because
the disposal of these materials as a hazardous waste imposes an unneces-
sary burden on the petitioner, if indeed these materials are non-hazar-
dous as defined by 40 CFR 261. Thif action will affect only the waste
stream generated at the metal finishing shop of the above-mentioned
facility.
Testing of the sludges in question indicates that: (a) the leachate
from the sludge does not exceed the EP Toxicity Limits shown in Table 1,
Section 261.24; (b) it does not contain appreciable amounts of the
constituents for which it was listed as hazardous (as given in Part 263,
Appendix VII); and (c) it contains no other constituents that would
render it hazardous as defined in 40 CFR 261.
5. Certification of Accuracy and Responsibility [260.22(i)(12) ]
I certify under penalty of law that I have personally examined
and am familiar with the information submitted in this demon-
stration and all attached documents, and that based on my
inquiry of those individuals immediately responsible for ob-
taining the information, I believe that the submitted informa-
tion is true, accurate, and complete. I am aware that there
are significant penalties for submitting false information,
including the possibility of fine and imprisonment.
Frederick Lewis ~L»i At J I
VP for Operations 1/ILKJ*^L* (~~4^L*-^
Waste Generator, Title or
Authorized Representative*
of Waste Generator, Title
*Note: An "authorized representative" is a person respon-
sible for the overall operation of a facility or an opera-
tional uni:E^H4pr example, a plant manager, superintendent,
or person of equivalent responsibility). Consultants or
other outside parties may not sign the certification state-
ment.
1-6
-------
SECTION B: Production Processes
1. Description of Manufacturing Processes and Other Operations
L260.22(i)(5)].
a. Please provide a brief description of the on-site
manufacturing/generating process(es) that produce the
waste stream. Include descriptions of major equipment
items and production lines. Also, describe the stages of
the typical operating cycle on a daily, weekly, or other
basis as appropriate.
The on-site processes that produce the waste stream are from metal
finishing operations that are outlined in (b) below.
b. Please provide a description of all surface and equipment
preparation, cleaning, degreasing, coating or painting
processes used in your facility that you have not de-
scribed in (a) above. (See Attachment I)
1. Chromate conversion coating of aluminum / MIL-C-5541
2. Passivation of corrosion resistant steels / QQ-P-35 Types II,IV,V
3. Anodizing of aluminum alloy parts / MIL-A-8625
4. Phosphatizing, light, iron
5. Cadmium plate*
6. Cyanide copper plate*
7. Sulfamate nickel
8. Electroless nickel plate
9. Woods nickel strike
10. Tin plate*
11. Various cleaning of oils and coolants from machinery
*NOTES:
All of the above process solutions are followed by one or more water
rinse tanks which also pass through the treatment facility.
All pretreatments for plating operations use the same cleaning steps
as alodine, anodize, or passivate, and are therefore not listed
separately.
c. Attach a schematic diagram of all manufacturing processes,
surface~~p^eparation, cleaning, and other operations that
may provide influent into the waste stream.
(See Attachment I)
1-7
-------
ATTACHMENT I
Process Flow
TEXAS INSTRUMENTS/LEMMON AVENUE
RECEIVE
RAW MATERIAL
MACHINING
MILL
GRIND
LATHE
TAPPING
HEAT TREATING •*-
CLEAN/SURFACE PREP*
SANDBLAST
PARTS WASH
PAINT
INSPECT/
SHIPMENT
METAL JOINING
DIP BRAZE
BONDING
PLATING/CHEMICAL FINISH*
SYMBOLIZATION
* WATER USED IN THESE TWO OPERATIONS IS THE ONLY WATER PROCESSED THROUGH
WASTE TREATMENT.
1-8
-------
2. Materials Used or Produced
You may comply with the requirements for additional
information in either of two ways; see Section 4 of the
Guidance Manual for a detailed description of the two
approaches.
Approach A;
a. List all materials used or produced in the manufacturing
or other process generating the waste stream(s) of con-
cern. Use the correct chemical name wherever possible.
Include materials such as:
Raw materials
Intermediate products
By-products
Products
Oils and hydraulic fluids
Surface preparation materials
(solvents, acids, cleaners, surface
preparation agents, paints, etc.)
Also:
• For each material on the list, indicate whether it is
discharged to or likely to be present in the waste, and
the estimated amount entering the waste stream annual-
ly. (Specify kilograms, pounds, or similar units.)
Describe your estimation method.
For each material on the list that you do not expect to
be present in the waste, give supporting reasons for
this expectation. Supporting reasons may include mass
balance and process information. gEE
Attach Materials Safety Data Sheets (MSDS) for all
materials that are identified by trade or generic name
only and that are discharged into or likely to be
present in the waste stream.
Estimated Amount
Material Entering the Waste
Stream Annually
Sodium Hydroxide _ 6 kg _
Sodium cyanide _ .5 " _
Sodium dichromate .5
Sodium carbonate none
(Continue on additional sheets as necessary.)
1-9
-------
Item (d) continued:
Estimated Amount
Material Entering the Waste
Stream Annually
Potassium dichrornate .5 kg
Nickel metal 40 "
Nickel sulfamate 32 "
Liquid nickel chloride .6 "
Nickel acetate .8 "
Stannous sulfate .5 "
Rochelle salt none
Black dye none
Acid phosphate salts 20 "
Cadmium oxide 60 "
Copper cyanide 25
Chromic acid 12
Hydrochloric acid 30
Boric acid 12
Oxalic acid 8
Nitric acid -5
Sulfuric acid .5 "
Chromic acid, flake .2 "
Potassium sulfate none
SAE 90 gear lube none
White grease none
SAE 10W light oil " none
(MSDS's attached for the following:)
Ebonol C Special 200 "
Enbond US-35 375 "
Luster-on Utility 15 436 "
Oakite 190 56 "
Shipley Catalyst 9F 43 "
Niposit R Nickel Replenisher 7 "
Niposit Electroless Nickel 65M 8 "
NOTES: 1. Estimates of amounts of each substance in the waste
stream have been calculated using mass balances. The
calculations are available to EPA upon request.
2. Supporting calculations for why we believe certain of
these materials to be absent from the waste are
available to EPA upon request.
[Note to the reader; The Agency would request the supporting
calculations referred to above; proper procedure would be to
submit them with the original petition.]
1-10
-------
Material Safety Data Sheet
c«r USOL Safety and H«a«n Regulations
(O/ S1'CY«'<3 employment (29 CFR 1915)
U.S. Department of Ljbcr
Occupational Safety and Heaim Admmwration
OM8 NO 1218-0074
Expiration Oat* OS/31 /36
lection I
Manufacturer J Name
Shipley Company Inc.
Emergency Taieonone Numoer
(617) 969-5500
Aaaresa (Mumper. Slreet. Oly. sala. tnd ZIPCocel
2300 Washington Street
CnermcaiNeme
anoSynonym* n.a.
Newton. MA 02162
TratM Nam*
andSynonym* NIPOSIT® NICKEL REPLENISHER 65S
Cnacnical
Formua,
n.a.
Proprietary
Section II - H
TLV (Un«s) A«oy« and M«U«e
* TT.V (Un»ts|
Pigm«ms
n.a.
Catalyst
n.a.
V«OK3»
n.a.
SoNvnta
n.a.
AOOltlvM
n.a.
n.a.
BaMMatai
n.a.
Alloy*
n.a.
Metallic Coatinqa
n.a.
F««r M«iai
Pius Coating or Cor* Flux n.a.
Otrwrs
n.a.
% TUV (Umtsi
Sodiiim Hypophosphite
Ammonium Carbonate
Lead, soluble compounds" (as Pb) less than
25
18
.01
unknown
unknown
0.15
mg/m3
Section III • Ptnrtfcai Oat*
Soiling Poir* («F)
212
n.a.
n.a.
Specific Gravity (H,O-1 )
Porcant Voiaul* oy voium* (H)
Evaporatnh Ral*
•')
1 .18
n.a.
n.a.
Complete
Appearance and Ooor
Water-white liquid ammoniacal odor
Section IV - Fir* and Kiytrmten Hoard Omtm
Non-Flammable
Flammaot* Um«s
Lai
n.a.
U«t
n.a.
Water, C02, Dry Chemical
Spec* Fir* Figrmng Procaourea
None
Unusual Fir* and Expwaon Haimrta
Dried residues may be ignited or decomposed by excessive heat,
1-11
-------
2A-8b
NIPOSIT NICKEL REPLENISHER
Section V • Healtn Hasard Oau
Thresnoid t-'<™ value
0.1 mg/m3 - based on nickel
verexocsure
As for nickel
Emergency nrsl AXI Proceouies
Swallowing: Contact physician immeiately; Eye Contact: Flush with copious amounts of
water; Inhalation: Move to fresh air.
Section VI • Reectfvtty Oeta
Staouity
Unsiaoie
Suwe
X
Conanons to Avoid
inccrrpaiaoiiity tMaianais to Avoid)
Strong oxidants
Hazarcous Oecomoosmon Products
Unknown
Haiaroous
Polymerization
Mey Occur
Will Not Occur
X
Conations to Avoid
Section VII - Spin or Ue* Proceduree
Siecs to oe Tanen m Case Material is Released or Swuea
Flush with cold water
Waste Oooosai Meinod
Contact Shipley Product Services Department
Section VIN • i«
:tion Information
fl«so»aiory Protecuon (Specify Type)
n.a.
Ventilation
Local Exneost
Local Exhaust Recommended
Mecnanical (General)
Protective Gloves
Yes
Soeoal
Otter
Eye Protection
Yes
Otner Protective Eaucmem
Suitable protective clothing
Section IX • Special Precautions
Precautions to oe Taxed in Handling ana Storing
Treat as an acidic solution of nickel salts. Store in a dry area, away from strong
oxidants, at 50-90°F. Do not store in direct sunlight. Keep sealed when not in use.
Otner Precautions ~~"~~~~~~~~""~^~~~~~~~~~'"~~^~^~~~~~~~~~~~~^^~
1-12
farm CSHA-20
-------
b. Please give your assessment of the likelihood that the
processes, operations, or feed materials described above
might produce a waste stream that is not included in this
petition.
It is unlikely that the manufacturing process or the waste treat-
ment, process described could produce a waste that is not covered by
this petition. The flow diagram of the waste water treatment system
(Attachment II) shows that chromium, cyanide, and cadmium, are treated
prior to metal filtration. This system produces a sludge of uniform
composition with little variation from week to week or month to month.
Approach B:
You need not furnish any other information regarding your
facility's processes and materials. You must, however, test
your waste for additional constituents as described in Chap-
ters 4 and 6 of the Guidance Manual.
1-13
-------
CADMIUM RECOVERY SYSTEM LOCATED IN PLATING SHOP.
TREATMENT TANK IS CLOSED LOOP FLOW TO REACTOR - ALSO LOCATED IN SHOP.
FLOW FROM SECOND RINSE IS PLUMBED FROM TANK INTO CYANIDE SYSTEM.
Flow to
CADMIUM
PLATING
TREATMENT
TANK
Cyanide Treatment
Tank
RINSE
TANK
(Cd 10 ppm)
Dragout from Plating Bath to Reactor
Treated Water from Reactor back to Treatment
Attachment II
Page 1 of 5
(Closed-Loop Flow)
CADMIUM RECOVERY SYSTEM
-------
25% Sodium
Hydroxide
Waste Cyanide
Effluent
I
M
Ul
Concentrated
Sulfuric
Calcium
Hyperchlorite
& Water
Slurry
Both
pH & ORP Probes
Used in this
Stage
STAGE I
pH 9 - 11
Calcium
Hyperchlorite
& Water
Slurry
Treated
Cyanide
Both
pH & ORP Probes
Used in this
Stage
STAGE II
pH 8.5
Attachment II
Page 2 of 5
CYANIDE DESTRUCTION
-------
Waste or Concentrated
Sulfuric Acid
Sodium
Metabisulphate & Water Slurry
Waste Chromate
Effluent
STAGE I
pH 2.0 - 2.5
Treated Chromate
STAGE II
Stream
STAGE III
pH 8.0 - 9.0
CHROMATE REDUCTION
Attachment II
Page 3 of 5
-------
I
M
-J
Heavy Metals Sump
Treated Cyanide
Treated Chrome
r
' '
Final pH Adjust
Tank
pH 8.0 - 9.0*
1
ADMIX
TANK
(DE & Water)
Metal
Precipitate
PRECOAT
TANK
i
I
^
Precipitated Metals
and Admix to Filters
Attachment II
Page 4 of 5
HEAVY METALS PRECIPITATION
* pH Adjusted using Caustic or Acid as Required.
-------
Precipitated Metals
and Admix
I
i--
00
Filter*
No. 2
Filter*
No. 1
Treated
Filtered
Water
Final
Holding
Tank
Waste to
City
Automatic
Sampler
* Only one filter is operational at a time. While filter #1
is being cleaned, flow is directed to filter #2.
FILTER OPERATION
Attachment II
Page 5 of 5
-------
SECTION C: The Waste Stream
1. EPA hazardous waste number and description of waste stream
(from 261.31 or 261.32):
No. F006 Description Wastewater treatment sludge from elec-
troplating operations
Form of the waste (e.g., aqueous solution, sludge, dry solids):
Sludge ^
If the waste is a sludge, give the percent solids: 55 %
2. Estimated average and maximum monthly and annual quantities
generated: (Please use consistent units of measurement.)
Average Maximum
Monthly 22 cu yd 60 cu yd*
Annually 264 cu yd 335 cu yd
*This number is atypically high; it represents the firs.t month
that, we were required to ship our wastes.
3. This waste stream: (check all that apply)
X Is currently being generated.
X Will be generated in the future.
X Has been generated in the past and is currently
being treated/stored on site.
Has been generated in the past and is currently
being treated/stored off-site.
1-19
-------
4. Present methods of on-site storage, and amounts being stored:
Amount
Surface impoundment, NA
Evaporation pond NA
Percolation bed HA
Waste pile(s) NA
Tank(s) NA
Containers One 30 cu yd hopper
Landfill NA
Drums NA
Other (please specify)
5. Waste Management Methods:
Briefly describe:
(a) how the waste is currently managed;
(b) how it was managed before November 19, 1980; and
(c) how it will be managed if this petition is approved.
As appropriate, provide names and locations of off-site treat-
ment, storage or disposal facilities, and names and addresses
of waste transportation firms.
If the waste is treated prior to disposal, please attach a
schematic flow diagram of your present waste treatment system,
showing the processes and equipment used.
(a) The petitioner treats waste water from its Long Horn Avenue metal
finishing shop with a treatment facility that is designed to totally
reduce hexavalent chromium, destroy cyanide, and precipitate metal
oxides. In addition, the facility has recently installed a Cadmium
Recovery System which recovers cadmium oxide from the rinse tank prior
to the waste treatment process. Metal ions produced in the process
include chromium, cadmium, copper, and nickel. Cyanide is present, but
is reduced completely during the treatment process to carbon dioxide
and nitrogen gas. Precipitated metal hydroxides are filtered through a
filter precoated with diatomaceous earth (DE) and additional DE is
added during filtration to improve filterability; this process occurs
during treatment. The sludge is thus composed of DE primarily, and
0.04 to 1.0 percent metal oxides. (See Attachment II.)
1-20
-------
The current disposal method used for the sludge employs the
following offsite Subtitle C facility:
Rolling Haulers
2300 Fieldcrest Road
Deer Crossing, TX 77556
(b) Prior to November 19, 1980, the waste sludge was disposed of at:
Dallas Municipal Landfill
Walnut Hill Road
Dallas, TX 75266
(c) Upon reclassification, the sludge will once again be disposed of
at the Dallas Municipal Landfill.
1-21
-------
SECTION D: Selection of Constituents for Testing
The procedures described below apply to all types of wastes
other than those from petroleum refineries and multiple waste
treatment facilities. Petitioners for these facilities should
refer to Section 4 of the Guidance Manual and adapt this
section of the petition appropriately.
1. If you have followed Approach A in Section B above, please
submit test results on representative samples for the follow-
ing:
• The specific hazardous constituents for which the
waste was listed (i.e., total concentration of each
listed constituent found in Appendix VII of Part
261);
• The four hazardous waste characteristics (but see the
Note immediately below);
• Appropriate leachate tests for the EP toxic metals,
nickel, and cyanide;
• Total concentrations of the EP toxic metals and
nickel;
• Total organic carbon (TOC); and
• Total oil and grease.
Note; If you can explain why the waste cannot exhibit one or
more of the four hazardous waste characteristics, you may
submit your rationale in lieu of test results for those char-
acteristics. For example, if the waste is composed exclusive-
ly of organic solvents and there is no chance (on the basis of
process considerations) that it contains any of the EP toxi-
cants, you need not test for the EP Toxicity characteristic.
You may omit the rest of this section and go to Part E.
2. If you have opted for Approach B in Section B above, then you
must perform the tests specified in the above paragraph, and
you should test for all hazardous constituents that may "rea-
sonably be expected" to be in the waste, whether or not they
were used as a basis for listing.
The remainder of this section is to be used to support your
decision regarding which constituents to test for.
1-22
-------
a. List the constituents (from Appendix VIII to Part 261)
that may reasonably be expected to be in the waste. De-
scribe the engineering, chemical, or other considerations
that support your choice.
Constituent: None
Reasons for Selection:
Although several Appendix VI11 constituents are included in
our materials listings, we believe that mass balance considera-
tions render these substances absent from the waste stream.
Therefore, it is unreasonable to expect their occurrence in the
waste.
(Repeat as necessary.)
[Mote to the reader; The Agency would request the supporting
calculations referred to above; proper procedure would be to
submit them with the original petition.]
b. For each of the remaining hazardous constituents (or
groups of constituents) in Appendix VIII of Part 261,
specify why it may not reasonably be expected to occur in
the waste stream.
Constituent (or group of constituents): See above
Reasons for non-occurence: See above
(Repeat as necessary.)
1-23
-------
SECTION E: Sampling and Testing the Waste
The purpose of the data requested below is to demonstrate that
representative samples of the waste stream:
a. Do not exhibit any of the criteria (e.g., hazardous waste
characteristics or constituents) for which the waste was
listed, and
b. Do not exhibit any other criteria that could cause it to
be listed.
Additional information is also requested as a check on the test
results. Refer to the accompanying Guidance Manual for instruc-
tions on developing a sampling plan (Chapter 7), selecting proper
test methods, (Chapter 8) and presenting the test results (Chapter
9).
1. General Information
a. Name and address of the laboratory facility performing the
sampling [260.22(1)(1)]:
Name
Street
City State Zip
Telephone: ( ) -
If sampling was done by in-house staff, check here:
For each individual person who (a) designed the sampling
plan or (B~)collected samples, please provide the follow-
ing information and attach a resume or other statement of
qualifications [260.22(i) (2) ].
Name Susan Smith
Affiliation ABC Industries, Inc.
Title Process Engineer
(resume attached)
(Repeat as necessary.)
1-24
-------
Susan Smith
24 Green Street
Dallas, Texas 75206
Education
August 1975 - May 1979
University of Missouri - Columbia,
B.S. Chemical Engineering
G.P.A. 2.75/4.0
Work Experience
June 1979 - May 1980
May 1980 - June 1981
June 1981 - Present
ABC Amalgamated Industries, Inc.
Optics Department - set up process
documentation and process control
procedures for optics fabrication.
ABC Amalgamated Industries, Inc.
Process Engineering - provide pro-
cess support for organic coating
area. Evaluate new coating mate-
rials, procedures.
ABC Amalgamated Industries, Inc.
Process Engineering - support waste
treatment/chemical finishing, plat-
ing operations. Maintain data on
waste treat system, documents for
solid waste disposal, and applicable
permits. Technical support for
plating shop and waste treatment.
Perform troubleshooting and new sys-
tem evaluations.
1-25
-------
b. Name and address of the laboratory facility performing the
testing, if different from the sampling laboratory
[260.22(1)(1)]:
Name
Street
City State Zip
Telephone: ( ) -
If testing was done by in-house staff, check here: X
For each individual person who (a) designed the testing
plan or (b) performed tests, please provide the following
information and attach a resume or other statement of
qualifications [260.22(1) (2) ].
Name Thomas Roberts
Affiliation ABC Indus-tries, Inc.
Title Engineering Analyst
(resume attached)
(Repeat as necessary.)
1-26
-------
Thomas Roberts
29 Turner Street
Lewisville, Texas 75067
Education
1972 - 1974
St. Louis University - St. Louis/ MO
Courses taken included, but were not limited
to, Chemistry 101 and 102, Quantitative
Analysis (with emphasis on atomic absorption
analysis), Organic Chemistry, Physical
Chemistry and Biology 101 and 102.
1982
Lancerette Laboratories
Received Certification for both flame and
flameless atomic absorption spectrophotometry
on the Instrumentation laboratory 551 video
spectrophotometer.
Work History
1972 - 1974
U.S. Army Corps of Engineers, Water Quality
Lab, Foot of Arsenal Street - St. Louis, MO
Work included sampling and analysisi of Corps
controlled bodies of water in the Missouri
and Illinois districts. Analysis included
wet chemistries as well as atomic absorption
and biological testing.
1974 - 1978
1978 - 1980
Washington University, Department of Pediatrics
- St. Louis, MO
Hematology and Oncology research and routing
clinical testing of cancer patients on drug
therapy.
Enreglory Engineering, Inc.
Analysis Laboratory - work on the effluent
guidelines project 1434 and 1444 and RCRA for
the EPA.
Duties included metals analysis by atomic
absorption, phenolics, cyanides and pesti-
cides and other analysis.
1-27
-------
Tom Roberts
Page 2
Work History - (Continued)
1980 - Present ABC Amalgamated Industries, Inc.
Process Engineering Lab - Senior Technician in
research, routine evaluations, plating,
wastewater, sludge analysis and training of
technical personnel in the use of atomic
absorption spectrophotometry.
1-28
-------
c. Describe the sampling strategy you followed to insure that
the samples were representative [260.22(i) (9)]. Please
address specifically:
• the variation of the waste stream over time; and
• the variation of the waste stream in space.
All waste stream outflows or storage locations to which
this petition applies must be sampled. The Delisting
Petition Guidance Manual (see Instructions to this form)
gives directions for developing a sampling plan.
Time-composite sampling was used, with an interval that coin-
cided with each dumping of the filter cake from the filter press.
This averaged three times per week.
Each time that a filter was dumped into the small (1.5 cu yd)
hopper (see Attachment III) the waste treatment operator notified
the Process Engineer*. The Process Engineer then put on a neoprene
glove and collected four samples from the hopper using a trier.
Sample locations were selected by dividing the hopper horizontally
into quadrants and taking one sample from the centroid of each
quadrant. The samples, approximately twenty grams each, were then
stored in heavy-walled plastic bags and sealed to main-tain fresh-
ness. At the end of each week, equal weight samples were taken
from the individual bags to compile the composite 100 gram sample,
which was then used for the leachate test.
The small hopper is emptied into the larger (30 cu yd) hopper
following each filter dump.
d. State whether the Chain of Custody procedures in Section
1.3 of SW-846 were followed. Please describe any devia-
tions from those procedures and the reasons for them.
All chain-of-custody procedures as outlined in Section 1.3 of
SW-846 were followed.
1-29
-------
NOTE: After each filter was dumped into the
hopper, four samples were obtained, the
waste was then emptied into a larger
30 yd-* hopper, and the process repeated
3 to 4 times per week.
1 .5 CUBIC YARD CAPACITY
I
u>
o
Tilts 40 Below Horizontal
Safety Latch
36'
Fork Lift
Insert Here
Restraining Bar
Attachment III
Skid or Caster Assembly to be
Mounted for Increased Mobility under Filters
-------
2. Sample-Specific Information
For each individual sample, please furnish the information
requested in the form on the following page. The notes below
refer to those items on the form that are not self-explana-
tory. The Guidance Manual contains additional instructions.
Notes
Item f, "Parameter/Constituent Tested For": Enter the hazardous
waste characteristic or constituent that was the subject
of the test.
Item i, "Test Method and Source": See Chapter 8 of the Guidance
Manual for a listing of applicable test methods. Sources
for test methods may be designated by number, as follows:
1. "Test Methods for Evaluating Solid Waste:
Physical/Chemical Methods," EPA SW-846 (second
edition), July, 1982, and supplements.
2. "Methods for the Evaluation of Water and
Wastewater," EPA 600 14-79-020, March, 1979.
3. "Standard Methods for the Examination of Water
and Wastewater," (14th Edition).
4. Appendix J of the Guidance Manual
Item j, "Sample Workup or Preparation Method": See Section Four
of Reference 1 above.
Item 1, "Test Results": Enter concentrations in mg/1, ppm, etc.
as appropriate.
1-31
-------
Sample Number:
Sampling Information;
a. Sampling location: The 1.5 cu yd hopper
b. Person(s) who drew the sample: Susan Smith
c. Equipment used for drawing the sample: Trier
Daily at 9:00 a.m.
d. Date and time when the sample was drawn: 10/4 /82, PTHH-
to 10/8/82
e. Handling, containerization, and preservation techniques used:
Daily samples were combined & mixed to get a weekly composite.
Composites were stored in sealed, heavy-weight plastic bags.
Test Procedures and Results; (Repeat for each test conducted)
f. Parameter/Constituent Tested For: All EP metals. Hi, Cu, Zn,
Total cyanide
g. Date Test Performed: 10/12 /82
h. Person(s) who performed the test: Thomas Roberts
i. Test Method (or Number) and Source: see Summary Table
j. Sample Workup or Preparation Method: see Summary Table
k. Equipment: Name Model Number
Perkin-Elmer 603
Perkin-Elmer 406
Bausch & Lomb Sectronic 23
Perkin-Elmer 54B
Instrumentation Laboratories 251
Atomic Absorption Spectrophotometer
1. Test Results: see Attachment IV
1-32
-------
Sample Number:
Sampling Information;
a. Sampling location: The 1.5 cu yd hopper
b. Person(s) who drew the sample: Susan Smith
c. Equipment used for drawing the sample: Trier
Daily at 9:00 a.m.
d. Date and time when the sample was drawn: 10/11/82,
to 10/15/82
e. Handling, containerization, and preservation techniques used:
Daily samples were combined & mixed to get a weekly composite.
Composites were stored in sealed, heavy-weight plastic bags.
Test Procedures and Results; (Repeat for each test conducted)
f. Parameter/Constituent Tested For: All EP metals, Ni, Cuf Zn,
Total cyanide
g. Date Test Performed: 10/19 /82
h. Person(s) who performed the test: Thomas Roberts
i. Test Method (or Number) and Source: see Summary Table
j. Sample Workup or Preparation Method: see Summary Table
k. Equipment: Name Model Number
Perkin-Elmer 603
Perkin-Elmer 406
Bausch & Lomb Sectronic 23
Perkin-Elmer 54B
Instrumentation Laboratories 251
Atomic Absorption Spectrophotometer
1. Test Results: see Attachment V
1-33
-------
Sample Number:
Sampling Information;
a. Sampling location: The 1.5 cu yd hopper
b. Person(s) who drew the sample: Susan Smith
c. Equipment used for drawing the sample: Trier
Daily at 9:00 a.m.
d. Date and time when the sample was drawn: 10/18/82, PTHH-
to 10/22/82
e. Handling, containerization, and preservation techniques used:
Daily samples were combined & mixed to get a weekly composite.
Composites were stored in sealed, heavy-weight plastic bags.
Test Procedures and Results; (Repeat for each test conducted)
f. Parameter/Constituent Tested For: All EP metals, Hi, Cu, Zn,
Total cyanide
g. Date Test Performed: 10/26 /82
h. Person(s) who performed the test: Thomas Roberts
i. Test Method (or Number) and Source: see Summary Table
j. Sample Workup or Preparation Method; see S'i"""ary Table
k. Equipment: Name Model Number
Perkin-Elmer 603
Perkin-Elmer 406
Bausch & Lomb Sectronic 23
Perkin-Elmer 54B
Instrumentation Laboratories 251
Atomic Absorption Spectrophotometer
1. Test Results: see Attachment VI
1-34
-------
Sample Number:
Sampling Information;
a. Sampling location: The 1.5 cu yd hopper
b. Person(s) who drew the sample: Susan Smith
c. Equipment used for drawing the sample: Trier
Daily at 9:00 a.m.
d. Date and time when the sample was drawn: 10/25/82, p-r»r
to 10/29/82
e. Handling, containerization, and preservation techniques used:
Daily samples were combined & mixed to get a weekly composite.
Composites were stored in sealed, heavy-weight plastic bags.
Test Procedures and Results; (Repeat for each test conducted)
f. Parameter/Constituent Tested For: All EP metals. Hi, Cu, Zn,
Total cyanide
g. Date Test Performed: ll/ 2 /82
h. Person(s) who performed the test: Thomas Roberts
i. Test Method (or Number) and Source: see Summary Table
j. Sample Workup or Preparation Method: see Summary Table
k. Equipment: Name Model Number
Perkin-Elmer 603
Perkin-Elmer 406
Bausch & Lomb Sectronic 23
Perkin-Elmer 54B
Instrumentation Laboratories 251
Atomic Absorption Spectrophotometer
1. Test Results: see Attachment VII
1-35
-------
3. Summary Table of Analytical Results
For each sample, please enter the Test Results from Item 2
above onto the form contained in the following pages.
4. Analytical Discussion
Please furnish explanations or additional information on the
following topics as necessary:
a. Inconsistencies or deviations in the analytical results
presented above.
b. Additional reasons as to why the waste stream should be
delisted.
1-36
-------
Summary Table
Analytical Methods Used;
Arsenic
Barium
Cadmium
Chromium (tot..)
Lead
Mercury
Selenium
Silver
Nickel
Cyanide (tot.)
TOC
Oil & Grease
Workup
1310
1310
1310
1310
1310
1310
1310
1310
1310
Analysis
7060
7080
7130
7190
7420
7470
7740
7760
7520
9010
502D
415.1
1-37
-------
SUMMARY OF TEST RESULTS
I
u>
00
Sample Number:
Sampling Location:
Date Sample Taken:
1 . Ignitability
Liquids Flash point
Non- liquids Spontaneous
combustion
Compressed Flammability
Gas
Oxidizer Oxygen yield
2. Corrosivity pH
Corrosivity
towards steel
3. Reactivity Violent chemical
change
Reacts violently
with water
Water-reactive;
explosive
1
1.5 cu yd
hopper
Oct 4-8 '62
2
I . 5 cu yd
hopper
Oct 11-15
3
1 . b cu yd
hopper
Oct 18-22
4
1.5 cu yd
hopper
Oct 25-29
-------
SUMMARY OP TEST RESULTS (Continued)
I
u>
vo
Sample Number:
3. Reactivity Water-reactive;
(Cont.) toxic gases,
vapors , fumes
Cyanide or sulfur-
bearing wastes
which, when exposed
to acidic/basic
conditions, gen-
erate toxic gases,
vapors, or fumes
Explosive when
subjected to
force or heat
Explosive at stan-
dard temperature
and pressure
DOT explosive
4. Total Arsenic
Metals
(Complete Barium
Acid
Digestion) Cadmium
Chromium
-------
SUMMARY OF TEST RESULTS (Continued)
Sample Number :
4 . Total Lead
Metals
(cont.) Mercury
Selenium
Silver
Nickel
5. EP Toxicity Arsenic
— Metals
Barium
Cadmium
Chromium
Lead
Mercury
Selenium
Silver
Nickel
1
.11 ug/l
.01
.06
.05*
.05*
.05
.01
.01*
2.00
2
1.0
0.3
0.12
.05*
.01*
.05
.02
.01*
1.00
3
1.0
0.3
0.12
.05*
.01*
.05
.02
.01*
0.11
4
1.0
0.2
0.18
.05*
.01*
.05
.02
.01*
0.58
*Less than
-------
SUMMARY OF TEST RESULTS (Continued)
Sample Number:
6 . EP Toxicity Arsenic
— Metals;
Oily Waste Barium
Methods*
Cadmium
Chromium
Lead
Mercury
Selenium
Silver
Nickel
7. EP Toxicity Endrin
— Pesticides
Lindane
Methoxychlor
Toxaphene
8. EP Toxicity 2,4-D
— Herbicides
2,4,5-TP (Silvex)
*For wastes containing greater than 1% total oil and grease,
-------
SUMMARY OF TEST RESULTS (Continued)
I
^
to
9. EP Toxicity
— Organics
Sample Number:
10. Total Organ-
ic Carbon
11. Oi 1 and
Grease
12. Cyanide
13. Other
Total
Free
Extraction
procedure
Photodegradable
Appendix VIII
constituents
(Add sheets as
necessary)
1
0.8 ppm
0.01 ppm
2
1.0
0.18
3
0.9
0.07
4
0.9
0.18
-------
Quality Assurance and Quality Control
a. For inorganic substances, describe the procedures used for
Standard Additions Analysis. Provide the following for
each substance tested:
SEE ATTACHED SHEETS
Spike Recovery Percent
Substance Concentration Concentration Recovery
For organic substances, describe the procedures used for
analysis of spiked samples. For each substance tested,
provide the information requested in the following table.
Also, describe in writing the procedures used to cali-
brate the analytical equipment.
Substance Surrogate, Spike Recovery Percent
Tested For if any Cone. Cone. Recovery
Describe any other QA/QC measures followed in regard to
the sampling and analysis procedures.
1-43
-------
STANDARD ADDITION ANALYSIS FOR WEEK 1
Attachment IV (cont.)
Concentration
Cr
0.00 mg/1
Concentration
Cd
=0.06 mg/1
3
2
1
0
-1
-2
-3
ABS
0.0000
0.0040
0.0080
0.0160
.005
.01
CONG
0.000
0.500
1.000
2.000
.015
3
2
1
0
-1
-2
-3
ABS
0.0060
0.0350
0.0650
0.1270
CONC
0.000
0.500
1 .000
2.000
.02
.06
.12
.18
Concentration =0.05 mg/1
Pb
Concentration
Ni
2.00 mg/1
.3
2
0
.1
.2
.3
ABS
0.0040
0.0160
0.0220
.006
.012
CONC
0.000
0.100
0.200
.018
6
4
2
0
-2
-4 _
-6 _
.024 0
> — l*^ '
^^ ABS
0.0140
0.0210
0.0350
0.0490
CONC
0.000
1 .000
3.000
5.00
.015
.03
.045
1-44
-------
6
4
2 .
0
-2
-4
-6 L
STANDARD ADDITION ANALYSIS FOR WEEK 1 (cent.)
Attachment IV (cont.)
Concentration = 0.00 mg/1
Cu
ABS
0.000
0.020
0.040
0.050
.02
.04
CONG
0.000
1 .000
2.000
3.000
.06
-2 ,.
-.8 _
-1.2
Concentration
Zn
=0.38 mg/1
ABS
0.0220
0.0430
0.0530
0.0830
.08
.025
.05
CONC
0.000
0.300
0.500
1.000
.075
1.5
1.0
.5
Concentration = 0.00 mg/1
Ag
-.5
1.0
1 .5
0
0
0
0
.
ABS
.0000
.0090
.0200
.0290
CONC
0.000
0.500
1 .000
1.500
.008
.016
.024
.032
1-45
-------
ORGANIC WASTESTREAM
OPTIONAL FORM:
DELISTING PETITION FOR WASTE STREAM
K027 — Centrifuge and Distillation Residues from Toluene
Diisocyanate Production
Submitted by:
Nayblor Chemical Corporation
Ardmore Boulevard
Pittsburgh, PA 15208
Date:
April 15, 1982
1-47
-------
4. Description and Justification for the Proposed Action
Please describe briefly the proposed delisting action, why it
is needed, and how it will affect your operation. Describe
why you believe that the waste stream of concern (a) is not
hazardous for the reasons it was originally listed and (b)
contains no other constituents or characteristics that render
it hazardous as defined in 40 CFR 261. [260 . 20(b) ( 2 ) , (3) and
(4)]
Mayblor Chemical Corporation proposes to exclude EPA Hazardous Waste No.
K027, Centrifuge and distillation residues from toluene diisocyanate
production, from Subpart D, 40 CFR 261.32. This residue was listed by
EPA as a hazardous waste from a specific source because the residue was
considered reactive (R) and toxic (T). Mayblor 's process currently
produces this residue in such a manner that it eliminates the residue ' s
characteristics of reactivity and toxicity. Additional testing by May-
blor indicates that the residue contains no other constituents or charac-
teristics that render it hazardous as defined in 40 CFR 261.
The need for the proposed action is to relieve Mayblor of the burden and
cost of disposing of this residue. The proposed action will affect
Mayblor 's operations by allowing for the marketing of the processed
residue as a supplemental fuel for steam and/or electrical generating
plants. In addition to these benefits, scarce landfill capacity will not
be utilized by a material with definite resource recovery potential.
5. Certification of Accuracy and Responsibility [260. 22 (i) (12) ]
I certify under penalty of law that I have personally examined
and am familiar with the information submitted in this demon-
stration and all attached documents, and that based on my
inquiry of those individuals immediately responsible for ob-
taining the information, I believe that the submitted informa-
tion is true, accurate, and complete. I am aware that there
are significant penalties for submitting false information,
including the possibility of fine and imprisonment.
Signed,
Waste Generator, Title or
Authorized Representative*
of Waste Generator, Title
*Hote: An "authorized representative" is a person respon-
sible for the overall operation of a facility or an opera-
tional unit (for example, a plant manager, superintendent,
or person of equivalent responsibility). Consultants or
other outside parties may not sign the certification state-
ment.
1-49
-------
SECTION B: Production Processes
1. Description of Manufacturing Processes and Other Operations
[260.22(i)(5)].
a. Please provide a brief description of the on-site
manufacturing/generating process(es) that produce the
waste stream. Include descriptions of major equipment
items and production lines. Also, describe the stages of
the typical operating cycle (e.g., startup, steady-state
operation, cleaning and maintenance) on a daily, weekly,
or other basis as appropriate.
Toluene diisocyanate (TDI) distillation residues are isolated
during the distillation of TDI from the by-product higher-molecular-
weight polymers that are formed during the reaction of toluene diamine
(TDA) with phosgene. This reaction produces the product TDI.
Mayblor Chemical's process as described above is generally
represented by the schematic and process description given in EPA's
"Listing Background Document: Toluene Diisocyanate Production."
A more detailed explanation of the process and associated equipment
has been supplied to EPA. Because of its confidential nature this
description is not included in the public record file.
b. Please provide a description of all surface and equipment
preparation, cleaning, degreasing, coating or painting
processes used in your facility that you have not
described in (a) above.
See above.
Attach a schematic diagram of all manufacturing processes,
surface preparation, cleaning, and other operations that
may provide influent into the waste stream.
See above.
1-50
-------
2. Materials Used or Produced
You may comply with the requirements for additional
information in either of two ways; see Section 4 of the
Guidance Manual for a detailed description of the two
approaches.
Approach A;
a. List all materials used or produced in the manufacturing
or, other process generating the waste stream(s) of con-
cern. Use the correct chemical name wherever possible.
Include materials such as:
Raw materials
Intermediate products
By-products
Products
Oils and hydraulic fluids
Surface preparation materials
(solvents, acids, cleaners, surface
preparation agents, paints, etc.)
Also:
o For each material on the list, indicate whether it is
discharged to or likely to be present in the waste, and
the estimated amount entering the waste stream annual-
ly. (Specify kilograms, pounds, or similar units.)
o For each material on the list that you do not expect to
be present in the waste, give supporting reasons for
this expectation. Supporting reasons may include mass
balance and process information. OWR NOTES
Attach Materials Safety Data Sheets (MSDS) for all
materials that are identified by trade or generic name
only and that are discharged into or likely to be
present in the waste stream.
Estimated Amount
Material Entering the Waste
Stream Annually
Tolaene-2 , 4-diaau.ne none
2,6-Toluene-diamine none
o-Dichlorobenz ene none
1
gaseous phosgene none
2
Toluene diisocyanate none
1-51
-------
NOTES TO MATERIALS LIST
1. These materials are completely consumed in the TDI production
process, and therefore do not appear in the waste stream.
2. TDI is the process end-product. Analytical tests indicate
that it is undetectable in the waste (see Section E below).
1-52
-------
b. Please give your assessment of the likelihood that the
processes, operations, or feed materials described above
might produce a waste stream that is not included in this
petition.
The waste-generating operation is carried out in a completely
closed process. All inputs and outputs nave been identified. There-
fore, it is highly unlikely that a waste stream not included in this
petition would be produced from the processes, operations and feed
materials described above.
Approach B;
You need not furnish any other information regarding your
facility's processes and materials. You must, however, test
your waste for additional constituents as described in Chap-
ters 4 and 6 of the Guidance Manual.
1-53
-------
SECTION C: The Waste Stream
1. EPA hazardous waste number and description of waste stream
(from 261.31 or 261.32):
No. K027 Description Centrifuge and distillation residues
from toluene diisocyanate production
Form of the waste (e.g., aqueous solution, sludge, dry solids)
Sludge
If the waste is a sludge, give the percent solids: 80 %
2. Estimated average and maximum monthly and annual quantities
generated: (Please use consistent units of measurement.)
Average Maximum
Monthly 300 tons 550 tons
Annually 3600 tons 6600 tons
3. This waste stream: (check all that apply)
X Is currently being generated.
X Will be generated in the future.
X Has been generated in the past and is currently
being treated/stored on-site.
Has been generated in the past and is currently
being treated/stored off-site.
1-54
-------
4. Present methods of on-site storage, and amounts being stored:
Amount
Surface impoundment,
Evaporation pond
Percolation bed
Waste pile(s)
Tank(s)
Containers
Landfill
Drums
NA
NA
NA
NA
NA
Less than or equal to 550 tons
NA
NA
Other (please specify)
5. Waste Management Methods:
Briefly describe:
(a) how the waste is currently managed;
(b) how it was managed before November 19, 1980; and
(c) how it will be managed if this petition is approved.
As appropriate, provide names and locations of off-site treat-
ment, storage or disposal facilities, and names and addresses
of waste transportation firms.
If the waste is treated prior to disposal, please attach a
schematic flow diagram of your present waste treatment system,
showing the processes and equipment used.
a) The waste is currently held on-site in large, covered containers
until our contracted hauler arrives on the twentieth of each month.
The hauler then delivers the residue to either a fuel burning
facility (with interim storage and staging) or, more often, to a
properly permitted landfill.
Hauler: ABC Trucking & Hauling
22 Dalean Avenue
Thurston, PA
Landfill: XYZ Landfill
102 Lancer Street
Sewickley, PA
Fuel burners: Steam Generators, Inc.
2 Tavern Lane
Thurston, PA
1-55
-------
b) Prior to November 19, 1980, the treated residue was shipped solely
to Steam Generators, Inc. for resource recovery.
c) If this petition is approved, we shall employ resource recovery to
the largest extent possible to manage the residue.
Attachment I: Toluene Diisocyanate Production Schematic — includes
diagram of present waste system, showing processes and
equipment used. A more detailed explanation of the process
and associated equipment has been supplied to EPA. Be-
cause of its confidential nature, this description is not
included in the public record file.
1-56
-------
Attachment I
TOLUENE DIISOCYANATE PRODUCTION SCHEMATIC
Toluene
Diamine
Phosgenation
Crude
TDI
Product Toluene Diisocyanate
Primary
Distillation
TDI
Secondary
Distallation
Phosgene
Residue
Resource
Recovery
Disposal
Deactivation
Polishing
Step
(2)
Residue
Deactivation
^
1-57
-------
SECTION D: Selection of Constituents for Testing
The procedures described below apply to all types of wastes
other than those from petroleum refineries and multiple waste
treatment facilities. Petitioners for these facilities should
refer to Section 4 of the Guidance Manual and adapt this
section of the petition appropriately.
1. If you have followed Approach A in Section B above, please
submit test results on representative samples for the follow-
ing:
• The specific hazardous constituents for which the
waste was listed (i.e., total concentration of each
listed constituent found in Appendix VII of Part
261);
• The four hazardous waste characteristics (but see the
Note immediately below);
• Appropriate leachate tests for the EP toxic metals,
nickel, and cyanide;
• Total concentrations of the EP toxic metals and
nickel;
• Total organic carbon (TOG); and
• Total oil and grease.
Note; If you can explain why the waste cannot exhibit one or
more of the four hazardous waste characteristics, you may
submit your rationale in lieu of test results for those char-
acteristics. For example, if the waste is composed exclusive-
ly of organic solvents and there is no chance (on the basis of
process considerations) that it contains any of the EP toxi-
cants, you need not test for the EP Toxicity characteristic.
You may omit the rest of this section and go to Part E.
2. If you have opted for Approach B in Section B above, then you
must perform the tests specified in the above paragraph, and
you should test for all hazardous constituents that may "rea-
sonably be expected" to be in the waste, whether or not they
were used as a basis for listing.
The remainder of this section is to be used to support your
decision regarding which constituents to test for.
1-58
-------
List the constituents (from Appendix VIII to Part 261)
that may reasonably be expected to be in the waste. De-
scribe the engineering, chemical, or other considerations
that support your choice.
Constituent: Toluene diisocyanate
Reasons for Selection:
. This is the only Appendix VIII constituent that is not
totally consumed in the production process.
(Repeat as necessary.)
b. For each of the remaining hazardous constituents (or
groups of constituents) in Appendix VIII of Part 261,
specify why it may not reasonably be expected to occur in
the waste stream.
Constituent (or group of constituents): All others
Reasons for non-occurence:
All Appendix VIII constituents except for TDI are completely
consumed in the closed production process.
(Repeat as necesssary.)
1-59
-------
Sample Number:
Sampling Information;
a. Sampling location: Reaction container
b. Person(s) who drew the sample: T. Hugent
c. Equipment used for drawing the sample: grain sampler
a.m.
d. Date and time when the sample was drawn: 3 / 1/82, 7
e. Handling, containerization, and preservation techniques used:
Sampling container was immediately capped, labelled and _
sealed. Sample was then immediately delivered to the _
laboratory .
Test Procedures and Results ; (Repeat for each test conducted)
f . Parameter/Constituent Tested Fors Toluene diisocyanate _
g. Date Test Performed: 3/5 /82
h. Person(s) who performed the test: Barney Kessel _
i. Test Method (or Number) and Source: 9O10, SW-846 _
j. Sample Workup or Preparation Methods As in (i) above _
k. Equipment: Name Model Number
Perfcin Elmer Model 5000
1. Test Results: Not detectable
1-60
-------
3. Summary Table of Analytical Results
For each sample, please enter the Test Results from Item 2
above onto the form contained in the following pages.
4. Analytical Discussion
Please furnish explanations or additional information on the
following topics as necessary:
a. Inconsistencies or deviations in the analytical results
presented above.
b. Additional reasons as to why the waste stream should be
delisted.
The attached material from the International Isocyanate Institute, Inc.
comprises our additional reasons for delisting this waste.
1-61
-------
INTERNATIONAL SSOCYANATE SNSTITUTE. INC.
P.O. ec* !268
71 ELM Srntrr
NCW C'XAAW, COMM.
CABLE
ISOC'f AN».TI-NCW CANAAN. CONN. (2O3i 966-73SS
July 16, 1930
Docket Clerk (Docket No. 3000)
Office of Solid Waste (WH-562)
United States Environmental Protection Agency
401 M Street, S.W.
Washington, D. C. 20460
Dear Sir;
The following comments have been prepared by the International Isocyanat
Institute (III) regarding the Hazardous Waste Management System Part 251
Indentification and Listing of Hazardous Waste, Subpart D - List of
Hazardous Waste as published in the May 19, 1980 Federal Register
(Vol. 45 No. 98). Specifically the III would like to offer comments on
the listing of centrifuge residue from toluene diisocyanate production
(Section 261.32 EPA Hazardous Waste No. K-027) and on the listing of
Urethane (Section 261.33 of EPA Hazardous Waste No. U-238)."
The International Isocyanate Institute, Inc., was four.ded August 18. IS",
as a non-profit Corporation. It is organized under the laws of the
United States and is registered in the State of New York. As presently
constituted, the Institute has 22 members who are located in tne Americ;
Europe and Japan. To qualify for Membership, a company ccust be engaged
in the manufacture of Isocyanates. A list cf the present Member Compan
will be found on the last page of thi^ submission.
/
Centrifuge/residue from toluene tliisocyanata production has been designa
as hazardous waste No. K-027 in Section 261.32 of the May 19th, 1980
Federal Register Regulations. The EPA listed both toxicity and raactiv
as the properties that allegedly qualify this material for inclusion or
the list.Examination of the listing background docunent (Document #11
pp 431-432) produces several questions relative to the accuracy of this
data, and therefore, the validity of the hazardous waste designation,.
The following comments are offered for the Agency's consideration rela;
to the listing of TDI centrifuge residue as a hazardous waste:
1-62
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I. The EPA characterizes the waste from TDI production as centrifuge
residues in the Federal Register while the background document makes
reference to "Evaporator residue processing centrifuge or vacuum dis-
tillation." It is unclear if the Agency intends to limit the scope of
the listed material to only the wastes generated via a centrifuge
unit operation.
1. In general, each TDI producer deactiv/ac-33 T13I residue differently
am! each firm does employ some foria of aging or ?ther means ~f ca-
activation after generation ot" t'~;e final cist:".!lotion cr centrifuge
bottoms. The III believes <':he lire ing cf TI?I residue n^eds furtner
clirifi. sf'.on that it is limited ".c, cnce.-icuiv/ar.eJ c;at^.rial a* it is
directly discharged from the 'Jistillatirr- cr centrifuge unir. operation
and not de-activated materials..
If a TDI producer ciec":-' to include additional processing steps
(i. 2. hydrolysis, additional JistiJ.lar.ior,, aging, etc.) tc render the
material less reactive or non-reactive the;- the resultant material
should be evaluated again3" tha criteria found in Sub-part C-
Characteristics of Hazardous Warr.'i 261.20 - £bl./M.
3. The background document indicates -he centrifuge residue (contains
toxic organic substances, mutagenic substances and substances that are
probably carcinogenic". It' further states that toluene diisocyanate,
toluene diamine and polymeric tars ara "suspected carcinogens".
These statements raise several questions:
(a) It has not been documented that all centrifuge residue contains
toluene diamine. In general, companies indicate that either TDA is not
present or if present it is only in low ppm concentrations. The analytical
techniques used to conduct this determination are subject to variability
and are currently being evaluated by industry.
(b) Although the Federal Register (Appendix VII of the Hay_ 19, 1980
publication - basis for. listing hazardous wastes) sites benzidimidazapone as
the principal compound in tars, we are not aware cf the-existence of this
substance and any data'that exists tc substantiate the claim that it is
mutagenic or carcinogenic.
(c) TDI has not been declared a suspect carcinogen. In che illOSII
Criteria for a Recommended Staadar-i...Occupational Exposure tc Diisocyanates
published in September 1978., there is the statement "Nc reports were
found to indicate that TDI, MDI, HDI, JDI, or otrer ciisocyanates produce
carcinogenic, teratogenic, or raproductive effects in hucans or animals."
The Isocyanates as a class of compounds are net listed in the 03HA
proposed carcinogen regulations.
1-63
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(d) Only the meta-isomer of TDA is a suspect carcinogen.
4. Disposition of raw centrifuge residue in drum quantities in a'
landfill is- generally not practiced as a "known management method
for'this waste."
Therefore, on the basis of apparent inaccuracies in che background
document, the III respectfully requests the EPA to review and
clarify its data and information based on the items enumerated in
this correspondence.
On another matter, the EPA designates urethane as a commercial chemical
product or manufacturing intermediate (Section 261.33f) that will be
subjected to the Hazardous Waste Regulations. (An examination of the
"Urethane" terminology reveals that this term was improperly applied
in 1960.)
It is most imperative that this gross misnomer be corrected. Twenty
years ago Hueper published a paper (W.C. Hueper. Experimental Productici
of Cancer by Means of Implanted Polyurathane Plastic, Ar.er .Jour. Clin. ?a
34: p.334-337, October I960) - Hueper's work and subsequent work by the
National Cancer Institute was with etnyl carbaniate (urethan* which he
erroneously thought was synonymous with "urethane". In spite of con-
siderable effort on the part of some of us to correct this misnomer
(wnich is even perpetuated by the 1973 Toxic Substances List, No.5015),
polyurethanes continue to be associated with the known human carcinogen
ethyl carbamate or "urethan".
In view of the name similarity of. urethan (ethyl carbamate) and
polyurethane plastics, it is important to point out the differences
in chemical structure of both compositions in order to avoid
confusion.
It is readily apparent that urethan (ethyl carbamate) is not a precurso1
of the polyurethanes. Thus there is no basis for assuming that any tox
city characteristics associated with ethyl carbamate in any way appl;
to the polyurethanes.
The III respectfully requests that to clarify this ambiguity, the EPA
replace urethane (hazardous waste No. U-238 with the proper chemical
terminology - ethyl carbamate.
We would welcome an opportunity to discuss this matter further with you
or other appropriate EPA personnel. If you have any questions or comm
regarding this issue, please do not hesitate to call me.
Sincerely,
Arthur B. Chivvis
Managing Director
ABC:vor
1-64
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APPENDIX J
TEST METHODS NOT AVAILABLE IN SW-846
Extraction Procedure for Oily Wastes
Total Organic Carbon
Total Oil and Grease
Determination of Reactive Cyanide and Sulfide
Determination of Photodegradable Cyanide
-Explosive Hazard
-------
EP TOXICITY TEST FOR OILY WASTE
(Proposed as Method 1330 in SW-846)
1. Separate the sample (minimum 100 gm) into its solid and liquid compo-
nents. The liquid component is defined as that portion of the sample
which passes through a 0.45 urn filter media under a pressure differen-
tial of 75 psi.
2. Determine the quantity of liquid (ml) and the concentration of the
toxicants of concern in the liquid phase (mg/1).
3. Place the solid phase into a Soxhlet extractor, charge the concentration
flask with tetrahydrofuran, and extract for 3 hours.
4. Remove the flask containing tetrahydrofuran and replace it with one
containing toluene.
5. Extract the solid for a second time, for 3 hours, with the toluene.
6. Combine the tetrahydrofuran and toluene extracts.
7. Analyze the combined extracts for the toxicants of concern.
8. Determine the quantity of liquid (ml) and the concentration of the
toxicants of concern in the combined extracts (mg/1).
9. Take the solid material remaining in the Soxhlet thimble and dry it at
100°C for 30 minutes.
10. Run the EP on the dried solid.
11. Calculate the mobile metal concentration (MMC) using the following
formula:
MMC = 1000 ([Q1 + Q2 -t- Q31/[L1 + L2])
Q- = Amount of toxicant in initial liquid phase of sample (amount of
liquid X concentration of toxicant) (mg)
Qj = Amount of toxicant in combined organic extracts of sample (amount of
liquid X concentration of toxicant) (mg)
Q3 = Amount of toxicant in EP extract of solid (amount of extract X
concentration of toxicant) (mg)
LI = Amount of initial liquid (ml)
L2 = Amount of liquid in EP = weight of dried solid from step 9 X 20 (ml)
J-3
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TOTAL ORGANIC CARBON
Method 415.1 (Combustion or Oxidation)
(Proposed as Method 9060 in SW-846)
1. Scope and Application
1.1 This method includes the measurement of organic carbon in drinking,
surface and saline waters, domestic and industrial wastes. Exclu-
sions are noted under Definitions and Interferences.
1 .2 The method is most applicable to measurement of organic carbon
above 1 mg/1.
2 . Summary of Method
2.1 Organic carbon in a sample is converted to carbon dioxide (CO-) by
catalytic combustion or wet chemical oxidation. The C02 formed can
be measured directly by an infrared detector or converted to me-
thane (CH4) and measured by a flame ionization detector. The
amount of C02 or CH, is directly proportional to the concentration
of carbonaceous material in the sample.
3. Definitions
3.1 The carbonaceous analyzer measures all of the carbon in a sample.
Because of various properties of carbon-containing compounds in
liquid samples, preliminary treatment of the sample prior to analy-
sis dictates the definition of the carbon as it is measured. Forms
of carbon that are measured by the method are:
A) soluble, nonvolatile organic carbon; for instance, natural
sugars.
B) soluble, volatile organic carbon; for instance, mercaptans.
C) insoluble, partially volatile carbon; for instance, oils.
D) insoluble, particulate carbonaceous materials; for instance,
cellulose fibers.
E) soluble or insoluble carbonaceous materials adsorbed or
entrapped on insoluble inorganic suspended matter; for in-
stance, oily matter adsorbed on silt particles.
3.2 The final usefulness of the carbon measurement is in assessing the
potential oxygen-demanding load of organic material on a receiving
stream. This statement applies whether the carbon measurement is
made on a sewage plant effluent, industrial waste, or on water
taken directly from the stream. In this light, carbonate and
bicarbonate carbon are not a part of the oxygen demand in the
stream and therefore should be discounted in the final calculation
J-5
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or removed prior to analysis. The manner of preliminary treatment
of the sample and instrument settings defines the types of carbon
which are measured. Instrument manufacturer's instructions should
be followed.
4. Sample Handling and Preservation
4.1 Sampling and storage of samples in glass bottles is preferable.
Sampling and storage in plastic bottles such as conventional poly-
ethylene and cubitainers is permissible if it is established that
the containers do not contribute contaminating organics to the
samples.
NOTE 1: A brief study performed in the EPA Laboratory indicated
that distilled water stored in new, one quart cubitainers did not
show any increase in organic carbon after two weeks exposure.
4.2 Because of the possibility of oxidation or bacterial decomposition
of some components of aqueous samples, the lapse of time between
collection of samples and start of analysis should be kept to a
minimum. Also, samples should be kept cool (4°C) and protected
from sunlight and atmospheric oxygen.
4.3 In instances where analysis cannot be performed within two hours (2
hours) from the time of sampling, the sample is acidified (pH<2)
with HCl or H2SO4.
5. Interferences
5.1 Carbonate and bicarbonate carbon represent an interference under
the terms of this test and must be removed or accounted for in the
final calculation.
5.2 This procedure is applicable only to homogeneous samples which can
be injected into the apparatus reproducibly by means of a micro-
liter type syringe or pipette. The openings of the syringe or
pipette limit the maximum size of particles which may be included
in the sample.
6. Apparatus
6.1 Apparatus for blending or homogenizing samples: Generally a
Waring-type blender is satisfactory.
6.2 Apparatus for total and dissolved organic carbon:
6.2.1 A number of companies manufacture systems for measuring
carbonaceous material in liquid samples. Considerations
should be made as to the types of samples to be analyzed,
the expected concentration range, and forms of carbon to be
measured.
6.2.2 No specific analyzer is recommended as superior.
J-6
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Reagents
7.1 Distilled water used in preparation of standards and for dilution
of samples should be ultra pure to reduce the carbon concentration
of the blank. Carbon dioxide-free, double distilled water is
recommended. Ion exchanged waters are not recommended because of
the possibilities of contamination with organic materials from the
resins.
7.2 Potassium hydrogen phthalate stock solution, 1000 mg carbon/liter:
Dissolve 0.21 28 g of potassium hydrogen phthalate (Primary Standard
Grade) in distilled water and dilute to 100.0 ml.
NOTE 2: Sodium oxalate and acetic acid are not recommended as
stock solutions.
7.3 Potassium hydrogen phthalate, standard solutions: Prepare standard
solutions from the stock solution by dilution with distilled water.
7.4 Carbonate-bicarbonate stock solution, 1000 mg carbon/liter: Weigh
0.3500 g of sodium bicarbonate and 0.4418 g of sodium carbonate and
transfer both to the same 100 ml volumetric flask. Dissolve with
distilled water.
7.5 Carbonate-bicarbonate, standard solution: Prepare a series of
standards similar to step 7.3.
NOTE 3: This standard is not required by some instruments.
7.6 Blank solution: Use the same distilled water (or similar quality
water) used for the preparation of the standard solutions.
Procedure
8.1 Follow instrument manufacturer's instructions for calibration,
procedure, and calculations.
8.2 For calibration of the instrument, it is recommended that a series
of standards encompassing the expected concentration range of the
samples be used.
Precision and Accuracy
9.1 Twenty-eight analysts in twenty-one laboratories analyzed distilled
water solutions containing exact increments of oxidizable organic
compounds, with the following results:
Increment as Precision as Accuracy as
TOC Standard Deviation Bias, Bias,
mg/liter TOC, mg/liter %_ mg/liter
4.9 3.93 +15.27 +0.75
107 8.32 + 1.01 +1.08
(FWPCA Method Study 3, Demand Analyses)
J-7
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Bibliography
1. Annual Book of ASTM Standards, Part 31, "Water", Standard D 2547-79, p 469
(1976).
2. Standard Methods for the Examination of Water and Wastewater, 14th Edi-
tion, p 532, Method 505, (1975).
J-8
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EXTRACTION METHOD FOR TOTAL OIL AND GREASE
(Proposed as Methods 9070 (liquids) and 9071 (solids) in SW-846)
1. General Discussion
a. Principle: Drying acidified sludge by heating leads to low results.
Magnesium sulfate monohydrate is capable of combining with 75% of
its own weight in water forming the heptahydrate and is used to dry
sludge. After drying, the oil and grease can be extracted with
freon.
b. Interference: See 502C.1b.
2. Apparatus
a. Extraction apparatus, Soxhlet.
b. Vacuum pump or other source of vacuum.
c. Extraction thimble, paper.
3. Reagents
a. Hydrochloric acid, HCl, cone.
b. Magnesium sulfate monohydrate. Prepare MgS04 H20 by overnight
drying of a thin layer of MgSO4'7H20 in an oven at 103°C.
c. Freon (1,1,2-trichloro-1,2,2-trifluoroethane), boiling point 47°C.
The solvents should leave no measurable residue on evaporation.
Distill if necessar-y.
d'. Grease-free cotton: Extract non-absorbent cotton with freon.
4. Procedure
In a 150 ml beaker weigh a sample of wet sludge 20+0.5 g, of which the
dry-solids content is known. Acidify to pH 2.0 (generally 0.3 ml cone.
HCl is sufficient). Add 25 g MgS04*H20. Stir to a smooth paste and
spread on the sides of the beaker to facilitate subequent removal. Allow
to stand until solidified, 15 to 30 min. Remove the solids and grind in a
porcelain mortar. Add the powder to a paper extraction thimble. Wipe the
beaker and mortar with small pieces of filter paper moistened with freon
and add to the thimble. Fill the thimble with glass wool or small glass
beads. Extract in a Soxhlet apparatus, using freon, at a rate of 20
cycles/hr for'4 hr. If any turbidity or suspended matter is present in
the extraction flask, remove by filtering through grease-free cotton into
another weighed flask. Rinse flask and cotton with freon. Distill the
solvent from the extraction flask in water at 70°C. Place the flask on a
warm steam bath for 15 min and draw air through the flask by means of an
applied vacuum for the final 1 min. Cool in a desiccator for exactly 30
min and weigh.
J-9
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5. Calculation
... ,., gain in weight of flask, g X 100
Grease and oil as % solids = ~—rr—7 r2—rri ~^ r- ^
weight of wet solids, g X %dry solids
6. Precision
The examinination of six replicate samples of sludge yielded a standard
deviation of 4.6%.
Source: Standard Methods For the Examination of Water and Wastewater, 14th
edition, pp. 519-520.
J-10
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TEST METHOD FOR THE DETERMINATION OF
REACTIVE CYANIDE AND SULFIDE CONTAINING WASTES
FINAL METHOD
1. Scope and Application
1.1 This method is applicable to water, vastevater and industrial wastes.
1.2 This method provides a fast and simple method to determine if a
waste is a reactive waste as a result of its tendency to release
toxic levels of hydrogen cyanide or hydrogen sulfide upon contact
with acidic medium. The approach is based on a reasonable "worst
case" disposal scenario.
1.3 This method is designed to measure only the hydrogen cyanide and/or
hydrogen sulfide gas evolved at the test conditions and not to re-
flect the total concentration of these gases, or their precursors,
in the sample. Variations in temperature, ionic strength and total
volume of the test solution will affect the amount of gas evolved.
The total volume of solution is kept constant from test to test.
Temperature and ionic strength are not controlled as they are in-
herent properties of each waste.
2. S"™ary of Method
2.1 An aliquot of the waste is acidified to pH 2 in a closed system.
The gas generated is swept from the reaction chamber using a pump
and passed through a calibrated gas detector tube. The detector
tube reading is used to calculate the concentration of gas evolved.
3. Sample Handling and Preservation
3.1 Samples containing, or suspected of containing sulfide or a com-
bination of sulfide and cyanide wastes, should be collected with
a minimum of aeration. The sample bottle should be filled completely,
excluding all head space, and stoppered. Analysis should commence
as soon as possible and samples should be kept in a cool, dark place
until analysis begins.
3.2 Samples containing or suspected of containing cyanide wastes without
the presence of sulfide compounds, can be preserved if analysis can
not begin immediately. Samples are preserved by adjusting to pH 12
with strong sodium hydroxide solution and storing in a cool, dark
place.
3.3 Determination should be performed in a well ventilated hood.
4. Interferences
4.1 The analyst should consult manufacturers' literature on the type and
natur* of potential interferences when using specific detector tubes.
5. Apparatus
5.1 Three neck round bottom flask with 24/40 ground glass joints, 250 mL.
5.2 Magnetic stirrer bar with magnetic stirring apparatus.
-------
5.3 Separator? funnel with pressure equalizing line and 24/40 ground
glass joint, 125 mL.
5.4 Straight glass adapter tubes with ground glass joint 24/40 and rubber
adapter sleeve, 2 each.
5.5 Flexible tubing to make connection from detector tube to pump.
5.6 Detector tubes: HCN detector tube with range of 10-120 yL (Draeger
67 28441 or equivalent). H2S detector tube with range 5-60 uL
(Draeger 67 28141 or equivalent).
5.7 pH meter and pH electrode of sufficient length to reach liquid level
(approximately 13 cm).
5.8 Pump capable of pulling 60 mL per minute ± 3 mL per minute (MSA
Model C-210 or equivalent).
5.9 Bubble meter for calibrating pump.
5.10 Stopwatch.
6. Reagents
6.1 Sulfuric acid, H2SOU, 1 U.
6.2 Cyanide Reference Solution: Dissolve approximately 2.5 g KOH and
2.51 g KCN in one liter distilled water. Concentration approximately
1 mg/mL.
6.3 Sulfide Reference Solution: Prepare from crystals of sodium sulfide
as described in Method 376,2 (Sulfide, Colorimetric, Methylene Blue)
Section 5.8 of Methods for Chemical Analysis of Water and Wastes,
EPA 600/4-79-020, March, 1979. The solution may be standardized by
the titrimetric iodine Method 376.1 of the same publication, al-
though this is not required.
7. System Check
7.1 The operation of the system can be checked using the cyanide or
sulfide reference solutions. It is difficult to predict a detector
tube reading from a known amount of reference solution due to vari-
ations in response of detector tubes of different sources. Reaction
flask temperature variations and total volumes also influence the
amount of gases evolved. However, the reference solutions can be
used to verify system operation and replicates can be expected to
agree to within approximately ± 20%
8. Procedure
8.1 Place 10g* of the waste to be tested into a beaker. Add approximately
80 mL deionized water and determine the amount of 1 II H2SOU required
to adjust pH to 2.0.
8.2 Place a second 10g* aliquot of the waste into the 250 mL round bottom
flask. Add deionized water in an amount so that the sum of Che volume
of water and the volume of 1 jfl H2SOU required for pH adjustment, will
equal 100 mL.
* or 10 mL
J-12
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8.3 Assemble the apparatus as shovn in Figure 2 using the proper de-
tection tube or tubes (see Figure 1).
8.4 Calibrate the pump in line to a flow of 60 mL/min ± 3 mL/min using
the bubble meter attached to the pump outlet. The flow can be
checked during and after the test period.
8.5 Begin stirring and make sure all connections are tight.
8.6 Carefully adjust the test solution to pH 2.0 using the 1 N H2SOU.
8.7 Note the readings of stain length at five minute intervals. If the
length of the stain exceeds the capacity of the detector tube, re-
analyze using a smaller aliquot. If very little or no stain develops,
the aliquot size may be increased, depending on the nature of the
sample. Solid samples require a certain amount of dilution to reach
a slurry state so that the acid may contact all portions of the sample
and so that stirring may take place.
8.8 Continue to monitor Che pH of the test solution, adjusting if neces-
sary to maintain at pH 2.0. Continue the pump operation for 30 min.
from the time of initial pH adjustment.
8.9 Stop the pump and record the final reading on the detector tube.
Note 1: The chemistry of some detector tubes may permit their
use in series to determine both H2S and HCN concurrently.
With the use of the Draeger detector tubes mentioned in
Section 5.6, the H2S tube must be first tube in the system.
Other detector tubes may operate differently.
Mote 2: As an optional step to determine a "total" evoluable gas
yalue, at the end of 30 minutes, the pH can be lowered to
less than pH 1 and a sand bath used to elevate the tempera-
ture. Increased evolution rates may be observed from some
samples.
9. Calculations
9.1 The concentration of gas evolved may be calculated as follows:
ppm gas evolved (3CN or 3sS)/g or mL *
final detector tube reading (ML)
volume of gas passed through detector tube (L) x aliquot
(g or mL)
and:
volume of gas passed through detector tube (L)*
pump flov rate (mL/ain) X length of test (min)
1000
9.2 The time of maximum gas evolution rate can be determined by com-
paring the rate of change over each five minute period to the
elapsed time.
J-13
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10. Precision and Accuracy
10.1 The precision of the method as determined by evaluation on standards
can be expected to be approximately ± 17%.
10.2 The accuracy of the method cannot be determined directly due to
the difficulty of providing a sample of known gas evolution
qualities. Calibration of the detector tubes used in
method (see Section 5.6) with standard gas mixtures indicate
the bias of the H2S tubes to be approximately + 162 at 20*C
and the bias of the HCK tubes to be approximately + 35Z at 20°C.
FIGURE 2
TEST APPARATUS
FINAL METHOD
Class Tub*
Detector Tube
•Outlet
Waste
Staple
Stir
J-14
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MtTHOD 9011
Method for the Determination of Photodegradable Cyanides
1.0 Scope and Application
1.1 Method 9011 1s used for the determination of photodegradable cyanides in
wastes under hypothetical field conditions. It is used to determine
whether particular wastes will form releasable cyanides (cyanide amenable
to cnionnate) as a result or exposure to UV radiation.
2.U Summary ot Method
2.1 Four representative waste samples are tested, tach sample is split into
two equal portions. One portion is suojected to UV irradiation oy a low
pressure mercury arc lamp to test for pnotodegradation. During irradation,
any HCN evolved is trapped in the gas absorber. After photolysis is
completed, each portion is analyzed according to method 9010. The presence
of photodegradable cyanides is determined by the differences in results.
3.U Interferences
3.1 Refer to Method 9010
4.U Apparatus and Materials
4.1 Quartz tube, (1.26 cm I.D. x 15 cm, "Vycor" brand from corning, or 11-
Jb9E in Fisher catalogue) witn provision for air inlet and vacuum outlet,
transparent to UV frequencies greater than 220nm.
4.2 Low pressure mercury lamp (G15T3 lamp, General Electric or equivalent
capable of emitting UV radiation at a frequency Deiow JUOnm).
4.3 Microburet; refer to Method 9U1U.
4.4 Flasks, condenser, and tubing are needed as shown in Figure 1. Ine
boiling flasn should be of 1-liter size witn inlet tune and provision for
a condenser. The gas absorber may oe a Fisher-Mi I Iigan scrubber. Assemoie
as shown in Figure 1.
b.U Keagents
b.l Refer to Method 9010.
6.0 Sample Collection, Preservation and Handling
6.1 Refer to Method 9010.
7.U Procedure
/.I fest for interferencs according to the procedure in Method yuiu.
7.2 Take a 20 gram sample of waste and split into two 10 gram portions.
7.3 Analyze one portion (A) for total and amenaoie cyanide according to Method
9uio.
J-15
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7.4 Take the second 10 gram portion (8) of the sample and place in a quartz
tube.
7.4.1 Connect quartz tube inlet to an air source and the tuoe outlet
to tne adsorber as specified in procedure 7.3 in Method yuiu.
7.4.2 Using the mercury arc lamp at a distance of twelve inches from
tne quartz tube, irradiate for tnirty minutes wniie drawing air
through the system.
Caution: Low pressure mercury arc lamps emit high energy ultra-
violet radiation, use caution to avoid exposing eyes or skin.
7.4.3 Determine the presence or total and amenable cyanide according
to procedures 7.J - 7.5 in Method yulO on tne sample in the
quartz tube.
7.4.4 [Determine the amount or (JN in the scruooer.
/.b Keport results for the rive measurements from each sample.
hXAMPLE: Cw m Pf1^
lotal Cn Amenable Scrubber
Sample 1A 82.5 10.4
Sample 18 63.1 21.8 5.7
This example would result from a sample which converted complexed
cyanide to amenable.
7.6 Spiked standards and check standards should be routinely analyzed.
a.O Quality Control
8.1 All quality control data should be maintained and available for easy
reference and inspection.
8.2 Employ a minimum of one blank per sample batch to determine if contamination
or any memory effects are-occurring.
8.J Analyze check standards after approximately every Ib samples.
8.4 Run one duplicate sample for every iO samples. A duplicate sample is a
sample brought through the whole sample preparation process.
8.b Spiked samples or standard reference materials snail be periodically
employed to ensure that correct procedures are being followed and that
ail equipment is operating properly.
a.b The method of standard additions shall be used for the analysis of aii
samples tnat surfer from matrix interferences.
J-16
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Air Inlec Tube
Quartz Tube
Connecting Tube
\\\
I II
fr
Gas Absorber
¥
Suction
Figure 1. Apparatus for Cyanide Distillation
J-17
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EXPLOSIVE REACTIVITY
(From "Department of Defense Explosives Hazard Classification
Procedures," Army Technical Bulletin 700-2, September 1982)
5-1. General, a. This chapter prescribes tests
that are required by Title 49 Code of Federal Regula-
tions for transport purposes and by STANAG No. 4123
and DOD for the establishment of storage hazard
classification.
b. Lethal and incapacitating chemical munitions
will be tested under criteria which are unique to
chemical weapons.
c. Binary chemical munitions will be classed in ac-
cordance with their industrial chemical hazards until the
essential components are combined with their explosive
components at which time paragraph b above applies.
5-2. Transport Testing Require-
ments, a. These tests must be conducted prior to
shipment in commerce of any explosive or propellant
composition except liquid explosives and are intended to
develop data on stability and sensitivity of new com-
positions of bulk explosives and solid propellants to
determine if they are safe to handle, transport and store.
Laboratory samples are used, with weights and dimen-
sions limited to the minimum necessary for drawing
conclusions. Preliminary testing with even smaller
samples is recommended to provide test personnel with
an indication of hazards to be encountered. The tests
specified in this paragraph generally do not require in-
strumentation other than that normally associated with
the equipment involved, e.g., ovens for thermal stability
tests.
b. Recording of data. The results of tests perform-
ed under this paragraph are to be recorded in a manner
simtlar to that shown in figure 5-1. The format shown is
intended only as a guide and maybe modified as re-
quired to fit a particular test program.
c. Instrumentation. Due to the limited quantity of
material involved in these tests, instrumentation to
record peak pressure, impulse, and ambient
temperature as well as high speed photography may be
eliminated.
d. Equipment. The following equipment is re-
quired for tests under this paragraph:
(1) One Bureau of Explosives impact apparatus.
Drawings are available at the Bureau of Explosives,
Association of American Railroads, 1920 *L' Street,
NW, Washington, DC 20036.
(2) One ventilated explosion-proof oven capable
of maintaining a temperature of 75 °C or above for a
period of 48 hours. The oven will be equipped to con-
tinuously record the temperature. Dual thermostats that
fail safe will be provided for temperature control.
(3) Number 8 electric blasting caps or caps of
equivalent strength as required. A number 8 blasting
cap means a cap which contains 0.4—0.45 grams of
PETN base charge pressed into an aluminum shell with
bottom thickness not to exceed 0.03 inch, to a specific
gravity of not less than 1.4 grams/cubic centimeter, and
primed with standard weights of primer, in accordance
with the manufacturer's specifications.
(4) One blasting machine or equivalent for in-
itiating electric blasting caps.
(5) Kerosene-soaked sawdust sufficient for three
beds, 1-foot square and Vi-inch thick.
(6) Electric match-head igniters as required.
(7) Solid lead cylinders 1 Vi -inch diameter by 4 in-
ches high as required.
(8) One piece of mild steel plate SAE 1010 to 1030,
'/i-inch thick by 12 inches square.
(9) Mild steel plates (SAE 1010 to 1030) 6-inch x
6-inch x 3/8-inch as required.
(10) Tubing, steel, cold drawn seamless,
mechanical, composition 1015, 1-7/8 inch OD, 0.219
inch wall thickness variations ± 10 percent acceptable
by 5Vi inches long as required.
(11) Cellulose acetate, or equivalent, cards,
2-inch diameter by 0.01-inch thick as required.
(12) Wire (demolition cable) as required for con-
necting blasting machine to electrically initiated items.
(13) Engineers special electric blasting caps (J-2)
as required.
(14) Two inch diameter by 1-inch long pressed
pentolite pellet, National Stock No. 1375-991-8891 as
required.*
e. Test samples. The following test samples are re-
quired for this paragraph:
(1) Twelve samples 2 ± '/<-inch cubes. (Cardboard
containers of comparable size to be used for granule;
substances.)
(2) Ten lOmg (approx) samples suitable for use :ii
the Bureau of Explosives impact apparatus (0.20 in. ±
.02 in. diameter x 0.10 in. ± .02 in. long).
•Available from: Commanding Officer, Navy Ships Parts
Control Cnuer, Mtvharucsburg, PA. 17055, ATfN: Code 370.
J-19
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Date
Sponsoring Agency
Contract No.
Explosive or Propellant Identity (Type No.)
Spec. Batch
Mfg. Date
Detonation Test
No. 8 Blasting Cap Test 1
Test II
Test III
Test IV
Test V
Samples: Five 2-inch cubes.
Detonated
Yes No
Burned
Yes No
Fragmented
Yes No
Test: One blasting cap per sample4
Ignition & Unconfined Burning Test
One 2-inch cube
One 2-inch cube
Four 2-inch cubes
Samples: Six 2-inch cubes.
Exploded
Yes No
Average Burning Time
Seconds
Test: 48 hours at 75°C in vented oven.
Card Gap Test
50% Value
(No. of Cards)
Impact Sensitivity Test
Bureau of Explosives Impact Apparatus
Ten 3 3/4" (+ 1/16") Drop Test
lO~Trials
Ten 10" (+ 1/16") Drop Test
To Trials
Number of Trials Exhibiting
Explosion
Flame and
Noise
Decomposition
Smoke
No Noise
No 'Reaction
No Smoke
No Noise
Number of Trials Exhibiting
Explosion
Flame and
Noise
Decomposition
Smoke
No Noise
No Reaction
No Smoke
No Noise
Approved:
Test Director
Test Department Head
Assigned Classification
DOT Forbidden
DOT Restricted*
DOT Class A
DOT Class B
DOT Class C
UN Number
DOD Approval (see para 3-2)
Signature
Title
Organization
*Shipping instructions are to be requested from DOT.
Figure 3-1. Sample summary data sheet.
J-20
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(3) Samples sufficient to fill 12 each of item
5-24(10) above (para 5-2y'(l)(b).
/. Detonation test.
(1) Place one lead cylinder (5-24(7)) upon the
steel plate (5-24(8)). Place a No. 8 blasting cap (5-24(3))
perpendicular to and in contact with a flat surface of the
2-inch cube sample (5-2e(l)) which is then placed on top
of the lead cylinder. A 2-inch diameter wood block with
a hole drilled in its center similar to that shown in figure
5-2 may be used for positioning the blasting cap. Defor-
mation (mushrooming) of the lead cylinder 1/8-inch or
more will be considered as evidence of detonation. Con-
duct this test a minimum of five times, or until detona-
tion occurs, whichever is the least number of tests.
(2) Data from this test will be recorded under
Detonation Test.
g. Ignition and unconfined burning test.
(1) Place a 2-inch sample (5-2e(l)) on a bed of
kerosene-soaked sawdust (3-24(5)), and ignite the
sawdust with an electric match-head igniter (5-24(6)).
Perform this test twice.
(2) Place four 2-inch (5-2e(l)) samples end-to-end
in a single row in contact with each other on a single bed
of kerosene-soaked sawdust (5-24(5)) and ignite the
sawdust with an electric match-head igniter (5-24(6)) at
one end.
(3) Record results under Ignition and Unconfined
Burning Test.
h. Thermal stability test.
(1) Place one 2-inch sample (5-2e(l)) in constant
temperature explosion-proof oven (5-24(2)). Raise the
temperature of the oven to 75°C and maintain the
temperature at 75°C for a period of 48 hours. The
temperature will be continuously recorded. Constant
observation is not required.
(2) Record results under Thermal Stability Test.
/. Impact sensitivity test.
(1) This test need not be conducted if:
(a) The substance did not detonate in the
detonation test (para 5.If), or
(b) The substance is in a granular or powder
form encased into a finished article and is not to be tran-
ported in bulk containers, or
(c) The substance detonated in the detonation
test (para 5.2f) and is to be cast, pressed or extruded in-
to cases.
(2) Conduct ten individual tests at each height us-
ing one sample (5-2e(2)) per test in the Bureau of Ex-
plosives impact apparatus (5-24(1)).
(3) The sample (5-2e(2)) is placed in the cup
assembly, the weight is then dropped from the desired
height (from 3-3/4" 10 times). If no explosion occurs,
repeat the test dropping the weight from 10-inches.
Observe results to supply data as required under Impact
Sensitivity.
(4) Use cleaning equipment as required to
thoroughly clean and dry the anvil and cup assemblies
of the impact apparatus prior to each test. Apparatus
must be at ambient temperature (room temperature)
25°C ± 5° prior to each test.
(5) Check that the equipment is properly leveled
and replace the tools when worn.
j. Card gap test.
(1) Materials required for each test are as follows:
(a) One each tubing (5-24(10))
(b) Sample (5-2e(3)) cast into or machined to
fit into above tubing.
(c) Two pentolite pellets 2-inch diameter by 1
inch long 5-24(14).
(d) One Engineers Special Blasting Cap J-2
(5-24(13)).
(e) One steel plate 6-inch x 6-inch x 3/8-inch
(5-24(9)).
(0 Cellulose acetate, or equivalent, cards
2-inch diameter x 0.01-inch thick (5-24(11)).
(g) Four pieces of plastic material 1/16-inch x
'/i-inch x '/i-inch.
(2) Test configuration. The components of the
test are arranged in the following manner. The witness
plate is supported on two edges parallel to and approx-
imately 6 inches above the ground surface. Four small
pieces of plastic material 1/16-inch x '/2-inch are placed
on the plate to support the pipe containing the test sam-
ple, and maintain the 1/16-inch air gap, which should
not overlap onto the propellant or explosive. The air
gap between the acceptor and witness plate should be
free of solid material. The test sample is to be located
approximately in the center of the witness plate. The
pentolite booster is then placed on top of and in contact
with the sample at the top of the pipe and the J-2
blasting cap attached. The arrangement of components
for this test is similar to that shown in figure 5-2 except
the cellulose acetate cards and the cardboard tube are
omitted in the first test. Detonation is indicated when a
clean hole is cut in the witness plate. The test sample and
explosives booster are to be at a temperature of approx-
imately 25°C ± 5° at time of test. Should no detonation
occur in the first test, it will be repeated two times for a
total of three tests. If detonation occurs, proceed to
paragraph 5-2y(3)).
(3) The following tests are to be performed when
the test sample detonates in the above tests (5-2/(2)).
If no detonation of the test sample occurs in the above
tests, this test will not be performed.
J-21
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ENGINEERS SPECIAL
BLASTING CAP (J-2)
WOOD BLOCK
PENTOLITE BOOSTER
CARD GAP CELLULOSE
ACETATE CARDS
0.01 INCH EACH
PROPELLANT OR
EXPLOSIVES COMPOSITION
SAMPLE
CARDBOARD TUBE
STEEL TUBE
1/16 INCH AIR GAP BETWEEN
STEEL TUBE AND PLATE
3/8 INCH
WITNESS PLATE
WOOD STAND
GROUND
FIGURE 5-2. SET-UP FOR CARD GAP TEST
J-22
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(a) The test samples, high explosive boosters
and witness plates used in these tests are as given in
paragraph 5-2y'(l) above. The attenuation cards used
are 0.01-inch cellulose ace^:? sheet or equivalent
(S-2d(l 1)). These tests are to be conducted with :!ie test
sample and booster at a temperature of approximately
25°C ±5° throughout." The test setup is as shown in
figure 5-2. The cellulose acetate cards should be held
firmly but not pressed.
(b) The first test to be performed will utilize 8
cards; if a detonation occurs, the number of cards will
be doubled (i.e., 16 cards) for the second test. If no
detonation occurs, reduce the number of cards by one-
• half (i.e., 4 cards). Doubling of the number of cards will
be continued in succeeding tests until no detonation oc-
curs. When a number of cards is reached that prevents
detonation, the next test will be with the number of
cards reduced by half the preceding increment of in-
crease (i.e., if detonation occurs at 32 cards but not at
64 cards, the next test will be with 48 cards). If detona-
tion occurs at the reduced number of cards (48 cards in
the example cited above) the number of cards in the next
test will be increased by one-half the preceding incre-
ment (i.e., from 48 to 56 cards), etc. This procedure will
be followed until the point of 50 percent probability of
detonation is obtained. If the card gap sensitivity of a
similar propellant or explosive composition is known
testing should begin at approximately that number of
cards.
(c) Detonation is indicated when a clean hole is
cut in the witness plate. The measure of charge sensitivity
is the length of attenuation (gap length) at which there is
50 percent probability of detonation according to the
above criterion. The charge sensitivity will be expressed
in terms of number of 0.01-inch cards necessary for the
50 percent value between detonation and no detonation.
Normally, a maximum of 12 tests will be required to
detemine the 50 percent value.
5-3. Tests Required by STANAG 4123
and Department of Defense for Storage
Hazard Classification.
a. The following tests will be performed on end
items:
(1) Single package test — uses internal source of
ignition or detonation, respectively, for items that are
expected to deflagrate or detonate, to cause article(s) to
function in order to ascertain the violence and extent of
deflagration or propagation of detonation, and to assess
the external hazard. Where more than one initiator is
present, the initiator capable of producing the most
energetic reaction will be functioned.
(2) Stack test — uses internal source of ignition or
detonation, respectively, for items that are expected to
deflagrate or detonate, to ascertain the violence and ex-
tent of deflagration or prepigation of detonation, and
to assess the external hazard when one iicrn or package
in a stack of five unpackaged items or five packages of
items is ignited or initiated. In special cases the DODC
may specify a different number.
(3) External fire, stack test — to ascertain the ef-
fect of fire external to the items or packages and, in the
event that the fire causes deflagration, detonation, or
explosion, to ascertain the violence and extent of pro-
pagation and the external hazard.
b. Test program.
(1) The simplest program of tests to prescribe is
that any new item should be subjected to each of the
three types of tests, with appropriate replication.
However, this would often waste effort and money
because it is not always necessary to perform all the
tests. Certain types of ammunition and certain results in
the early tests permit short cuts in the program. The
flow chart figure 5-3 shows appropriate combinations
of tests.
(2) Replication of tests. It is usual to perform the
single package test three times at least, to demonstrate
that the observed effects are reasonably reproducible.
Though this limited amount of replication s statistically
insignificant, it does provide the possibility to detect any
gross mistakes in the conduct of the tests and does
enable a controlling authority to exercise judgment in
the interpretation of results. Furthermore, in those tests
where it is possible to observe the proportions of the ar-
ticles that explode rather than a simple go/no-go result,
limited replication enables an experienced worker to
assess the reproducibility of the tests and the level of
confidence.
(3) Curtailment of testing. Some of the classifica-
fion tests are quite costly so that inevitably there must be
a compromise between the number of tests performed to
give a reliable, comprehensive picture of the behavior of
a product and the requirement for economy. Sometimes,
it is possible to curtail the testing program in the light of
the results of early tests. For example, there is no point
in continuing with a second and third test with single
packages or stacks if the first test gives explosion of the
total contents. Due caution requires that this result be
accepted at face value so that testing may proceed
directly to the next stage in the program. Also there is
always the option at any stage of detonation testing to
assume the worst assessment (risk of mass detonation)
and to proceed directly to the external fire test.
J-23
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c. Packaging to be recorded. Records of tests
should included details of the method and materials of
packaging used in the tests, so that the need for further
tests can be properly judged if the method or materials
of packaging should be changed at a later date.
d. Required instrumentation is given under each
type test. Details of this instrumentation are given in
chapter 6.
e. Single package test.
(1) Scope of test. Figure 5-3 indicates the two cir-
cumstances when this test may be used as a cheaper pre-
liminary to the expensive test with a stack of packages.
In the event of certain favorable results, it is then un-
necessary to perform the stack test. The first circum-
stance is an outer package containing more than one ar-
ticle. The second is a package containing only a single
article when it is anticipated that the article will present no
significant hazard and thus qualify for class division 1.4.
(2) Test procedure. Place the package containing
the product(s) to be tested on the ground. To provide
the necessary confinement, surround and cover the
package with sacks or boxes filled with earth or sand
creating a barrier in every direction. In the case of
packages exceedng 1m in any dimension, the barrier
should be at least 1m in every direction. Another
method is to place the package in a pit of sufficient
depth and cover it with earth or sand-filled sacks or
boxes to the specified thickness. An article near the
center of the package should be caused to function by
using its own integral detonator or igniter or a stimulus
of similar power to the detonator or igniter. For articles
which do not function by an integral detonator or ig-
niter, a device which simulates the detonation or igni-
tion of one article near the center, or other appropriate
stimulus,* is used. Perform the test a minimum of three
times unless detonation of the total content occurs first.
Blast instrumentation as specified in chapter 6 will be
utilized. Fragment collection is not required.
/. Stack test.
(1) Scope of test. Figure 5-3 indicates four cir-
cumstances in which a test should be performed in a
stack of five packages or five unpackaged articles. The
term "severe effects" refers to effects falling short of
explosion of the total contents (in a package containing
more than one item) but being so severe or so directional
as to raise doubts about their effect in a stack.
(2) Test procedure. Stack a minimum of five pack-
ages or unpackaged articles to simulate storage or
stowage conditions. They should be stacked in such a
manner that their contents are in a position most likely
to cause propagation of explosion. To provide the
necessary confinement, surround and cover the stack
with, jacks of boxes filled with earth or sand creatiag a
barrier 1 meter thick in every direction. An article near
the centered package or an article most nearly centered
should be caused to function by using its own integral
detonator or igniter or a stimulus of similar power to the
detonator or igniter. For articles which do not function
by an integral detonator or ignitor, a device which
simulates the detonation or ignition of one article near
the center, or other appropriate stimulus, is used. Per-
form the test a minimum of three times, unless an explo-
sion of the total contents occurs earlier. Blast in-
strumentation as specified in chapter 6 will be utilized.
Fragment collection and analysis as specified in chapter
6 is not mandatory but is encouraged to obtain addi-
tional information on this possible hazard.
g. External fire, stack test.
(1) Scope of test. An external fire test on a stack
of packages or articles is required. Fragment collection
and analysis will be made for each test other than those
of bulk high explosives packaged in wooden or fiber-
board containers. Fragment collection,-blast instrumen-
tation and analysis of results as specified in chapter 6
are to be employed for each test, except that when the
anticipated reaction is other than mass explosion, blast
instrumentation need not be employed.
(2) Test procedure. Stack a minimum of five pack-
ages or unpackaged articles on a wooden platform
about 1m above the ground surface. Place a steel band
around the stack to maintain it during the test. Pile
kindling, or other air dried wood not thicker than 30mm
beneath the platform and around the stack of packages
to give at least one half meter in every direction to pro-
mote uniform test results. Drench the kindling with
about 15 gallons of diesel fuel or kerosene. Ignite the
pile on two sides by means of an electric squib, an ig-
niting composition, small arms propellant, or other
suitable means. The test is usually performed once only.
5-4. Interpretation of Results and
Transport TeStS. Results of paragraph 5-2 tesis
will be interpreted as follows:
a. DOT "Forbidden" if the following occurs:
Thermal stability test (5-2/0 results in either a
detonation, burning, or marked decomposition of the
sample.
•For bulk granular propellants, an electric squib and 2 oz. of black powder will be placed within 4-inches of the bottom of the container (49CFR
173.53v).
J-24
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I
to
in
SUBSTANCE OR ARTICLE TO BE ASSESSED
PACKAGE CONTAINING MORE
THAN ONE ARTICLE
PACKAGE CONTAINING A SINGLE
ARTICLE. OR PACKAGE CONTAINING
SUBSTANCE WITHOUT INNER PACKAGING
SIGNIFICANT HAZARD
NOT EXPECTED
SINGLE PACKAGE TESTS
I
NDTC
I
DTC
NO SEVERE EFFECTS
SEVERE EFFECTS
I
NDTC
I
EXTERNAL FIRE TESTS
1
NDTC
DTC
l_
NO EFFECT
EXTERNAL TO
PACKAGE
DIVISION 1.4S
1
UNPACKAGED ARTICLE
LITTLE EFFECT
EXTERNAL TO
PACKAGE
DIVISION 1.4
MAIN EFFECT
FIRE OR
MASS-FIRE
DIVISION 1.3
SIGNIFICANT HAZARD
EXPECTED
MULTIPLE ARTICLE/PACKAGE TESTS
DTC
I
EXTERNAL FIRE TEST
MAIN EFFECT
FRAGMENTS
DIVISION 1.2
DETONATION
OF TOTAL
CONTENTS
DIVISION 1.1
FIGURE 5-3. HAZARD DIVISION ASSESSMENT
LEGEND:
OTC- DETONATION OF TOTAL CONTENTS
NDTC- NO DETONATION OF TOTAL CONTENTS
-------
b. DOT Restricted: Compositions with an explo-
sive impact sensitivity of less than 4-inches of drop
height (5-2/) will not be shipped until instructions
have been requested and received from the Materials
Transportation Bureau, Department of Transportation.
c. DOT Class A (DOD Class/Division 1.1) if one
or more of the following occur:
(1) Detonation, test (5-2/) resulted in an explo-
sion.
(2) Card gap tests (5-2/) have determind a detona-
tion sensitivity value of 70 or more cards.
(3) Impact sensitivity test (5-2/) produces an ex-
plosion at 4 inches or more, but not more than 10-in-
ches of drop height.
(4) Ignition and unconfined burning test (5-2g)
produces a detonation of the sample.
d. DOT Class B (DOD Class/Division 1.3) if all of
the following occur:
(1) Ignition and unconfined burning tests (S-2g)
resulted in burning deflagration.
(2) The Thermal stability test (5-2/0 did not result
in an explosion, burning, or marked decomposition.
(3) Test (5-2f) did not result in a detonation, and
card gap tests (5-2y) have indicated a detonation sen-
sitivity value of less than 70 cards or no reaction at zero
cards.
(4) Impact sensitivity test did not result in an ex-
plosion at 10 inches or less.
(5) The classifications derived from these tests
may be interim only. Final classifications will be based
on results of tests of packages as stored or transported.
5-5. Interpretation of STANAC and DOO Tests.
Results of tests given in paragraph 5-3 will be inter-
preted as follows:
a. The ammunition should be classified in the light
of the test results and of other relevant data in accor-
dance with the characteristics of the class divisions as in-
dicated hereunder. Sometimes, the observed hazard ef-
fects may vary among replicate tests or may not corres-
pond exactly to the definitions. When this occurs, the
DODC should use its judgment, or arrange for further
testing. It is prudent to err on the side of caution, par-
ticularly in the crucial decision as to whether or not a
product is susceptible to mass detonation.
b. Division 1.4 (DOT class Q comprises items
which are primarily a moderate fire hazard. They will
not contribute excessively to a fire. The effects, are largely
confined to the package. No fragments of appreciable
size or range are to be expected. An external fire must
not cause the simultaneous explosion of the total con-
tents of a package of such items. The least hazardous of
these items, namely those which are so designed and/or
packaged that any hazardous effect arising fTom ac-
cidental functioning during storage or transport is con-
fined within the artical or package, are called Safety
Ammunition and are placed in compatibility group S
regardless of their other inherent characteristics. Ar-
ticles containing about 1 ounce or less of explosives and
classified based on test results as 1.4S may be con-
sidered as inert for storage purposes and are not subject
to part 173 title 49 CFR for transport. Articles contain-
ing larger quantities of explosives, but also classified as
1.4S based upon tests may be considered inert for
storage purposes but must be reviewed on an individual
basis to determine if part 173 title 49 CFR is to be ap-
plied for transport.
c. Division 1.3 (DOT class B) comprises items which
are a mass fire hazard. Some items burn with great
violence and intense heat emitting considerable thermal
radiation. Others bum sporadically. They may explode,
but without the risk of mass detonation. Usually these
items do not produce dangerous fragments; however,
firebrands and burning containers may be thrown. (See
paragraph 4-2 and indicate minimum separation
distance when required.)
d. Division 1.2 (DOT class A) comprises items that
burn or detonate progressively, a few at a time. A con-
siderable number of fragments, firebrands and unex-
ploded items may be projected; some of these may ex-
plode on impact and propagate fire or explosions. Blast
effects are limited to the immediate vicinity. (See
paragraph 4-2 and indicate minimum separation
distances based upon data collected in accordance with
chapter 6.)
e. Division 1.1 (DOT class A) comprises items that
detonate en masse. The explosion will result in severe
structural damage, the severity and range being deter-
mined by the amount of high explosives involved. There
may also be a risk of fragmentation from the article or
package in which the explosion occares. (See paragraph
4-2 and indicate minimum separation distances required
based upon data collected in accordance with chapter
6.)
5-6. Identification of the Hazard
Assessment by Assignment of a Hazard
Classification. Based on results obtained from
J-26
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tests outlined herein, the appropriate Hazard Class/Divi- Title 49 CFR. Additionally, the appropriate United Na-
sion/Storage Compatibility Group can be assigned. To tions Serial Number will be determined by referring to
determine the DOT criteria, it is necessary to refer to appropriate lists of UN numbers (see paragraph 4—6).
J-27
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