Federal Register, Volume 80 Issue 14 (Thursday, January 22, 2015)

[Federal Register Volume 80, Number 14 (Thursday, January 22, 2015)]
[Proposed Rules]
[Pages 3380-3446]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 2015-00544]

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Vol. 80

Thursday,

No. 14

January 22, 2015

Part III

Environmental Protection Agency

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40 CFR Parts 110 and 300

National Oil and Hazardous Substances Pollution Contingency Plan;
Proposed Rule

Federal Register / Vol. 80 , No. 14 / Thursday, January 22, 2015 /
Proposed Rules

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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Parts 110 and 300

[EPA-HQ-OPA-2006-0090; FRL-9689-9-OSWER]
RIN 2050-AE87

National Oil and Hazardous Substances Pollution Contingency Plan

AGENCY: U.S. Environmental Protection Agency (EPA).

ACTION: Proposed rule.

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SUMMARY: The Environmental Protection Agency (EPA or the Agency)
proposes to amend the requirements in Subpart J of the National Oil and
Hazardous Substances Pollution Contingency Plan (NCP) that govern the
use of dispersants, other chemical and biological agents, and other
spill mitigating substances when responding to oil discharges into
waters of the United States (U.S.). The proposal addresses the
efficacy, toxicity, environmental monitoring of dispersants, and other
chemical and biological agents, as well as public, state, local, and
federal officials' concerns regarding their use. Specifically, the
proposal amends the Subpart J regulatory requirements for the NCP
Product Schedule (Schedule) by adding new listing criteria, revising
the efficacy and toxicity testing protocols, and clarifying the
evaluation criteria for removing products from the Schedule. The Agency
also proposes amended requirements for the authorities, notifications,
monitoring, and data reporting when using chemical or biological agents
in response to oil discharges to the navigable waters of the United
States and adjoining shorelines, the waters of the contiguous zone, and
the high seas beyond the contiguous zone in connection with activities
under the Outer Continental Shelf Lands Act, activities under the
Deepwater Port Act of 1974, or activities that may affect natural
resources belonging to, appertaining to, or under the exclusive
management authority of the United States, including resources under
the Magnuson Fishery Conservation and Management Act of 1976. These
requirements are anticipated to encourage the development of safer and
more effective spill mitigating products, and would better target the
use of these products to reduce the risks to human health and the
environment. Further, the amendments are intended to ensure that On-
Scene Coordinators (OSCs), Regional Response Teams (RRTs), and Area
Committees have sufficient information to support agent
preauthorization or authorization of use decisions.

DATES: Comments must be received on or before April 22, 2015.

ADDRESSES: Submit your comments, identified by Docket ID No. EPA-HQ-
OPA-2006-0090, by one of the following methods:
Federal Rulemaking Portal: http://www.regulations.gov.
Follow the on-line instructions for submitting comments.
Mail: The mailing address of the docket for this
rulemaking is EPA Docket Center (EPA/DC), Docket ID No. EPA-HQ-OPA-
2006-0090, 1200 Pennsylvania Avenue NW., Washington, DC 20460.
Hand Delivery: Such deliveries are only accepted during
the Docket's normal hours of operation, and special arrangements should
be made for deliveries of boxed information.
Instructions: Direct your comments to Docket ID No. EPA-HQ-OPA-
2006-0090. EPA's policy is that all comments received will be included
in the public docket without change and may be made available online at
http://www.regulations.gov, including any personal information
provided, unless the comment includes information claimed to be
Confidential Business Information (CBI) or other information whose
disclosure is restricted by statute. Do not submit information that you
consider to be CBI or otherwise protected through http://www.regulations.gov. The http://www.regulations.gov Web site is an
``anonymous access'' system, which means EPA will not know your
identity or contact information unless you provide it in the body of
your comment. If you submit an electronic comment, EPA recommends that
you include your name and other contact information in the body of the
comment and with any disk or CD-ROM you submit. If EPA cannot read your
comment due to technical difficulties and cannot contact you for
clarification, EPA may not be able to consider your comment. Electronic
files should avoid the use of special characters, any form of
encryption, and be free of any defects or viruses. Comments and
suggestions regarding the scope of any future rulemaking should be
clearly differentiated from comments specific to this proposal (e.g.,
label Suggestions for Future Rulemaking and Comments on Current
Proposal).
Docket: All documents in the docket are listed in the http://www.regulations.gov index. Although listed in the index, some
information is not publicly available, e.g., CBI or other information
whose disclosure is restricted by statute. Certain other material, such
as copyrighted material, will be publicly available only in hard copy.
Publicly available docket materials are available either electronically
in http://www.regulations.gov or in hard copy at the EPA Docket, EPA/
DC, EPA West, Room 3334, 1301 Constitution Avenue NW., Washington, DC.
The Public Reading Room is open from 8:30 a.m. to 4:30 p.m., Monday
through Friday, excluding legal holidays. The telephone number for the
Public Reading Room is 202-566-1744 to make an appointment to view the
docket.

FOR FURTHER INFORMATION CONTACT: For general information, contact the
Superfund, TRI, EPCRA, RMP, and Oil Information Center at 800-424-9346
or TDD at 800-553-7672 (hearing impaired). In the Washington, DC
metropolitan area, contact the Superfund, TRI, EPCRA, RMP, and Oil
Information Center at 703-412-9810 or TDD 703-412-3323. For more
detailed information on this proposed rule contact Gregory Wilson at
202-564-7989 (wilson.gregory@epa.gov) or Vanessa Principe at 202-564-
7913 (principe.vanessa@epa.gov). The contacts address is: U.S.
Environmental Protection Agency, Office of Emergency Management,
Regulations Implementation Division, 1200 Pennsylvania Avenue NW.,
Washington, DC 20460-0002, Mail Code 5104A, or visit the Office of
Emergency Management Web site at http://www.epa.gov/oem/.

SUPPLEMENTARY INFORMATION: The contents of this preamble are:

I. General Information
II. Entities Potentially Affected by This Proposed Rule
III. Statutory Authority and Delegation of Authority
IV. Background
A. Historical Background
B. Current Statute and Regulation
C. Advanced Response Planning
V. This Action
A. Discharge of Oil
B. Subpart A--Introduction
1. Definitions
C. Subpart J--Use of Dispersants, and Other Chemical and
Biological Agents
1. General
2. Authorization of Use
3. Monitoring the Use of Dispersants
4. Data and Information Requirements for Product Schedule
Listing
5. Submission of Confidential Business Information (CBI)
6. Addition of a Product to the Schedule
7. Mandatory Product Disclaimer
8. Removal of a Product From the Schedule
9. Appendix C to Part 300
10. Appendix E to Part 300
VI. Summary of Proposed Rule Provisions

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VII. Statutory and Executive Order Reviews
A. Executive Order 12866: Regulatory Planning and Review and
Executive Order 13563: Improving Regulation and Regulatory Review
B. Paperwork Reduction Act
C. Regulatory Flexibility Act (RFA)
D. Unfunded Mandates Reform Act
E. Executive Order 13132: Federalism
F. Executive Order 13175: Consultation and Coordination With
Indian Tribal Governments
G. Executive Order 13045: Protection of Children From
Environmental Health Risks and Safety Risks
H. Executive Order 13211: Actions That Significantly Affect
Energy Supply, Distribution or Use
I. National Technology Transfer and Advancement Act
J. Executive Order 12898: Environmental Justice

I. General Information

In April 2010, the Deepwater Horizon underwater oil well blowout
discharged significant quantities of oil into the Gulf of Mexico. The
blowout discharged oil from one mile below the sea surface.
Approximately one million gallons of dispersants over a three-month
period were deployed on surface slicks over thousands of square miles
of the Gulf, and approximately three quarters of a million gallons of
dispersants were, for the first time, injected directly into the oil
gushing from the well riser. This use of dispersants raised many
questions about efficacy, toxicity, environmental trade-offs, and
monitoring challenges that EPA seeks to address through the proposed
revisions to Subpart J.
The proposed revisions to Subpart J address the use of dispersants
and other chemical and biological agents to respond to oil discharges
into waters of the U.S. Over the past several years, EPA's Office of
Research and Development (ORD) has conducted research on improved
laboratory protocols for dispersant and bioremediation efficacy, and
revisions to Subpart J to address these new protocols were under
consideration. As a result of this research and the Deepwater Horizon
event, the new protocols in the proposed revisions, in addition to
increasing the overall scientific soundness of the data, take into
consideration not only the efficacy but also the toxicity, long-term
environmental impacts, endangered species protection, and human health
concerns raised during responses to oil discharges, including the
Deepwater Horizon blowout. Additionally, area planning requirements for
dispersant use authorization, toxicity thresholds and advanced
monitoring techniques are also proposed. The proposed amendments are a
major component of EPA's effort to inform the use of dispersants and
other chemical or biological agents when responding to oil discharges.
They incorporate lessons learned from the federal government's
experiences in the Gulf, and address recommendations specific to agent
testing and use in response to oil discharges from the National
Commission on the BP Deepwater Horizon Oil Spill and Offshore Drilling
Report to the President.
The proposed amendments would help to ensure that only products
that perform effectively in laboratory testing would be listed on the
NCP Product Schedule (Schedule) for use in mitigating the effects of
oil discharges in the environment. Manufacturers would be required to
provide more detailed product application materials, ecological
toxicity data, and human health and safety information, including more
detailed instructions for product application in the field.
Prohibitions on using products in certain areas under certain
conditions determined by On-Scene Coordinators (OSCs), Regional
Response Teams (RRTs), and EPA would help ensure that first responders
are better able to mitigate environmental effects when spills occur.
The required submission of additional product toxicity information
would aid OSCs and RRTs when evaluating specific product information
and when deciding whether and which products to use to mitigate hazards
to the environment and human health caused by discharges or threatened
discharges of oil.
Specifically in this action, the Agency proposes, for the following
areas:
Definitions. Amend definitions for Bioremediation agents,
Burning agents, Chemical agents, Dispersants, Sinking agents, Sorbents,
and Surface washing agents; add new definitions for Bioaccumulation,
Bioconcentration, Biodegradation, Biological agents, Bioremediation,
Herding agents, Products, and Solidifiers; and remove definitions for
Miscellaneous Oil Spill Control Agents (MOSCA) and Surface collecting
agents.
General Requirements. Revise to reflect new and amended
regulatory definitions.
Authorization of Use. Revise to clarify planning and
preauthorization responsibilities, establish limitations and
prohibitions on the use of certain agents, establish requirements for
storage and use of agents, clarify authorities for requiring
supplemental testing, monitoring and information on agents, establish
requirements for agent recovery from the environment, and establish
reporting requirements for agent use.
Monitoring the Use of Dispersant. Establish monitoring
requirements for dispersant use in response to major discharges and/or
certain dispersant use situations.
General Product Information for Schedule Listing. Revise
and establish requirements, including designation of and testing for
all product categories under which the listing is requested, Safety
Data Sheets, sample product labels, shelf life, collection and
recovery, persistence in the environment, storage and use conditions,
physical and chemical properties, component identities, concentration
limits on National Water Quality Criteria and Standards contaminants,
laboratory accreditations, submission of all testing data and
calculations, production capabilities, and any other data or
certification informing the product's performance capabilities or
environmental benefits.
Dispersant Testing and Listing Requirements. Revise the
efficacy testing methodology using a baffled flask test, establish new
developmental and sub-chronic toxicity testing requirements, revise the
acute toxicity testing methodologies, revise the listing criteria, and
establish use limitations to saltwater environments.
Surface Washing Agent Testing and Listing Requirements.
Revise the acute toxicity testing methodology and listing requirements,
establish efficacy testing requirements and listing criteria, and
establish use limitations based on product testing for salt and/or
freshwater environments.
Bioremediation Agent Testing and Listing Requirements.
Revise the efficacy and acute toxicity testing methodologies and
listing criteria, establish exceptions for specified non-proprietary
products, and establish use limitations based on product testing for
salt and/or freshwater environments.
Solidifier and Herding Agent Testing and Listing
Requirements. Revise the acute toxicity testing methodology and listing
criteria, and establish use limitations based on product testing for
salt and/or freshwater environments.
Sorbent Requirements. Establish a list of known, non-
proprietary sorbents to be made publicly available in lieu of listing
sorbents on the Schedule, and requirements for data and information for
sorbent products with components other than those specifically
identified in the rule.
Submissions of Confidential Business Information. Revise
the allowable confidential business information claims and reporting
procedures.

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Addition of a Product to the Schedule. Revise the
submission requirements including the package contents, EPA's review of
submission package, request for review of decision, changes to a
product listing, and transitioning of listed products from the current
Schedule to the new Schedule.
Mandatory Product Disclaimer. Revise the product
disclaimer requirements.
Removal of a Product from the Schedule. Revise the basis
for removal and appeals process.
Appendix C to part 300. Revise the requirements for
product testing protocols and summary test data including new
dispersant baffled flask efficacy and toxicity tests; new standard
acute toxicity tests for bioremediation agents, surface washing agents,
herding agents, and solidifiers; and revised bioremediation agent
efficacy test.
Appendix E to Part 300--Oil Spill Response. Remove this
appendix from the NCP.
EPA estimates industry may incur total incremental costs of
approximately $668,000 to $694,000 annually. The benefits of the
Subpart J amendments are assessed qualitatively. Such benefits include,
for example, greater clarity of regulatory requirements, as well as
less toxic products. This action does not pose significant impacts on a
substantial number of small entities. The Regulatory Impact analysis,
which can be found in the docket, provides more detail on the cost
methodology and benefits of this action.

Cost of the Proposed Rule
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Annualized costs, 20 years
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Annualized at Annualized at
3% 7%
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Costs................................. $667,610 $694,343
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II. Entities Potentially Affected by This Proposed Rule

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Industrial category NAICS code
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Chemical Manufacturing.................................. 325
Merchant Wholesalers, Nondurable Goods.................. 424
Professional, Scientific, and Technical Services........ 541
Waste Management and Remediation Services............... 562
Oil and Gas Extraction.................................. 211
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The list of potentially affected entities in the above table
includes manufacturers and users of chemical and biological agents, and
other oil spill mitigating devices and substances used as
countermeasures against oil discharges. The Agency's goal is to provide
a guide for readers to consider regarding entities that potentially
could be affected by this action. However, this action may affect other
entities not listed in this table. If you have questions regarding the
applicability of this action to a particular entity, consult the
person(s) listed in the preceding section entitled FOR FURTHER
INFORMATION CONTACT.

III. Statutory Authority and Delegation of Authority

Under sections 311(d) and 311(j) of the Clean Water Act (CWA), as
amended by section 4201 of the Oil Pollution Act of 1990 (OPA), Public
Law 101-380, the President is directed to prepare and publish the
National Oil and Hazardous Substances Pollution Contingency Plan (NCP)
for removal of oil and hazardous substances. Specifically, section
311(d)(2)(G) requires the President to include a schedule identifying
``dispersants, other chemicals, and other spill mitigating devices and
substances, if any, that may be used in carrying out'' the NCP. The
authority of the President to implement this portion of the CWA is
currently delegated to EPA in Executive Order 12777 (56 FR 54757,
October 22, 1991). Subpart J of the NCP governs the use of dispersants,
and any other chemical or biological agent to respond to oil discharges
(40 CFR part 300 series 900).

IV. Background

A. Historical Background

The Council on Environmental Quality (CEQ) first published the
National Oil and Hazardous Materials Pollution Contingency Plan in 1970
(35 FR 8508). Among its elements was Annex X--Schedule of Dispersants
and other Chemicals to Treat Oil Spills. Annex X provided a basic
regulatory framework that included authorization of use, restrictions,
and information requirements to be submitted to the Federal Water
Quality Administration (FWQA). This initial schedule advocated
mechanical and other control methods, and the removal and proper
disposal of oil from the environment. It also specified that
dispersants might be used in accordance with the schedule if other
control methods are judged to be inadequate or infeasible, and if
certain information requirements and usage requirements were met. As a
listing requirement, manufacturers had to provide the FWQA with methods
for analyzing the chemical components in fresh and salt water, or
reasons why such analytical methods could not be provided. Except to
prevent or substantially reduce the hazard to human life or limb, or
substantial hazard of fire to property, dispersants were restricted
from use on or in any: Distillate fuel oil; spill of oil less than 200
barrels in quantity; shoreline; waters less than 100 feet deep; waters
containing major populations or breeding or passage for species of fish
or marine life which may be damaged or rendered commercially less
marketable by exposure to the dispersant or dispersed oil; waters where
the winds and/or currents are of such velocity and direction that the
dispersed oil mixtures would likely, in the judgment of the FWQA, be
carried to shore areas within 24 hours; and waters where such use may
affect surface water supplies. The CEQ revised the National Oil and
Hazardous Materials Pollution Contingency Plan, renaming it the
National Oil and Hazardous Substances Pollution Contingency Plan (NCP)
in 1971 (36 FR 16215). The NCP was amended again in 1971 (36 FR 18411)
and 1972 (37 FR 28208), with no substantive changes to Annex X.
As a result of the Federal Water Pollution Control Act (Pub. L. 92-
500) of 1972, CEQ again revised the NCP, including revisions to Annex X
(38 FR 21887, August 13, 1973). The title of Annex X changed to the
``Schedule of Chemicals to Remove Oil & Hazardous Substances
Discharges.'' While the Schedule still advocated mechanical and other
control methods, and the removal and proper disposal of oil from the
environment, it broadened its applicability to chemical agents,
including dispersants. It also recognized separate authorizations of
use for chemical agents on minor, medium and major discharges. In
addition, the revised schedule required an official report from a
recognized laboratory with a description of the analytical methods
employed and results obtained in determining the chemical and
biological characteristics of the chemical agent, but no longer
required the submission of those analytical methods. Biological and
burning agents were not part of the Schedule, which expressed caution
on their use.
In 1975 CEQ again revised the NCP, including Annex X (40 FR 6282).
Annex X was now the ``Schedule of Chemicals and Other Additives to
Remove Oil & Hazardous Substances Discharges,'' and it was ``. . .
revised and expanded to provide more precise and definitive
information, concerning substances which may be employed to remove
discharges.'' Additionally, Executive Order 11735 (38 FR 21243, August
3, 1973) made EPA responsible for Annex X. Chemical agents or any other
substance not specifically defined in the

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Schedule were to be considered for use on a case-by-case basis. The
Schedule advocated the development and utilization of mechanical
control methods to remove or mitigate oil, and to remove, mitigate, or
neutralize hazardous substances discharges from the environment, with
subsequent proper disposal. The Schedule intended that no harmful
quantities of any substance were to be applied to waters to remove or
mitigate the effects of oil or hazardous substances discharges. The
Schedule also provided procedures for authorization of use for
different agent categories, and separate regulatory authorization of
use for dispersants or other chemical agents was established for minor,
medium, and major discharges. Product shelf life, toxicity and
effectiveness, and analytical methods needed to obtain such data were
among the technical data requirements. Similar provisions were tailored
to surface collecting agents and biological additives.
In 1982, EPA amended the NCP; the revision included rewriting of
Annex X as Subpart H of 40 CFR part 300 of the revised Plan (47 FR
31180). The Agency allowed OSCs to authorize the use of dispersants or
other chemicals to treat discharges of oil, provided they were listed
in the previous Annex X, with the following limitations:
Authorization applies only to discharges of oil, not to
releases of hazardous substances.
OSCs may only authorize the use of dispersant or other
chemicals on EPA's Acceptance list, which included the twenty-eight
products tested and found acceptable for their intended purpose in the
previous Annex X.
State consultation provisions regarding the use of any
dispersant or other chemicals in its waters required the OSC to obtain
concurrence from the EPA representative to the RRT.
The new Subpart H of 40 CFR part 300 also provided for a case-by-
case authorization by the EPA Administrator (``Administrator'') or
designee of the use of dispersants or other chemicals not on EPA's
Acceptance list in treating oil discharges or hazardous substances
releases. However, EPA did not include testing procedures or a process
for designation of dispersants or other chemicals as acceptable for
use.
In 1984, EPA published amendments to Subpart H, including adding
Appendix C (49 FR 29192). The amendments specified testing and data
requirements for listing of dispersants, surface collecting agents, or
biological additives on the Schedule to ensure sufficient data was
available for the OSC. Standardized testing procedures generated
comparable data regarding the products' effectiveness and toxicity.
Appendix C detailed the methods and types of apparatus to be used in
carrying out the revised standard dispersant effectiveness and toxicity
tests, as well as the format required for summary presentation of
product test data. Listing of a product on the Schedule was neither a
recommendation nor authorization for use on an oil discharge, but
rather a confirmation that data submission requirements had been
satisfied. EPA's listing on the Schedule did not confirm its safety or
effectiveness or constitute an endorsement; in fact, a new requirement
was established that either a written disclaimer to this effect or
EPA's written disclaimer be included in all product technical
literature or advertisements. Products previously listed under Annex X
were included on the new Schedule as the previous data requirements
were sufficient to permit OSCs to make informed decisions about product
use.
The amendments also provided for OSC authorization for use of
burning agents on a case-by-case basis with the concurrence of the EPA
RRT representative and the States, and prohibited the use of sinking
agents in waters of the United States. They encouraged advance planning
by allowing the OSC to act without the concurrence of the RRT and
affected States if these parties have approved a plan identifying the
products that may be used in specific contexts. The amendments also
allowed the OSC to authorize the use of any product (including products
not on the Schedule) without obtaining the concurrence of the EPA
representative to the RRT or the affected States if the use of a
dispersant, surface collecting agent, or biological additive is
necessary to prevent or substantially reduce hazard to human life, and
there is not sufficient time to obtain concurrence. However, the OSC
was to inform the EPA RRT representative and the affected States of the
use of a product as soon as possible, and obtain their concurrences for
the product's continued use in the situation once the threat to human
life had subsided. These provisions were designed to eliminate delays
in life threatening situations, such as spills of highly flammable
petroleum products in harbors or near inhabited areas. Subpart H was
re-designated as Subpart J with minor changes in 1990 (55 FR 8666),
with those definitions present in Subpart H moved to Subpart A, and a
new definition and data requirements for miscellaneous spill control
agents added.
In 1994, EPA revised the NCP in response to the passage of the Oil
Pollution Act in 1990 (59 FR 47384). The final rule significantly
revised Subpart J to its current regulatory requirements with respect
to authorization of use, data requirements, dispersant effectiveness
and toxicity testing protocols, surface washing agent toxicity testing
protocol, bioremediation agent effectiveness testing protocol, and
requirements for adding products to the Schedule. As a result, several
dispersants were re-classified as surface washing agents because they
did not pass the dispersant efficacy test threshold, but were effective
in removing oil from solid surfaces.

B. Current Statute and Regulation

Section 300.910 of Subpart J addresses the authorization of the use
of products on the Schedule and specifies the conditions under which
OSCs may authorize the use of dispersants, other chemicals, and other
spill mitigating substances. Sections 300.915 and 300.920 describe the
data requirements and the process for adding products to the Schedule.
To list a product on the Schedule, Subpart J currently requires the
submission of technical data on the product to EPA. Data on
dispersants, surface collecting agents, surface washing agents, and
miscellaneous oil spill control agents must include the results of the
toxicity test set for these products in Appendix C of the NCP. Data on
dispersants must also include the results of the dispersant
effectiveness test, while bioremediation agents must include results of
the bioremediation effectiveness test, also set forth in Appendix C.
These tests are conducted at the expense of the product manufacturers
and must be performed by laboratories experienced with Appendix C
protocols.
The raw data and a summary of the results from these tests are then
submitted to EPA, where they are reviewed to confirm that the data are
complete and that the specified procedures were followed. The data
requirements for placement of a product on the Schedule are designed to
provide sufficient data for the OSCs to judge whether and in what
quantities a product may be used to control a particular discharge.
Inclusion of a product on the Schedule means only that the data
submission requirements have been satisfied. The listing of a product
on the Schedule does not mean that the product is recommended or
authorized for use on any specific oil discharge nor does it imply that
EPA has in any other way endorsed the product for the use listed or for
other

[[Page 3384]]

uses. The standardized testing procedures set forth in Appendix C
provide OSCs comparable data regarding the toxicity, effectiveness, and
other characteristics of different products.

C. Advanced Response Planning

Under the current 300.910(a) regulation, RRTs and the Area
Committees (ACs) are required to address, as part of their planning
activities, the desirability of using appropriate dispersants, and
other chemical or biological agents. The RRTs and ACs generally develop
``preauthorization plans'' which address the specific context in which
products can be used under OSC direction. Preauthorization plans are
approved with concurrences from EPA, Department of Interior (DOI) and
Department of Commerce (DOC) natural resource trustees, and the
state(s) with jurisdiction over the water to the area, which they
apply. When a preauthorization plan approves in advance the use of
certain products under specified circumstances, the OSC may authorize
the use of the products without obtaining the specific concurrences
described elsewhere in that section of the regulation. The use of
chemical or biological agents is only one approach of many available,
such as mechanical collection or in-situ burning, and decisions about
their use should be weighed to achieve greater overall environmental
protection.
To facilitate the best possible response, it is important that the
regional-level and area-level contingency planning efforts of the RRTs
and ACs, respectively, are coordinated closely with each other and are
consistent. Section 300.910(a) authorizes the RRTs to review and either
approve, disapprove, or approve with modification the preauthorization
plans developed by Area Committees that addresses dispersants or other
spill mitigating substances. This advanced planning has allowed the OSC
to authorize the use of products without obtaining the specific
concurrences, if the RRT representatives from EPA and the states with
jurisdiction over waters to which a preauthorization plan applies, and
DOC and DOI natural resource trustees approve their use in advance. The
OSC primarily uses the Schedule to confirm if a product is listed,
analyze toxicity and efficacy data, note worker health and safety
precautions, understand proper product application, and compare one
product to another in order to make the most informed decision on how
to mitigate an oil discharge.
AC responsibilities include enhancing contingency planning;
ensuring preplanning of joint federal, state, and local response
efforts; and expediting decisions on the use of dispersants and other
spill mitigating devices and substances. The Area Contingency Plan
(ACP) must list the equipment, dispersants or other spill mitigating
substances, and personnel available to ensure effective and immediate
removal of a discharge. ACPs must also ensure the mitigation or
prevention of a substantial threat of a discharge; provide a
description of the procedures to be followed for obtaining an expedited
decision regarding the use of dispersants (which may be addressed in
applicable preauthorization plans); and identify the means to monitor
use of chemical countermeasures. Many coastal ACPs include some type of
preauthorization zones for dispersants, while most Regional Contingency
Plans (RCPs) address other product categories, such as bioremediation
and surface washing agents. RRTs, in cooperation with the states and
federal agencies, have addressed the requirements for the conduct of
in-situ burns (ISB) of oil discharges in their RCPs.
This planning has allowed consideration of chemical agent use on
oil discharges as a viable response tool in combination with other
mitigation measures. These agents have increasingly been considered and
used in the field, as evidenced by research and case studies presented
at national and international oil spill conferences, research and
development funding from private and government stakeholders, RRT
efforts to plan for their use, requests for EPA and other federal
experts to advise field personnel on the use of such products, and by
the response to the Deepwater Horizon oil spill. While many research
efforts have helped to clarify issues and added information on the
toxicity, efficacy, proper use, and human health impacts of these
response technologies, uncertainties still arise. The Agency has an
interest in resolving the issues that arise from the use of chemical
and biological agents in spill responses, as its representatives are
asked to concur with chemical and biological agent use for marine and
freshwater spills.
The use of non-mechanical oil spill mitigating technologies, such
as dispersants, surface washing agents, sorbents, solidifiers,
bioremediation agents, and others are among the available oil response
options that responders may consider in the United States and the
world. The National Academies' National Research Council report titled
``Oil Spill Dispersants: Efficacy and Effects'' (2005), recommends that
steps be taken to better support policymakers and spill responders
faced with making choices regarding the use of dispersants as part of
spill contingency planning efforts or during actual spills. The United
States Coast Guard has promulgated new requirements for certain vessels
to have only Schedule listed dispersant response capabilities while
operating in designated dispersant preauthorization zones (74 FR 45004,
August 31, 2009).
The proposed amendments are aimed at ensuring that chemical and
biological agents have met efficacy and toxicity requirements, that
product manufacturers provide important use and safety information, and
that the planning and response community is equipped with the proper
information to authorize and use the products in a judicious and
effective manner.

V. This Action

This proposal addresses the efficacy, toxicity, environmental
monitoring of dispersants, other chemical and biological agents, and
other spill mitigating substances, as well as public, state, local, and
federal officials concerns on their authorization and use. The sections
below explain the proposed requirements and revisions, and EPA is
requesting comments by section. Alternatives offered should include
rationale and supporting information in order for the Agency to include
the alternative in any final rule.

A. Discharge of Oil

The Agency is proposing revisions to harmonize 40 CFR part 110.4
with the definitions for chemical and biological agents proposed for
Subpart J. The current language in Sec. 110.4 is specific to
dispersants and emulsifiers. The proposal replaces the terms
``dispersants and emulsifiers'' with the broader terms of ``chemical
agent'' and ``biological agent'' as proposed to be amended in Sec.
300.5. The proposed definition for chemical agents includes elements,
compounds, or mixtures designed to facilitate the removal of oil from a
contaminated environment and mitigate any deleterious effects. The
proposed definition for biological agents includes microorganisms
(typically bacteria, fungi, or algae) or biological catalysts, such as
enzymes, able to enhance the biodegradation of a contaminated
environment. Chemical and biological agents would include both the
dispersants and emulsifiers cited in Sec. 110.4. By revising 40 CFR
part 110, the Agency is clarifying that any chemical or biological
agent added to a discharge of oil with the intent to circumvent any

[[Page 3385]]

provision of 40 CFR part 110 is prohibited. To further reflect the
proposed revisions, the Agency is proposing to also amend the section
title to ``Chemical or biological agents.'' EPA believes the proposed
amendment is consistent with U.S. Coast Guard (USCG) regulations, which
prohibit the discharge of chemicals or other substances into the sea
that circumvent discharge conditions specified in their regulation (33
CFR 151.10(g)). EPA requests comment on these revisions.

B. Subpart A--Introduction

1. Definitions
The Agency is proposing revisions to Sec. 300.5 that amend the
definitions for Bioremediation agents, Burning agents, Chemical agents,
Dispersants, Sinking agents, and Sorbents. The Agency proposes to
revise the term Surface washing agent and amend its definition.
Additionally, the proposal includes new definitions for
Bioaccumulation, Bioconcentration, Biodegradation, Biological agents,
Bioremediation, Herding agents, Products, and Solidifiers. Finally, the
Agency is removing the definitions for Miscellaneous Oil Spill Control
Agent (MOSCA) and Surface collecting agents.
(a) Revised Definitions
Bioremediation agent--The Agency is proposing to revise the
definition of bioremediation agents to identify as such biological
agents and/or nutrient additives. These agents would be deliberately
introduced into a contaminated environment to increase the rate of
biodegradation, which in turn would assist in mitigating deleterious
effects caused by contaminants. The proposed definition identifies as
bioremediation agents microorganisms and enzymes. It also identifies
nutrient additives such as fertilizers containing bio-available forms
of nitrogen, phosphorus, and potassium. The proposed definition
clarifies the current definition and adds specific examples of
bioremediation agents. This clarification will help manufacturers of
products in identifying the type of product, and hence, what testing
requirements they will need to comply with to have a product listed on
the Schedule.
Burning agents--The Agency proposes to revise the definition of
burning agents to identify as such those additives that improve the
combustibility of the materials to which they are applied. This could
be achieved through either physical or chemical means. Burning agents
include inorganic compounds in the form of gelling agents, such as
aluminum soap. For example, the fuel used in helitorch systems is a
mixture of powdered gelling agents with either gasoline, jet fuel, or a
diesel/gas mixture, which are organic compounds.\1\ The Agency believes
both the inorganic gelling agent and the organic fuel (e.g., gasoline)
meet the burning agent definition by improving the combustibility of
the materials to which they are applied through physical or chemical
means. The Agency considered including ignition devices in the
definition of burning agent because improving the combustibility of oil
and igniting that oil could be considered one and the same. The intent
would be to clarify the potential that not only substances, but also
the devices holding those substances, be considered in the case-by-case
authorization of use of such agents. The Agency rejected this approach
since many devices either deliver the agent to the oil to be burned and
do not enter the water, or are consumed in the burn along with the
agent. The Agency requests comment on whether it should add ignition
devices to the definition of a burning agent.
---------------------------------------------------------------------------

\1\ Fingas, Mervin, (Ed) (2011), Oil Spill Science and
Technology, Gulf Professional Publishing, pp. 836, ISBN: 978-1-
85617-943-0.
---------------------------------------------------------------------------

Chemical agents--The Agency proposes to revise the definition of
chemical agents to identify as such those elements, compounds, or
mixtures that are designed to facilitate the removal of oil. These
agents may be used to mitigate deleterious effects of the oil on a
contaminated environment. The proposed definition would include under
the chemical agent category burning agents, dispersants, herding
agents, sinking agents, solidifiers, surface washing agents, and those
bioremediation agents that consist of nutrient additives. The proposed
language reflects the distinction the Agency is now making between
chemical and biological agents, allowing product manufacturers to
better target the testing requirements and OSCs to better inform their
authorization of agent use in specific situations. The proposal also
removes from the definition agent categories that are either being
eliminated, prohibited or amended to conform to the changes, as
discussed below.
Dispersants--The Agency is proposing to revise the definition of
dispersants to identify them as those agents that promote the formation
of small droplets of oil in the water column by reducing the oil-water
interfacial tension. Dispersants are proposed to be defined as
typically mixtures of solvents, surfactants (including biosurfactants),
and additives. The proposed definition specifically addresses the
process through which these agents assist in mitigating the
consequences of a discharge, clarifying for manufacturers which testing
requirements they will be subject to when seeking to list a product on
the Schedule.
Sinking agents--The Agency is proposing to revise the definition of
sinking agents to identify them as those substances deliberately
introduced into an oil discharge to submerge the oil to the bottom of a
water body. The current definition is ambiguous in regards to how much
sinking below the water surface would qualify as a sinking agent, as
some submersion below the surface but generally not to the bottom of
the water body can also be associated with other agents, such as
dispersants. The proposed definition specifies these agents purposely
sink the oil to the bottom of a water body. The Agency is prohibiting
the use of sinking agents in the remediation of oil discharges in water
because of their potential for causing adverse effects on benthic
organisms vital to the food chain of the aquatic environment.
Sorbents--The Agency is proposing to revise the definition of
sorbents to identify them as inert, insoluble substances that readily
absorb and/or adsorb oil or hazardous substances. The proposed
definition specifies that sorbents are not combined with or act as any
other chemical or biological agent. The proposed definition also
specifies that sorbents are generally collected and recovered from the
environment and that they may be used in their natural bulk form, or as
manufactured products in particulate form, sheets, rolls, pillows, or
booms. The proposed definition identifies sorbents as substances
consisting of: (1) Natural organic substances (e.g., feathers, cork,
peat moss, and cellulose fibers such as bagasse, corncobs, and straw);
(2) inorganic/mineral compounds (e.g., volcanic ash, perlite,
vermiculite, zeolite, clay); and (3) synthetic compounds (e.g.,
polypropylene, polyethylene, polyurethane, polyester). The proposed
changes simplify the definition by removing the definitions of
absorption and adsorption that are embedded in the current definition
of sorbents. The Agency believes this is appropriate given these are
generally recognized scientific terms and the proposal does not
distinguish sorbents or in any way restrict their use based on whether
they absorb or adsorb the oil. The definition also adds the ``natural''
qualifier to organic substances, indicating that organic substances
that

[[Page 3386]]

have been treated with other substances would not necessarily fall
under this category of agents and should not immediately be considered
a sorbent. It also expands on and simplifies the examples by removing
the references to the type of birds that feathers could come from, by
adding bagasse to the examples for natural organic substances, and by
adding clay to the examples for inorganic/mineral compounds. The Agency
requests comments on whether the definition is appropriate or if there
are other materials that should also be included.
Additionally, the Agency requests comments on particulate materials
(e.g., clay) as sorbents. There is concern that particulate materials
with densities greater than the seawater (or freshwater depending on
where they may be used) have the potential to become sinking agents,
settling to the seabed and posing potential risks to benthic organisms.
This question is also relevant when considering emerging response
technologies such as the use of particulate materials to form oil-
mineral aggregates (OMAs) to promote dispersion. OMAs are stable
microscopic entities formed when particulate materials interact with
the oil droplets resulting in distinct oil and mineral phases. These
fine mineral particles could be intentionally introduced by themselves
to promote physical dispersion by preventing the oil to re-coalesce, or
can also be used in conjunction with dispersants to enhance chemical
dispersion. However, any particulate material that by itself, or when
combined with oil (e.g., OMA), results in overall densities less than
the waters where it may be used, would not be prohibited as a sinking
agent. The Agency requests comment on whether the use of sorbent
materials in particulate form should be specified for use only in booms
or other contained manufactured products, and whether there should be
limitations on the authorization of use on water for sorbents in loose
particulate form. Alternatively, the Agency also requests comment and
supporting rationale on other approaches, including whether particulate
materials in loose form, or specifically OMA technologies, should be
excluded from the regulatory definition of sorbents.
Finally, EPA also requests comments on the qualifier phrase ``that
are generally collected and recovered from the environment.'' For
example, a natural organic and biodegradable sorbent (e.g., bagasse)
may not necessarily need to be removed after it has absorbed/adsorbed
the oil when used in a wetland or salt marsh. Such removal may cause
more harm than the oil itself due to trampling in the wetland or salt
marsh. Once the oil is brought to the surface by the sorbent,
biodegradation of both the oil and the sorbent can take place,
especially if nutrients are added to enhance biodegradation. Another
example would be the use of OMA technology to promote dispersion, which
might not lend itself to collect or remove the aggregates from the
environment. Thus, the Agency is requesting comment on whether testing
and/or authorization of use requirements should be considered for
particulate materials in loose form or OMA technologies that may be
used in discharge situations where they would not be collected and
recovered from the environment.
Surface washing agents--The Agency is proposing to revise the term
surface washing agent and the definition for surface washing agents.
The proposed definition would identify surface washing agents as those
substances that separate oil from solid surfaces (e.g., beaches, rocks,
metals, or concrete) through a detergency mechanism. This detergency
mechanism would lift and float the oil for collection and recovery from
the environment. The use of these agents results in minimal
dissolution, dispersion, or transfer of oil into the water column. The
proposed changes revise the term from singular to plural to be
consistent with the other agent definitions and clarifies that these
agents are to be recovered from the environment along with the oil
being treated.
(b) New Definitions
The Agency is proposing to add several new definitions that serve
as the foundation for the new proposed biological agent classification:
Bioaccumulation, Bioconcentration, Biodegradation, Biological agents,
and Bioremediation. The proposed definitions include basic terminology
and are consistent with definitions of these terms generally understood
by the scientific community.
The Agency is also proposing new definitions for the terms herding
agents and solidifiers. The proposed definitions address types of
agents originally captured under the surface collecting agent or the
miscellaneous oil spill control agent categories respectively, and are
terms that are more commonly used in industry. The definitions more
specifically describe the specific process through which the product
affects the oil for the categories and are consistent with definitions
of these terms generally understood by the scientific community.
Finally, the Agency is proposing a new definition for the term
product to clarify the difference between a specific product and an
agent type or category. All of the proposed new definitions can be
found in the Sec. 300.5 of this action.
(c) Removed Definitions
The Agency is proposing to remove the definitions for surface
collecting agent and for miscellaneous oil spill control agent (MOSCA).
The surface collecting agent definition is being removed and replaced
with a new herding agent definition to better reflect the common
terminology used in industry for these agents. The MOSCA definition is
being removed and replaced with a number of new and/or revised
definitions for types of agents. The original MOSCA category was used
as a catchall for all types of products that did not meet other agent
definitions. As the Agency adds new, more stringent testing
requirements for listing products on the Schedule, there is a need for
more specific category definitions to assist manufacturers in
determining which of those testing requirements apply to their
products. The Agency believes it has identified categories that capture
all products to be listed on the Schedule; we request comment on
whether the MOSCA category should be retained, and whether the proposed
categories are appropriate, including sufficient information and
rationale to support the addition of any new categories.

C. Subpart J--Use of Dispersants, and Other Chemical and Biological
Agents

1. General
EPA is proposing to amend Sec. 300.900 by revising paragraphs (a)
and (c), and by adding paragraph (d) to reserve for ``Releases of
Hazardous Substances''. The proposed revisions clarify that Subpart J
addresses not only chemical agents, but also those agents that now fall
under the newly proposed biological agent category. The revisions
reaffirms the notion that Subpart J is not only comprised of a Schedule
of chemical and biological agents, but also includes testing
requirements and authorization of use procedures. Consistent with
current Subpart J regulatory requirements the Agency is proposing to
reserve a section for ``Releases of Hazardous Substances'' to take
place of the current placeholder in Sec. 300.905, which is proposed to
be removed. Based on all relevant circumstances, testing data and
information, and in accordance with the authorization of use procedures
(including the appropriate concurrences and consultations), the waters
and

[[Page 3387]]

quantities in which a dispersant, or other chemical or biological
agents may be safely used are to be determined in each case by the OSC.
When taken together, these testing requirements, listing of agents and
authorization of use procedures address the types of waters and the
quantities of listed agents that may be used in response to discharges
of oil or hazardous substances. The wide variability in waters, weather
conditions, organisms living in the waters, and types of oil that might
be discharged requires this approach.
2. Authorization of Use
Section 300.910 sets forth the provisions for the authorization of
use of products on the Schedule in response to oil discharges. Subpart
J does not state or imply that chemical or biological agents are
preferred over other response options such as mechanical recovery
devices. EPA believes that the circumstances surrounding oil discharges
and the factors influencing the choice of response methods are many.
During the DWH response, a priority countermeasures scheme was
established to first use mechanical recovery via skimming/booming or
in-situ burning followed by subsea dispersant and lastly surface
dispersant use. Following DWH, EPA and the NRT issued Interim Actions
regarding the use of dispersants on oil spills to NRT members and RRT
co-chairs \2\ and to EPA Regional Administrators \3\ for consideration
during response planning. While response actions are incident specific,
the availability of response methods that address the specific
discharge situation depends largely on contingency planning activities
and on how these requirements are implemented through the RCPs, ACPs
and vessel and facility response plans. In order for a response to be
effective, the NCP requires coordination between the regulatory and
planning entities responsible for all these response plans. The Agency
believes that preauthorization or expedited decision making plans are
critical elements of contingency planning activities. Regularly
reviewing or revising preauthorization or expedited decision making
plans provides those agencies in charge of preparedness planning the
opportunity to identify and resolve concerns in advance, leading to
quick and effective operations during removal actions. The Agency
believes these proposed revisions to the authorization of use
provisions will assist OSCs, RRTs, and ACs in their advanced planning
activities as they consider response methods that result in the
greatest environmental protection. The goal is to ensure that
preauthorization or expedited decision making plans are developed and
maintained to effectively support decisions by OSCs during removal
actions. In carrying out advanced planning activities, the Agency
believes the NRT can assist RRTs by providing guidance on national
level issues that may arise during planning activities.
---------------------------------------------------------------------------

\2\ Tulis, Dana S., EPA Chair and Caplis, Captain John, USCG
Vice-Chair, National Response Team, ``Use of Dispersants on Oil
Spills--Interim Actions;'' Memorandum to NRT Members and RRT Co-
Chairs; December 16, 2010.
\3\ Stanislaus, Mathy; Assistant Administrator, OSWER EPA;
``Revision of Area Contingency Plans/Regional Contingency Plans
Regarding Use of Dispersants on Oil Spills--Interim Actions;''
Memorandum to EPA Regional Administrators, November 2, 2010.
---------------------------------------------------------------------------

EPA is amending Sec. 300.910 by revising paragraphs (a) through
(f); and by adding paragraphs (g), (h) and (i). EPA is not proposing
major changes to the current authorities granted to OSCs, RRT
representatives to the RRTs, States, DOC, DOI, or other National
Response Team decision makers with regards to the authorization and
application of chemical or biological agents. However, EPA recognizes
that the planning for and prolonged use and monitoring of chemical
agents, especially dispersants, may require additional planning
activities and monitoring requirements. Thus, the Agency is proposing
to reorganize this section; to add titles to the paragraphs for ease of
use; to add several requirements addressing the storage and use of
agents, notification of agent use and recovery from the environment;
and to revise language to clarify established EPA policy. The proposed
revisions and clarifications are highlighted for each paragraph under
Sec. 300.910.
EPA is also confirming, consistent with the intent of the NCP, that
use of chemical or biological agents in response to oil discharges to
waters of the U.S. or its adjoining shorelines must be authorized by an
OSC in accordance with Subpart J. The unauthorized use can result in
violations of section 301 and 311 of the CWA. Section 301(a) makes
unlawful ``the discharge of any pollutant by any person,'' except in
compliance with certain provisions of the CWA. In addition, section
311(b) establishes penalties for persons who fail or refuse to comply
with any regulation issued under section 311(j) of the CWA.
(a) Use of Agents Identified on the Schedule on Oil Discharges
Addressed by a Preauthorization Plan
The Agency is proposing revisions to Sec. 300.910(a) of Subpart J
to address the preauthorized use of chemical and biological agents
identified on the Schedule. The proposed revisions clarify the process
for preauthorization, the responsibilities of all involved parties, and
the factors to consider during the preauthorization process, including
the authorization for the use of agents by the OSC at the time of a
discharge. EPA is also proposing to reorganize paragraph (a) to provide
greater clarity by making the regulatory text easier to read and
follow. The Agency believes that the proposed revisions do not change
its fundamental policies regarding roles of Federal, state and local
representatives involved in planning for and responding to an oil
discharge, but rather clarify the current requirements and further
explain the responsibilities for each party. The Agency is also
proposing added procedures and review requirements intended to ensure
preauthorization plans are up-to-date so they are most effective when
implemented in case of a discharge.
EPA believes RRTs and ACs must work together in order to
effectively and successfully manage contingency planning. Thus, the
proposed revisions continue to require that, as part of their planning
activities, RRTs and ACs address in the preauthorization plan whether
the use of chemical and biological agents listed on the Schedule on
certain oil discharges is appropriate. The Agency believes that the
proposed revision clarifies the meaning of the desirability of using
appropriate chemical or biological agents. The Agency is removing ``. .
. the desirability of using appropriate burning agents.'' from
paragraph (a) and addressing the use of burning agents under paragraph
(c) to provide greater flexibility to OSCs for authorization of use.
Under the current paragraph (a), ACs are responsible for developing
preauthorization plans. ACs are also responsible for developing ACPs,
providing a forum to evaluate the environments within a jurisdiction
and establishing protection priorities. The information gathered during
the ACP development process should inform the development of
preauthorization plans. Identified representatives from the RRTs are
responsible for approving or requesting modifications of
preauthorization plans developed by the ACs. ACs can advocate for local

[[Page 3388]]

concerns to be reflected in the preauthorization plans they develop,
and the RRTs will decide if the plans are adequate and address region-
wide and cross-regional issues. Since the RRTs should be in a position
to provide guidance to ACs on common attributes within a region, EPA
continues to believe RRTs and ACs should work together to develop
preauthorization plans, particularly when identifying discharge
situations where chemical or biological agents may be used. There may
be circumstances where it is appropriate to allow either the RRTs and/
or ACs to develop preauthorization plans. Preauthorization plans
developed by an RRT would allow for these plans to better reflect
overarching regional circumstances. Therefore, the Agency is proposing
to include RRTs as another planning entity with responsibility for
developing preauthorization plans, and is requesting comment on this
change, and on the advantages or disadvantages of keeping the
development of these plans at the AC level.
ACPs generally describe discharge situations for the geographical
area for which they apply. Discharge situations developed as part of
area contingency planning activities may consider likely scenarios from
vessels, and onshore or offshore facilities. While RRTs and ACs should
consider the discharge scenarios described in ACPs when identifying
discharge situations in developing preauthorization plans, the Agency
believes they should also have the flexibility to consider other
discharge scenarios. The proposed language states preauthorization
plans must specify limits for the quantities and duration of use, and
use parameters for water depth, distance to shoreline, and proximity to
populated areas for discharge situations identified in which agents may
be used. The Agency believes that clearly stating the use parameters in
a preauthorization plan will make it easier for planners to address
concerns of preauthorizing agent use and in turn for responders to
authorize their use.
In meeting these provisions, the preauthorization plans should
document how both regional and logistical factors were addressed when
establishing dispersant use limits and parameters. Regional factors
include the likely sources and types of oil that might be discharged,
various discharge scenarios, and the existence and location of
environmentally sensitive resources or restricted areas that might be
impacted by discharged oil. Logistical factors include inventory,
storage locations and manufacturing capability of available agents,
availability of equipment needed for agent use, availability of
adequately trained operators, and the availability of appropriate means
to monitor agent use. While the proposed revisions simplify the
language and clarify the requirements, the Agency believes it is
necessary to keep in place the fundamental elements that should be
considered. The proposed factors generally parallel those under the
current 300.910(a) regulation. Several revisions include identifying
some factors as ``regional'' and others ``logistical.'' The Agency is
identifying ``logistical'' factors to ensure the availability of
chemical and biological agents to address discharge situations
identified in the preauthorization plan. The Agency added ``various
discharge scenarios'' as a regional factor to be considered because
preauthorization plans may cover more than one ACP with multiple
discharge scenarios that RRTs and/or ACs may want to consider. The
Agency also added the existence and location of ``restricted areas''
along with ``environmentally sensitive resources'' as a factor to
consider. Environmentally sensitive resources would include fish,
wildlife and their habitats, and other special areas of ecological
sensitivity that may be adversely affected by a discharge. While
``restricted areas'' may include ``environmentally sensitive
resources'' some areas may be restricted from certain activities
because of biologically sensitive topographic features or critical
habitats, such as submerged rock formations colonized by species (e.g.,
coral) and the organisms they interact with and support. NOAA's
Environmental Sensitivity Index maps, the Fish and Wildlife and
Sensitive (FWS) Environments Plan in ACPs, or environmental impact
statements, may contain relevant information on ``environmentally
sensitive resources'' for the RRTs and ACs to consider.
The proposal revises the phrase ``potential sources and types of
oil that might be spilled'' to ``likely sources and types of oil that
might be discharged.'' EPA believes the phrase ``likely sources and
types of oil'' better focuses on the sources and types of oil specific
to the preauthorization plan for which agents may be used. In addition,
the proposal revises ``spill'' to ``discharge'' to be consistent with
terminology in the NCP. The proposal also revises the phrase ``the
available means to monitor product application and effectiveness'' to
``means to monitor agent use in the environment'' as the Agency
believes it provides for additional flexibility for the RRTs and/or the
ACs to consider the scope of the monitoring, and to include other
endpoints beyond product application and effectiveness. The Agency is
proposing to eliminate the ``available'' qualifier, as it believes it
is unnecessary. Likewise, the Agency proposes to eliminate the
``available'' qualifier before ``product and storage locations'' and
revise the phrase ``product and storage location'' to the broader
``inventory, storage locations and manufacturing capability of
available agents'' to address lessons learned from the Deepwater
Horizon incident, including the challenges posed by the potential
sustained use of dispersants.
When developing preauthorization plans, RRTs and ACs should use the
best available scientific information to assess environmental trade-
offs, including those identified by conducting an ecological risk
assessment. Environmental trade-offs should be considered in
determining response options that provide the greatest environmental
protection. The RRTs and ACs should identify the affected biological
resources and their habitats likely to be negatively impacted, as well
as those that are expected to benefit. The natural resource trustees
are critical partners that can assist in conducting these analyses.
As previously stated, all members of the RRT are afforded an
opportunity to review and provide input on a draft preauthorization
plan. However, only the RRT representatives from EPA and the state(s)
with jurisdiction over the waters and adjoining shorelines within the
preauthorization plan area and the DOC and DOI natural resource
trustees may approve, disapprove, or approve with modification the
draft preauthorization plan. The Agency believes this remains the
correct approach. Given preauthorization plans are developed during the
contingency planning phase, the Agency believes that DOC and DOI
natural resource trustee concurrence is preferred over just
consultation because it provides for sufficient time to identify and
resolve natural resource concerns. As noted in the 1994 NCP final rule,
the requirement for concurrence during the advanced planning phase
ensures trustee involvement in decision-making (59 FR 47398).
Addressing in advance concerns that might otherwise slow the action
ensures that operations during a removal action can be carried out
quickly and effectively. EPA believes natural resource trustee
concurrence with preauthorization plans satisfies the consultation
obligation since the preauthorization plans specify the use parameters
for chemical or biological

[[Page 3389]]

agents. Thus, the Agency is retaining this concurrence requirement for
preauthorization plans.
The Agency is proposing to revise the ``Approved preauthorization
plans shall be included in the appropriate RCPs and ACPs'' in the
current Sec. 300.910(a) regulation to ``RRTs and ACs shall, as
appropriate, include applicable approved preauthorization plans in RCPs
and ACPs.'' The Agency is proposing to modify the qualifier
``approved'' with ``applicable'' to clarify that RRTs and ACs need to
include the preauthorization plans only in those RCPs and ACPs to which
they apply, and remains consistent with current requirements.
The Agency considered adding specifically the EPA Administrator and
the senior EPA representative to the NRT (e.g. NRT Chair) to Sec.
300.910(a) and other paragraphs to make clear the EPA Administrator's
and senior EPA NRT representative's existing authority under section
311(d)(2)(G) of FWPCA and Executive Order 12777, along with the OSC to
authorize any chemical or biological agent use. The Agency is
clarifying that if the preauthorization plan is approved in advance for
chemical or biological agent use under specified discharge
circumstances, then the OSC may authorize the use of the agents on the
Schedule for their intended purpose without the incident specific
concurrences and consultations described in paragraphs (b) of this
section unless otherwise directed by the Administrator in accordance
with current concurrence authority. The Agency believes this
clarification would not impede rapid decision-making on the part of the
OSC, and that for the majority of discharge situations, the OSC will
remain as the sole authorizing entity for discharge situations covered
by preauthorization plans. Note that in situations like a spill of
national significance (SONS) or an event of extended duration, the
Administrator already has the authority for, and is likely to have a
more direct role in chemical or biological agent use decisions. The
authority, jurisdiction, and implementation provisions in the NCP flow
from section 311 of the Clean Water Act and are reflected in Executive
Order 12777. All authorities under CWA 311 are delegated either
directly to the Administrator by Congress, or by Executive Order 12777
from the President to the Administrator. While the Administrator's
authority may be further delegated through senior management on down to
the RRT representative, the Administrator (and other delegatees) retain
the authority to act. The mere delegation of authority does not
prohibit the delegator from exercising said authority. However, given
these situations are rare and that this is an existing authority, the
Agency is not proposing a regulatory amendment to clarify the
Administrator's authority at this time. We request comment on this
issue.
The Agency is clarifying that chemical or biological agents may
only be used for their intended use, given the different listing
requirements proposed for the various categories of chemical or
biological agents. For example, a chemical agent that is listed on the
Schedule solely as a surface washing agent cannot be authorized for use
as a dispersant, nor can a chemical agent that is listed on the
Schedule solely as a dispersant for use under saltwater conditions be
used in freshwater.
The Agency is proposing specific procedures for concurrence
withdrawals, allowing agencies to do so if they believe the
preauthorization plan no longer addresses or reflects existing
situations if it were to be implemented. While an agency with
concurrence authority may now decide to withdraw concurrence from an
approved preauthorization plan, there are currently no set procedures
to promptly address those situations. The proposal would require the
RRT and the ACs to address the withdrawal of approval of the
preauthorization plan within 30 days of the withdrawal, allowing an
opportunity to address the concerns. The proposal also calls for the
RRT to notify the NRT of the final status of the preauthorization plan
within 30 days from the withdrawal. The Agency requests comments on
whether this 30 day notification requirement should also include
notification to the public. In the event of an Agency withdrawing its
concurrence from an approved preauthorization plan, EPA believes the
advanced planning process should continue with consideration for all
the elements specified in paragraph (a) of this section. While the
absence of a preauthorization plan requires that authorizations for
agent use be conducted according to paragraph (b) of this section, the
Agency continues to believe that preauthorization plans serve as a
valuable advanced planning tool that provides a strong foundation to
support decision-making and strongly encourages the resolution of any
withdrawal.
Finally, EPA proposes a new requirement for RRTs and/or ACs to
review, and revise as needed, preauthorization plans: (a) At least
every 5 years to address revisions of the Schedule; (b) after a major
discharge or a spill of national significance (SONS); (c) to reflect
new listings of threatened and/or endangered species or; (d) after any
other change such as a new or revised worst case discharge estimate
that may impact the conditions under which the use of chemical and
biological agents is preauthorized. A 5-year review cycle is consistent
with facility response planning requirements; as those plans are
revised and updated, it seems reasonable that preauthorization plans
should be reviewed and revised accordingly. The Agency recognizes that
development of preauthorization plans can be resource intensive;
however, once developed, a periodic review and revision as needed
should require much less effort. EPA welcomes comment on this timeframe
and suggestions with supporting information for alternatives.
This review requirement is intended to ensure that preauthorization
plans are actively maintained and updated to reflect revisions to the
Schedule. Preauthorization plans, as well as the facility and vessel
response plans reflected in them, may include information on products
listed on the Schedule. A review at least every 5 years is expected to
provide greater consistency not only between any Schedule revisions,
but also between any ACPs, facility, and vessel response plans. For
example, an ACP revision that results in a change in the worst-case
discharge scenario could trigger a preauthorization plan review.
Additionally, the requirement specifically includes plan review and
revision requirements as appropriate to reflect new listings of
threatened and/or endangered species that may occur. The EPA RRT
representative, the DOC and DOI natural resource trustees, and, as
appropriate, the RRT representative from the state(s) with jurisdiction
over the waters of the area to which a preauthorization plan applies
must review and either approve, approve with modification, or
disapprove any revisions to the preauthorization plans. This review and
approval is intended to focus on any revisions, and is not intended as
a requirement for review and approval for those portions that do not
require modifications.
(b) Use of Agents Identified on the Schedule on Oil Discharges Not
Addressed by a Preauthorization Plan
The Agency is proposing revisions to Sec. 300.910(b) of Subpart J
to address use of chemical or biological agents identified on the
Schedule for discharge situations that have not been addressed in
preauthorization plans. The proposed revisions clarify the authorities
and responsibilities of all involved parties,

[[Page 3390]]

and the factors to consider when authorizing the use of listed chemical
or biological agents in these situations. The Agency believes the
proposed revisions do not change its fundamental policies regarding the
roles of Federal, state and local representatives involved in an oil
discharge response.
The proposed revisions maintain, with the appropriate concurrences
and consultations, the OSC's authority to authorize the use of chemical
or biological agents on the oil discharge, provided that the agents are
listed on the NCP Product Schedule. The concurrence of the EPA
representative to the RRT and, as appropriate, the concurrence of the
RRT representatives from the states with jurisdiction over the waters
and adjoining shorelines threatened by the release or discharge is
maintained. The requirement for consultation with the DOC and DOI
natural resource trustees is also maintained. However, the language is
amended by removing ``when practicable'' with respect to consultation
with the DOC and DOI natural resource trustees. The Agency believes
that the case-by-case decision making should include consultations with
natural resource trustees since these discharge situations may present
unique challenges when selecting a response option that involves
chemical or biological agents. While the Agency recognizes the time-
critical nature of decision making during a response, advances in
communication technology (e.g., smart phones, email) provide OSCs with
increased capabilities to communicate quickly. Therefore, the Agency
believes it is reasonable to expect an OSC to be able to notify and
explain the circumstances requiring use of the certain agents to
natural resource trustees in a timely manner. Of note, while
consultation with the trustees on removal actions as required by OPA
does not equate to a concurrence requirement, the Agency believes that
such concurrence is highly desirable. The Agency is also proposing to
revise the term ``navigable waters threatened'' to ``waters and
adjoining shorelines threatened'' to be consistent with the provisions
in paragraph (a) of this section.
The preauthorization plan requirements in paragraph (a) proposes to
remove the term ``specific context'' currently used and instead clearly
establish what the term refers to. The proposal specifically identifies
the parameters that must be considered by the OSC for authorizing agent
use. Similar requirements are proposed under paragraph (b). Thus, in
meeting the provisions of Sec. 300.910(b), the OSC must consider and
document the parameters for the use of agents including, but not
limited to, quantities to be used, the duration of use, the depth of
water, the distance to shoreline and proximity to populated areas, and
should address factors such as environmentally sensitive resources or
restricted areas that might be impacted, agent inventory and storage
locations, agent manufacturing capability, availability of equipment
needed for agent use, availability of adequately trained operators and
appropriate means to monitor agent use in the environment. These
considerations are parallel to those proposed under paragraph (a) for
preauthorization and planning purposes. While the Agency is not
including other factors that may inform preauthorization planning
development, such as various discharge scenarios, this does not mean
these factors cannot or should not be considered if RRTs and/or ACs
choose to develop expedited decision making plans. The Agency believes
these are fundamental elements that would inform an assessment of the
overall ecological risks for the OSC to consider when authorizing the
use of chemical or biological agents.
Finally, while not required, EPA strongly recommends advanced
planning for expedited decision making for cases where the discharge
situation is not addressed in the preauthorization plans. Some RRTs
have developed expedited approval guidelines that are not part of the
preauthorization plans, but that offer an opportunity for advanced
contingency planning by gathering information on the key parameters
discussed above. Because discharge situations not covered by
preauthorization plans need incident specific (i.e., case-by-case)
authorization concurrence,\4\ expedited approval guidelines can be used
to support expedited incident specific authorizations. For chemical or
biological agents listed on the Schedule that are not authorized for
use under a preauthorization plan, the ACs and RRTs should work
together to outline the process for expedited authorization decisions
regarding their use. It is important to note that while the NCP
requires that the ACPs include procedures for expedited decisions,
these procedures can include disapproving the use of agents, or
approving the use of agents with certain operational conditions. For
example, areas may be designated in which the use of certain agents or
other discharge mitigating devices is prohibited, situations where
limits are placed on the quantities of agents used, or situations that
require certain monitoring requirements be in place.
---------------------------------------------------------------------------

\4\ http://www.epaosc.org/sites/5083/files/rrt6_nearshore_dispersant_eap_031605.pdf.
---------------------------------------------------------------------------

(c) Burning Agents
The Agency is proposing to replace the current authorization of use
for burning agents in Sec. 300.910(c) with a provision that provides
greater flexibility to OSCs for authorizing the use of burning agents.
Specifically, the Agency proposes that OSCs may authorize the use of
burning agents for authorized in-situ burns. The proposed amendments
recognize that relatively small quantities of burning agents are
ignited prior to or immediately after they are introduced to an oil
discharge. Furthermore, they are composed of substances that are
expected to rapidly burn off during use, which serves to remove them
from the water. The Agency also recognizes that ISB has become an
important response option that is used more frequently and the proposed
revisions would allow OSCs to authorize the use of burning agents for
authorized burns. For example, a significant number of ISBs were
conducted during the Deepwater Horizon oil spill,\5\ and ISBs appear to
be gaining a more prominent role as a response option in federal waters
in remote locations, such as the Arctic. Therefore the Agency believes
the proposed revisions better address OSC authorities for these
situations, without compromising environmental concerns. Further,
because of the nature of burning agents and the proposed revisions to
the authorization of use for these products, the Agency continues to
believe it is not necessary to require product submissions for burning
agents. Thus, the proposal removes the provisions for burning agents
under the current data requirements. The Agency requests comments on
this approach.
---------------------------------------------------------------------------

\5\ http://www.restorethegulf.gov/release/2011/08/19/operations-and-ongoing-response-august-17-2011.
---------------------------------------------------------------------------

(d) Exceptions
The proposed rule maintains the provision allowing OSCs to
authorize the use of any agent, including products not on the Schedule,
when it is determined that the use of the agent is necessary to prevent
or substantially reduce a threat to human life. The proposed revisions
do not change previous policy, but rather clarify the intent of the
exception. The Agency believes that the protection of human life is the
primary consideration in responding to an oil discharge. Life-

[[Page 3391]]

threatening oil discharges (e.g., spills of highly flammable petroleum
products in harbors or near inhabited areas) may occur at locations
where chemical agents on the Schedule are not immediately available.
The Agency believes that in such cases, an OSC must have the ability to
use agents that, in his professional judgment, would effectively and
expeditiously mitigate the threat to human life. Allowing this
authorization to occur without the required concurrences for
preauthorization or authorization of use for products on the Schedule
under paragraphs (a) and (b) respectively, eliminates delays in
responding to potentially life-threatening situations. The Agency is
proposing to include ``without obtaining the immediate concurrence'' to
clarify the scope of the exception. The proposed revisions are
consistent with the intent of the current regulation which recognizes
that once the threat to human life has subsided, the continued use of a
product shall be in accordance with authorization of use paragraphs (a)
and (b) of the section. In addition, this exception is intended for
those extraordinary situations in which time is of the essence to
mitigate the threat to human life; revising the language to replace
``hazard'' with ``threat'' clearly establishes this. The Agency
emphasizes this authority is not intended to circumvent the
authorization of use provisions in paragraphs (a) and (b) of this
section, which serve to address all other situations.
The proposed revisions also specify that the OSC immediately
notify, and document the reasons for the use of an agent to the EPA RRT
representative and the affected states as soon as possible, and must
obtain their concurrences where continued use of chemical or biological
agents extends beyond 48 hours. The Agency believes that advances in
communication technologies (e.g., smart phones, email) provide OSCs the
increased capabilities to communicate quickly. Therefore, it is
reasonable to expect that the OSC notify and explain the circumstances
requiring use of the agent to the designated EPA RRT representative
and, as appropriate, the RRT representatives from the affected states
and the DOC/DOI natural resources trustees within 48 hours. The Agency
is requesting comments on these revisions, and specifically on the 48
hour timeframe within which the OSC shall be operating in accordance
with authorization of use paragraphs (a) and (b) of the section.
(e) Prohibited Agents
The Agency is maintaining the current prohibition for the
authorization of use of sinking agents, and is clarifying that this
prohibition also applies to any other chemical agent, biological agent,
or any substance that acts as a sinking agent when mixed with oil.
While certain chemical and biological agents may submerge oil below the
water surface (e.g. dispersants are designed to break up oil into
small, near neutrally buoyant particles that are entrained in the water
column between the surface and the bottom), they would not be
considered ``sinking agents'' for purposes of the proposed definition
and this prohibition, given that they do not completely submerge oil to
the bottom of the water body when applied to an oil discharge. Sinking
agents, when applied to oil discharges, function by sinking floating
oil to the bottom of any body of water where used, potentially causing
adverse effects on benthic organisms vital to the food chain of the
aquatic environment. Additionally, the oil and these agents are very
difficult to remove. The Agency has similar concerns regarding
substances that could directly cause the oil to submerge to the bottom
of the water body when used in an oil spill response, and thus it is
specifically proposing to exclude their use.
The Agency is also proposing to add a prohibition from listing on
the Schedule and from authorizing use of any chemical or biological
agents that contain nonylphenol (NP) or nonylphenol ethoxylates (NPEs)
as components. This prohibition reflects the Agency's concern for these
substances, as presented in the EPA Nonylphenol and Nonylphenol
Ethoxylates Action Plan, released August 18, 2010. The Action Plan
specifically addresses nonylphenol (NP) and nonylphenol ethoxylates
(NPEs). NP and NPEs are produced in large volumes, with uses that
currently lead to widespread release to the aquatic environment. NP is
persistent in the aquatic environment, moderately bioaccumulative, and
extremely toxic to aquatic organisms. NP's main use is in the
manufacture of NPEs. NPEs are nonionic surfactants that are used in a
wide variety of industrial applications and consumer products. Many of
these, such as laundry detergents, are ``down-the-drain'' applications.
Some others, such as dust-control agents and deicers, lead to direct
release to the environment. NPEs, though less toxic and persistent than
NP, are also highly toxic to aquatic organisms, and, in the
environment, degrade into NP. Both NP and NPEs have been found in
environmental samples taken from freshwater, saltwater, groundwater,
sediment, soil and aquatic biota. NP has also been detected in human
breast milk, blood, and urine and is associated with reproductive and
developmental effects in rodents. EPA has encouraged the ongoing
voluntary phase-out of NPEs in industrial laundry detergents, and
intends to evaluate how releases and exposures are mitigated through
the phase-out action prior to taking any final regulatory action under
the Toxic Substances Control Act.\6\ The Agency believes this
prohibition would not adversely affect product manufacturers given
there are viable alternatives to the use of NP and NPEs in product
formulations. However, we are requesting comment on the potential
impacts of modifying existing products to meet this new requirement,
including cost.
---------------------------------------------------------------------------

\6\ For more information, refer to http://www.epa.gov/oppt/existingchemicals/pubs/actionplans/np-npe.html.
---------------------------------------------------------------------------

Alternatively, EPA considered a broader prohibition from listing
and from authorizing the use of chemical or biological agents
formulated with any endocrine disrupting compounds (EDC). EDCs impact
exposed organisms by altering the hormonal and homeostatic systems that
allow them to interact with and respond to their environment. The group
of molecules identified as potential endocrine disruptors is highly
varied and may be present in chemicals used as industrial solvents or
surfactants that can be found in dispersants and surface washing
agents. Because of the common properties of these compounds and the
similarities of the receptors and enzymes involved in the synthesis,
release, and degradation of hormones, no endocrine system is immune to
endocrine disrupting compounds.\7\
---------------------------------------------------------------------------

\7\ For more background information on endocrine disrupting
compounds and their human health and environmental effects, please
see http://www.epa.gov/endo/pubs/edspoverview/index.htm.
---------------------------------------------------------------------------

The 1996 Food Quality Protection Act directed EPA to develop a
screening program, using appropriate validated test systems and other
scientifically relevant information, to determine whether certain
substances may have hormonal effects in humans; the 1996 amendments to
the Safe Drinking Water Act authorized EPA to screen substances that
may be found in sources of drinking water for endocrine disruption
potential. In response to these mandates, the Agency's Endocrine
Disruptor Screening Program is developing requirements for the
screening and testing of pesticides, commercial chemicals, and

[[Page 3392]]

environmental contaminants for their potential to disrupt the endocrine
system.\8\ The science related to measuring and demonstrating endocrine
disruption is relatively new and validated testing methods are still
being developed. When complete, EPA will use these validated methods or
assays to identify and characterize the endocrine activity of
pesticides, commercial chemicals, and environmental contaminants,
specifically in relation to estrogen, androgen, and thyroid hormones.
EPA plans to use the assays in a two-tiered screening and testing
process: Tier 1 will serve to identify chemicals that have the
potential to interact with the endocrine system; and Tier 2 will
determine the endocrine-related effects caused by each chemical and
obtain information about effects at various doses. With this two-tiered
approach, the Agency will gather information needed to identify
endocrine-active substances and take appropriate action, as mandated by
Congress. To date, EPA has developed and validated 11 assays that
comprise the Tier 1 Screening Battery. EPA's validation effort
continues with the current focus on Tier 2 tests and potential
replacement assays for Tier 1.\9\ When all tests are finalized and
chemical information begins to be collected, EPA may further consider
how to incorporate that information into the Subpart J NCP
requirements, including additional testing and listing requirements.
Because validated testing methods are still being developed, the agency
is not proposing any test requirements with respect to endocrine
disruption for products to be listed on the Schedule.
---------------------------------------------------------------------------

\8\ http://www.epa.gov/endo/pubs/edspoverview/background.htm.
\9\ http://www.epa.gov/endo/pubs/assayvalidation/index.htm.
---------------------------------------------------------------------------

However, because NP and the NPE are extremely or highly toxic to
aquatic organisms, the Agency is proposing a prohibition specific to
Subpart J products containing NP and NPE as components. The Agency is
not proposing to include a broad prohibition on Subpart J products that
contain substances in which at least part of the toxic mode of action
may include disruption of the organism's endocrine system, but is
requesting comments on prohibiting similar substances that may be found
in products/agents that could be listed on the Schedule, or to what the
criteria should be in order to make that determination. As an
alternative, the Agency could require that all product components be
tested for a toxic mode of action that includes disruption of the
organism's endocrine system and is requesting comment on this approach
as well.
The Agency believes the proposed prohibitions are appropriate in
all cases, notwithstanding the proposed provisions for case-by-case use
authorization of burning agents under Sec. 300.910(c), or for
authorization of use of any chemical or biological agent when it is
necessary to prevent or substantially reduce an immediate threat to
human life under Sec. 300.910(d). There are chemical and biological
agent alternatives to sinking agents and to agents containing NP or
NPE, as well as mechanical methods for responding to oil discharges,
including those situations that pose extreme threats or are time
critical.
(f) Storage and Use of Agents
Section 300.915 currently requires that information be provided on
recommended conditions of storage and use for each product at the time
an application for listing a product under Subpart J is submitted to
the Agency. This information is summarized in EPA's NCP Product
Schedule Technical Notebook. Specifically, this information includes:
Special handling and worker precautions for storage and field
application; maximum and minimum storage temperatures (optimum ranges
and temperatures that will cause phase separations, chemical changes,
or other alterations to product efficacy); shelf life of the product;
recommended application rates and procedures, concentrations and
conditions (considering water temperatures, salinity, types and ages of
the oil); and any other application restrictions.
The Agency proposes to add a new paragraph (f) to this section that
complements the existing information requirements for the person or
entity submitting a product for listing (``submitter''). The proposed
requirements focus on the use of this information by the responder and
the OSC. Specifically, the revised provisions require the OSC to only
authorize for use those products that are stored under the conditions
specified by the submitter of the product for listing, including the
maximum, minimum and optimum temperatures, humidity and any other
relevant conditions. Additionally, the Agency proposes to require that
the OSC only authorize for use those products whose date of use does
not exceed the expiration date listed on the container's label at the
time of an incident, unless the responsible party \10\ provides the OSC
documentation, developed in consultation with the submitter of the
product for listing, prior to product use, affirming the product has
maintained its integrity, including no changes in the composition,
storage conditions, efficacy, and toxicity of any product. In such
cases where the product expiration date has passed but the owner or
operator of the facility/vessel storing the product still wants to be
able to use the product inventory, EPA proposes that samples of the
expired product lot representative of all storage conditions at any end
user location be tested following the applicable testing protocols in
Appendix C. The testing documentation is to include laboratory
information (i.e., contacts, accreditations) and all test data and
calculations (i.e., raw data and replicates, notes and observations,
calculated means and standard deviations, stock solution preparations,
source and preparations of test organisms, test conditions, chain of
custody forms, and summary reports). Only if the owner or operator can
demonstrate that the product has maintained its integrity is the OSC
allowed to authorize the use of that product inventory. The owner or
operator of the facility/vessel, or their representative, must re-label
the tested product lots and maintain documentation of the test results
until those lots are used or discarded, and must retest the expired
product lot representative of the product at least once every 5 years
to ensure efficacy and to allow an OSC to authorize the product for
use. The intent of these proposed revisions is to ensure that products
being authorized and used have maintained their efficacy, even though
storage beyond the products' original shelf life may have occurred. The
Agency believes it is the owner or operator's responsibility to ensure
that any product it stockpiles for future use has maintained its
efficacy and has not changed from its listed composition, including the
possibility of degrading into more toxic byproducts, once the
manufacturer's expiration date has passed. This retesting provision is
supported by the proposed requirements that the submitter of the
product for listing provide not only the recommended storage
conditions, but the anticipated shelf life of a product at those
conditions, and that the product label include both the manufacture and
expiration dates, and conditions for storage. The flexibility in this
proposed

[[Page 3393]]

revision allows for the use of available product inventory that may
still be viable. To alleviate concerns that applications are submitted
that establish an extended or indefinite shelf life for a product, the
Agency is requesting comments on whether any additional data or
information requirements should be included for product listing
determinations specific to a product's shelf life, or whether
alternative approaches, such as limiting the shelf life for product
categories to a given timeframe, should be considered.
---------------------------------------------------------------------------

\10\ Responsible party is defined in the NCP under 40 CFR 300.5.
---------------------------------------------------------------------------

(g) Supplemental Testing, Monitoring, and Information
This proposal maintains RRT authority in that they may require
supplementary toxicity and efficacy testing, or available data or
information that addresses site, area, or ecosystem specific concerns
relative to the use of a product for both planning and authorization of
use. While parallel to the current provisions, the proposed revisions
provide added flexibility. The current provisions allow RRTs to require
supplementary toxicity and efficacy testing of products, in addition to
those specified as technical requirements following the test methods
described in Appendix C to part 300, due to existing site-specific or
area-specific concerns when developing preauthorization plans. EPA
proposes to remove the qualifier ``When developing preauthorization
plans'' to provide greater flexibility for RRTs to require
supplementary toxicity and efficacy testing, or available data or
information that addresses site, area, or ecosystem specific concerns
relative to the use of a product for situations even when
preauthorization plans are not being developed. For example, RRTs may
need additional testing or information for situations that fall under
paragraph (b) of this section, including when developing an expedited
decision making plan. The proposed revision also allows for RRTs to
require supplementary product toxicity and efficacy testing, or
available data or information for both planning and authorization of
use situations, and based on that information may consider establishing
limitations for the use of products in certain areas. The Agency is
including ``available data and information'' to compliment the
supplementary toxicity and efficacy testing provision recognizing that
existing data or information that addresses site, area, or ecosystem
specific concerns relative to the use of a product may be available.
The Agency is also proposing to include ``ecosystem'' with area and
site specific concerns, as RRTs may want to gather additional
information on the use of certain products when assessing the use of a
product relative to the biological communities specific to their area.
The proposal removes ``in addition to the test methods specified in
Sec. 300.915 and described in appendix C to part 300.'' While RRTs may
want to use the efficacy and toxicity testing protocols specified in
Appendix C of the NCP for comparative purposes, the proposed revisions
clearly establish the RRTs authority to require tests using parameters
beyond those specified in Appendix C. Furthermore, there may be
supplementary toxicity and efficacy testing information based on
recognized standard testing methods already available that RRTs may
want to consider when addressing site, area, or ecosystem specific
concerns.
This proposal also provides the RRT authority to request that the
OSC require a responsible party to conduct additional monitoring
associated with the use of a product during a discharge incident. The
proposed revision compliments the proposed monitoring requirements for
dispersant use, but also including other chemical or biological agents,
or other testing endpoints. The Agency believes the RRT must be
afforded the ability to request that the OSC direct the responsible
party to conduct additional monitoring under Subpart J for the use of a
product in the environment. The RRT may request that the OSC consider
additional monitoring during an oil discharge response to support
operational decisions on dispersant use. For example, the RRT may want
to monitor the exposure of marine mammals to oil constituents,
including dispersed oil, or to monitor toxicity in the water column
using biological assays. The Agency requests comments on these proposed
revisions.
(h) Recovery of Agents From the Environment
The proposal identifies certain agent categories and substances
intended to be removed from the environment following their use:
Solidifiers, sorbents and surface washing agents. For those categories,
the Agency expects the agents to be recovered from the environment to
minimize any potential adverse impact. The proposal adds a new
requirement that charges the responsible party, under OSC oversight, to
recover these products from the environment. Recovery activities after
the use of these agents would include containment of the agents in the
water, collection of the agents mixed with oil or any residual agent,
storage of the oil-agent waste prior to disposal, and disposal of that
oil-agent waste. The Agency also recognizes there may be situations
where the safety of response personnel is threatened, or where
additional harm to the environment could occur during recovery
operations. Consequently, we are proposing these factors be considered
when initiating recovery actions. While it is appropriate to have the
OSC ensure these activities take place, it is ultimately the
responsibility of the responsible party to conduct these activities and
ensure that the agents are recovered from the environment. The Agency
requests comments on this proposed requirement.
(i) Reporting of Agent Use
The proposal includes a new requirement for the OSC to provide to
the RRT certain information after the use of a chemical or biological
agent within 30 days of completion of agent operations. The information
required in this report includes the information on any chemical or
biological agent used, including product name, the quantity and
concentration of the agent used during the response, the duration of
use, the locations where the agent was used, and any data collected and
analysis of efficacy or environmental effects. The proposal allows this
information to be provided in the OSC report to the NRT or RRT as
required under section 300.165 of the NCP, if such a report has been
requested. While other existing notification requirements serve to
activate an immediate response to an event, the proposed requirement
gathers information that will be useful in specifically evaluating the
use of chemical or biological agents in the response. It will also
inform the review of preauthorization plans and provide a basis for any
necessary changes to improve environmental protection. Given that
response and removal actions can greatly vary depending on the
discharge situation, the Agency requests comments on whether it would
be appropriate to allow the timeframe for submitting the report to be
agreed upon by the RRT, rather than establishing a set timeframe. The
Agency is requesting comments on this proposed new requirement,
including on the proposed timeframe.
3. Monitoring the Use of Dispersants
The goal of establishing a Schedule under the NCP is to protect the
environment from possible damage related to spill mitigating products
used in response to oil discharges. The proposal establishes a
regulatory approach under Subpart J that includes test data and
information requirements

[[Page 3394]]

for certain chemical and biological agents, procedures for authorizing
the use of those agents, and monitoring requirements for certain
discharge situations.
Each oil discharge represents a unique situation with distinct
conditions, which may require various response methods. When
dispersants are applied to an oil discharge, field monitoring can be
used to inform operational decisions by gathering site-specific
information on the overall effectiveness, including the transport and
environmental effects of the dispersant and the dispersed oil. The
revisions to product test data and information requirements are
intended to provide OSCs, RRTs, and ACs with the best information
available when selecting products for use on an oil discharge. While
laboratory test protocols allow for comparison between different
products under standardized laboratory conditions and may be useful
during the monitoring and assessment of a discharge event and/or for
selection of the agents used in the response, they do not necessarily
reflect field conditions. Monitoring of agents in the field informs the
OSC and other agencies on the overall effectiveness of dispersant use,
including the environmental effects and transport of dispersed oil.
The Agency believes that comprehensive monitoring in certain
discharge situations is necessary to determine the overall
effectiveness of dispersants and should transcend from the initial
dispersant application to include the transport and environmental
effects of the dispersant and dispersed oil in the water column.
Monitoring the overall effectiveness of dispersant use in the field
provides those Agencies with responsibility for authorizing the use of
dispersant product information for decision-making during subsurface or
prolonged surface dispersant applications. Adverse effects on
ecological receptors from exposures to dispersed oil depend on the
length of time and concentration of the exposure, which in turn is
dependent on the transport of dispersed oil. Because these exposures
may vary depending on the discharge situation, the Agency believes
comprehensive monitoring is important for certain discharge situations.
This monitoring data will enhance the information needed for an
effective response without delaying the use of agents under these
conditions.
Equipment is being contemplated to inject dispersants subsurface,
directly into the oil near the source of the discharge.\11\ This type
of application is intended to minimize dispersant dilution in the water
before the dispersant has had an opportunity to interact with the
oil.\12\ This application approach that is closer to the source is
expected to reduce potential adverse environmental consequences from
the use of excessive quantities of dispersants.\13\ However, applying
dispersant to an oil discharge does not result in the physical recovery
of oil from the environment. Instead, dispersing oil increases the
potential exposure of aquatic organisms to the dispersant-oil mixture,
at least transiently, and subsurface application has the potential to
more immediately and effectively increase these exposures near the
discharge. The Agency believes this new subsurface application approach
requires new environmental monitoring capabilities to support
operational decision-making. These new monitoring capabilities must be
able to meet the operational conditions (e.g., water depths,
temperatures) and be supported by knowledgeable personnel familiar with
them.
---------------------------------------------------------------------------

\11\ http://marinewellcontainment.com/expanded_system.php.
\12\ NRC, (2005), Oil Spill Dispersants: Efficacy and Effects,
The National Academies Press, pp. 138, http://www.nap.edu/catalog.php?record_id=11283.
\13\ Ibid.
---------------------------------------------------------------------------

The proposed rule adds Sec. 300.913 establishing requirements for
the responsible party to monitor any subsurface use of dispersant in
response to an oil discharge, surface use of dispersants in response to
oil discharges of more than 100,000 U.S. gallons occurring within 24
hours, and surface use of dispersants for more than 96 hours in
response to an oil discharge, as directed by the OSC. The purpose of
monitoring subsurface application is to characterize the dispersed oil,
follow the plume integrity and transport with the underwater current,
and identify and assess the potential adverse effects from the
dispersed oil. The proposal requires the responsible party to implement
monitoring for any subsurface dispersant use in response to an oil
discharge upon initiation and for the duration of subsurface dispersant
use. The Agency believes monitoring subsurface use of dispersants is
critical to inform response actions to minimize potential environmental
effects.
While surface application of dispersants is not a new approach and
understood for small, short duration discharges, the Agency believes it
is appropriate to require comprehensive monitoring for situations where
dispersants are used for an extended period of time or in cases of
major oil discharges. The Agency chose 100,000 U.S. gallons as a
threshold criterion for a major oil discharge because the NCP
classifies a discharge of more than this quantity to coastal waters as
major. In addition, EPA is proposing to this quantity monitoring of
dispersant use in response to major oil discharges occurring within 24
hours since a larger quantity of dispersant may be required in a short
time frame for an incident of this scale. The Agency also believes
comprehensive monitoring should be required when surface dispersant is
used for more than 96 hours because of potentially longer exposures of
biological aquatic resources to dispersant and dispersed oil. Further,
many acute toxicity studies use 96-hour exposure durations, including
the acute toxicity tests using Menidia beryllina described in this
proposal. While other toxicity tests have shorter exposure durations
(e.g., 24, 48, or 72 hours), the Agency believes 96 hours is a
reasonable threshold given its commonality of use in the toxicology
field. Therefore, the proposal requires a responsible party to
implement monitoring for surface dispersant use in response to an oil
discharge under these discharge conditions and for the duration of
dispersant use. The proposal also requires the submission of a Quality
Assurance Project Plan for approval to the OSC covering the collection
of all environmental data to ensure and maximize its quality,
objectivity, utility, and integrity. The Agency welcomes comments on
the proposed monitoring requirements, including the thresholds.
Specifically, the Agency requests comments on whether it should also
consider a threshold for surface use of dispersants that is based on
the quantity of dispersant used within a given timeframe. Alternative
thresholds must include a rationale in order for the EPA to consider
them for final action.
(a) Dispersant Application
The proposal requires the responsible party to document the
characteristics of the source oil; best estimate of the oil discharge
flow rate, periodically reevaluated as conditions dictate, including a
description of the method, associated uncertainties, and materials;
dispersant(s) product used, rationale for dispersant choice(s),
including the results of any efficacy and toxicity tests, recommended
dispersant-to-oil ratio; and the application method and procedures,
including a description of the equipment to be used, hourly application
rates, capacities, and total amount of dispersant needed. For
subsurface discharges, the proposal also

[[Page 3395]]

requires the responsible party to document the best estimate of the
discharge flow rate of any associated volatile petroleum hydrocarbons,
periodically reevaluated as conditions dictate, including as
description of the method, associated uncertainties, and materials.
This would provide the OSC with the necessary information for
operational decision-making and coordination of the dispersant
application monitoring.
Because of the many factors that influence the selection of a
dispersant product (e.g., its availability, the type of oil it will be
used on, the prevalent weather conditions, and the particular discharge
situations) the Agency proposes that the responsible party document its
product choice and selection rationale. Documenting the characteristics
of the source oil provides specific chemical data to identify the oil
associated with discharge and to inform decisions on dispersant use.
Documenting application methods and procedures ensures that dispersant
use is consistent with the dispersant manufacturer's recommended
concentrations, and conditions provided as part of the data
requirements for listing the product on the Schedule. Documenting
results of any additional efficacy and toxicity testing, or available
data or information specific to the area or site conditions will assist
the OSC in establishing the appropriateness of the dispersant choice.
Documentation and clear understanding of the estimated daily oil
discharge flow rate and the recommended dispersant-to-oil ratio (DOR)
allows a dispersant rate to be established that would aid the OSC in
determining the adequate dispersant usage. The OSC can compare the
recommended DOR to the manufacturer's recommended application
concentration to ensure it is within the recommended range or to
provide an opportunity for the responsible party to explain any
deviations that may arise due to operational considerations.
The biodegradation of petroleum constituents may result in a
reduction in the dissolved oxygen concentration in the water column
that could lead to hypoxia, which could be detrimental to marine
organisms. The best estimate of the oil discharge flow rate,
periodically reevaluated as conditions dictate, is an important
consideration for monitoring dispersant use since the estimated amount
of oil discharged may be used to provide insight into the potential
oxygen demand exerted on the water column and to characterize the
potential oil distribution. The proposal would also require the
responsible party to document the best estimate of the discharge flow
rate of any associated volatile petroleum hydrocarbons for subsurface
applications. Volatile petroleum hydrocarbons (e.g., methane, and low
molecular weight alkanes such as ethane, propane, and butane)
associated with the discharge could contribute to a reduction in
dissolved oxygen as a result of microbial degradation. The Agency is
not proposing this requirement for surface applications given these
compounds are expected to readily evaporate, making it unlikely they
would be incorporated into the water column in quantities that would
result in hypoxia.
The proposal requires the documentation of the dispersant
application method and procedures to include a description of the
equipment to be used, including hourly application rates, capacities,
and total amount of dispersant needed. Dispersant and equipment should
be available to maintain the hourly dispersant application rate without
significant deviation from the set rate. The Agency believes this
information will assist in ensuring a consistent dispersant application
rate. Dispersant application rates outside of established parameters
may result in their over or under use, altering their effectiveness.
Significant fluctuations in dispersant application rates could also
indicate equipment malfunctions, requiring a reassessment of the
response technique. EPA welcomes comment on the proposed requirements
for dispersant application. Alternatives must include a rationale in
order for the Agency to consider them for final action.
(b) Water Column Sampling
The proposal requires the responsible party to collect
representative background samples from the water column at the closest
safe distance determined by the OSC from the discharge, and in any
direction of likely transport. The sampling should consider surface and
subsurface currents and oil properties. Establishing background
information prior to oil contamination from the discharge source
provides reference data to compare against the results from water
samples taken during the response. In establishing the background
information, the responsible party should consider other potential
sources of petroleum hydrocarbons (e.g., natural seeps) in the water
column. The background samples would be collected in areas not affected
by the discharge of oil throughout the water column upon initiation of
dispersant use, at the closest safe distance as determined by the OSC
from the oil discharge. Sampling would be conducted in any direction of
likely transport considering surface and subsurface currents and the
oil properties in those areas. The responsible party should consider
using trajectory models that incorporate relevant factors such as oil
type to determine the likely direction of the dispersed oil to inform
where the water samples should be collected.
The Agency is requiring that sample collection follow established
standard operating and quality assurance procedures that are reliable
and defensible. An accurate assessment of environmental data depends on
the reliability, timeliness, and integrity of the data collected.
Standard operating procedures should describe the appropriateness of
the sampling method; the equipment needed for sample collection; a
description of potential interferences, problems that may be
encountered and corrective actions that would be taken; the sample
collection procedure, including the preparation steps, representative
sampling considerations, and sampling steps for each sampling device
used; sample preservation, containers, handling, and storage;
decontamination of sampling equipment; and record keeping and quality
control procedures. These elements are generally described in various
guidance documents on standard operating and quality assurance
procedures for environmental sampling.^{14 15}
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\14\ http://www.epa.gov/quality/qa_docs.html.
\15\ http://www2.epa.gov/region8/environmental-sampling.
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In addition to the background water sample collection, the proposal
requires the responsible party to collect water column samples daily in
the dispersed oil plume at such depths and locations where dispersed
oil is likely to be present. EPA believes the dispersed oil plume
captures the presence of oil from either the subsurface or the surface
application of dispersant, including where oil could be rising to the
surface from a subsurface discharge or the dispersed oil plume at the
water surface as a result of surface dispersant application. The
responsible party also would need to analyze for:
In-situ oil droplet size distribution analysis, including
the mass or volume mean diameters between droplet sizes ranging from
2.5 to 2000 [mu]m, with the majority of data collected between the 2.5
and 100 [mu]m sizes. Droplet size distribution, which is an important
component to understanding the chemical and hydrodynamic effectiveness
of dispersants, can be measured with devices such as the Laser

[[Page 3396]]

In-Situ Scattering and Transmissometry (LISST) instrument or other
similar instruments. Small oil droplets (e.g., diameters in the tens of
[mu]m range) have such low rise velocities that they tend to remain
suspended in the water column (neutrally buoyant), where they can
become widely dispersed by advective forces, turbulent motion, and to a
lesser extent diffusion. These small droplets are more readily amenable
to biodegradation due to their higher surface area to volume ratio. In
contrast, large oil droplets (e.g., diameters >100 [micro]m) will tend
to recoalesce and rise faster to the surface.\16\ Effective application
of dispersants is expected to generate a larger number of small
droplets, reducing the average droplet size.\17\ This will change the
trajectory of rising oil that is subjected to stratified horizontal
subsurface currents. Near the water surface, hydrodynamic and other
environmental factors also influence the oil droplet size distribution.
Mixing energy, especially from breaking waves, dictates the breakup of
large oil droplets into smaller droplets and the depth of submergence
of the droplets. Plunging breaking waves under experimental conditions
produced the smallest oil droplets.^{13 14} Additionally,
studies indicate that the type of chemical dispersant used is an
important factor in controlling the dispersed oil droplet size
distributions. Further, wave tank studies have shown that the
chemically dispersed oil may result in a droplet size distribution that
has not been observed without the use of dispersants (i.e., physically
dispersed oil), both in terms of a smaller volumetric mean diameter and
a bimodal distribution for droplet size diameters below 100 [mu]m.\18\
EPA recognizes that the aforementioned studies were conducted under
conditions characteristic of surface waters. However, the effect of the
high velocities of oil that may occur from a discharge from a
subsurface oil well on the oil droplet size distribution requires
further scientific investigation to understand the contribution of
physically dispersed oil relative to chemically dispersed oil. In
either event, it is clear droplet size distribution analysis provides
important data useful in optimizing operational guidelines and decision
making, modeling transport and fate, and potentially evaluating
biological effects of chemically dispersed oil. The proposal also
includes larger oil droplet sizes of up to 2000 [mu]m, intended to
provide information that can inform the oil distribution using
trajectory modeling analysis.
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\16\ Li, M. and Garrett, C., (1998) The Relationship Between Oil
Droplet Size and Upper Ocean Turbulence, Mar. Poll. Bull., Vol. 36,
pp. 961-970.
\17\ Li, Z., Lee, K., King, T., Boufadel, M.C., Venosa, A.D.,
(2008) Assessment of Chemical Dispersant Effectiveness in a Wave
Tank under Regular Non-Breaking and Breaking Wave Conditions, Mar
Pollut Bull, Vol. 56, pp. 903-912.
\18\ Li, Z., Lee, K., King, T., Boufadel, M.C., Venosa, A.D.,
(2009) Evaluating Chemical Dispersant Efficacy in an Experimental
Wave Tank: 2--Significant Factors Determining In Situ Oil Droplet
Size Distribution, Env Eng Scien, Vol. 26, pp 1407-1418.
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In-situ fluorometry. When exposed to ultraviolet (UV)
light, certain compounds absorb energy that can elevate electrons into
an excited higher energy level. The wavelength that excites electrons
into a higher energy state is typically referred to as the excitation
wavelength. Electrons unstable at the higher energy state return to a
lower energy state, emitting energy at longer emission wavelengths
resulting in fluorescence.\19\ Many organic compounds fluoresce at
specific excitation and emission wavelengths that allow for identifying
many of the components of dissolved organic matter and other compounds
(e.g., crude oil) in seawater.\20\ For crude petroleum oils, the
aromatic fraction is responsible for the fluorescence property of
petroleum, and these compounds are used to determine the specific
excitation and emission wavelengths for monitoring. When subject to
excitation at certain wavelengths in the near ultraviolet spectrum,
polycyclic aromatic hydrocarbons (PAH) fluoresce over a range of higher
wavelengths, depending on the number of aromatic rings in the
structure.\21\ Fluorometers can be targeted to the type of oil
discharged, and the excitation and emission wavelengths chosen should
match the aromatic properties of the oil discharged. Although this
measure does not include all oil constituents, fluorescence is a
valuable screening tool deployed during a response,\22\ providing a
rapid indication of potential dispersed oil in the water column, as
well as an indicator of dispersion effectiveness as discussed in the
following section. The Agency request comments on alternative
spectroscopy techniques such as absorption measurements that may be
used to rapidly estimate oil concentrations in the water during a
discharge event.
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\19\ Henry, C.B., Roberts, P.O., Overton, E.B., A Primer on In
Situ Fluorometry to Monitor Dispersed Oil, IOSC 1999;246.
\20\ Coble, P.G., (2007) Marine Optical Biogeochemistry: The
Chemistry of Ocean Color, Chem. Rev., Vol. 107, pp. 402-418.
\21\ Bugden, J.B.C., Yeung, C.W., Kepkay, P.E., Lee, K. (2008)
Application of Ultraviolet Fluorometry and Excitation-Emission
Matrix Spectroscopy (EEMS) to Fingerprint Oil and Chemically
Dispersed Oil in Seawater, Mar Pollut Bull, Vol. 56, pp. 677-685.
\22\ Conmy, R.N., Coble, P.G., Farr, J., Wood, A.M., Lee, K.,
Pegau, W.S, Walsh, I.D., Koch, C.R., Abercrombie, M.I., Miles, M.S,
Lewis, M.R., Ryan, S.A., Robinson, B.J., King, T.L., Kelble, C.R.,
and Lacoste, J. (2014) Submersible Optical Sensors Exposed to
Chemically Dispersed Crude Oil: Wave Tank Simulations for Improved
Oil Spill Monitoring, Environ Sci Technol, Vol. 48, pp. 1803-1810.
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Fluorescence signatures. In addition to in-situ
fluorometry, the proposal requires the responsible party to conduct a
fluorescence intensity analyses on water samples collected to determine
fluorescence signatures of the dispersed oil. EPA proposes to use
fluorescence signatures as a relatively simple and rapid means to
assess dispersion effectiveness. This includes but is not limited to,
identifying the peak wavelength position, magnitude and ratios of
fluorescence intensity of the dispersed oil. For example, measuring the
reduction in an intensity ratio after applying dispersant to the oil in
seawater may provide an estimate of the effect of chemical
dispersion.^{23 24} Ratios of fluorescence intensity are
derived from the three dimensional excitation/emission matrix spectra
(EEMS) acquired by combining multiple emission spectra obtained from
oil exposed to individual excitation wavelengths typically using a
scanning spectrofluorometer. If the optimal excitation and emission
bands are known, then these ratios may be derived from measuring the
fluorescence intensity at two different fixed emission wavelengths at a
single fixed excitation wavelength. The ratios are calculated by
dividing the fluorescence intensity of the shorter emission band by the
fluorescence intensity of the longer band. Studies have shown that
adding dispersants to crude petroleum oil increases the fluorescence
intensity of the longer emission band, driving down the value of the
ratio. Although individual petroleum oils may have common spectral
characteristics, the ideal three-dimensional EEMS for the discharged
oil should be obtained from scanning the source oil. Therefore, the
monitoring should include procedures to obtain the EEMS using the
source oil to determine the optimal excitation-emission wavelengths.
The Agency

[[Page 3397]]

request comments on alternative techniques or measurements that may be
used to rapidly assess dispersion effectiveness during a discharge
event.
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\23\ Bugden, J.B.C., Yeung, C.W., Kepkay, P.E., Lee, K. (2008)
Application of Ultraviolet Fluorometry and Excitation-Emission
Matrix Spectroscopy (EEMS) to Fingerprint Oil and Chemically
Dispersed Oil in Seawater, Mar Pollut Bull, Vol. 56, pp. 677-685.
\24\ Kepkay, P.E., Yeung, C.W., Bugden, J.C.B., Li, Z., and Lee,
K. (2008) Ultraviolet Fluorescence Spectroscopy (UVFS): A New Means
of Determining the Effect of Chemical Dispersants on Oil Spills,
IOSC, pp. 639-644. http://ioscproceedings.org/doi/abs/10.7901/2169-3358-2008-1-639.
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Dissolved oxygen (DO). Dissolved oxygen is an important
variable to monitor in the application of dispersants, particularity in
subsurface waters that may inform operational decisions. For surface
dispersant application, dissolved oxygen is expected to be higher in
the mixed layer in the surface water. Dissolved and/or dispersed oil
represents a readily available carbon source for microbial oxidation,
and this metabolic activity can lead to a decrease in the DO content in
the water column. The oil degrading community in the water is an
important DO sink for the mass transfer of hydrocarbons in the
subsurface, and advantage can be taken of this fact during a response.
The decline in DO due to hydrocarbon biodegradation could approach or
exceed levels of concern (i.e., hypoxia) and thus be detrimental to
surrounding organisms (e.g., invertebrates and vertebrates). Dissolved
oxygen, which relies on the diffusion of molecular oxygen through a
membrane in the sensor, is commonly measured during oceanographic
survey cruises using an in-situ DO instrument that provides real-time
results. However, a DO sensor instrument that passes through a
dissolved and/or dispersed oil layer is subject to contamination by the
oil and could lead to questionable measurements if such fouling of the
electrodes occurs, particularly at depths where the dissolved and/or
dispersed plume depth are expected to coincide with depressions in
dissolved oxygen. Therefore, the Agency is concerned that relying
solely on measurements from in-situ oxygen instruments may lead to an
erroneous interpretation of oxygen data. Thus, the Agency believes that
ex-situ confirmatory DO measurements should also be conducted using
Winkler titrations to confirm in-situ dissolved oxygen measurements.
Total petroleum hydrocarbons, individual resolvable
constituents, including volatile organic compounds, aliphatic
hydrocarbons, monocyclic, polycyclic, and other aromatic hydrocarbons,
including alkylated homologs, and hopane and sterane biomarker
compounds. The Agency is proposing that the responsible party analyze
each water sample collected for total petroleum hydrocarbons (TPHs),
individual resolvable constituents, including volatile petroleum
hydrocarbons, and branched and normal aliphatic hydrocarbons. The
analysis would also include monocyclic, polycyclic and other aromatic
hydrocarbons (e.g., heterocyclic aromatic hydrocarbons), including
their alkylated homologs, and hopanes and steranes biomarker compounds.
TPHs are best measured using gas chromatograph (GC) equipped with a
flame ionization detector (FID). TPH analysis measures total alkanes
and aromatics, can be obtained relatively quickly, and provides a good
measurement for initial screening. Given that PAHs and biomarkers are
typically measured using GC/MS, the proposal includes GC/MS analysis to
provide the alkanes, PAHs, and biomarker (e.g., hopane) specificity
important in identifying certain oil constituents that may be present
in the oil discharge. Identifying the concentrations of PAHs and
biomarkers assists responders in making informed operational decisions
regarding the dispersant application because these compounds can be
compared against the composition of the source oil, which serves as a
reference to determine the degree of weathering for oil.
Carbon Dioxide (subsurface only). The aerobic
biodegradation of oil constituents not only consumes dissolved oxygen,
but would also produce carbon dioxide. Increases in the concentration
of carbon dioxide that coincide with decreases in the concentration of
dissolved oxygen would provide credible evidence that biodegradation of
oil is occurring. Thus, the Agency believes that measuring the in-situ
carbon dioxide for subsurface dispersant applications would be a good
indicator of microbial oxidation and inform the OSC on the potential
fate.
Methane if present (subsurface only). The microbial
degradation of methane may contribute to a reduction in dissolved
oxygen. Thus, the Agency believes that, when present, subsurface in-
situ methane measurements are an important factor to consider in
evaluating dissolved oxygen levels.
Heavy metals analysis, including nickel and vanadium.
Crude petroleum oil may contain certain heavy metals, including nickel
and vanadium.^{25 26 27} Dispersing oil may increase the
bioavailability of certain associated heavy metals to marine organisms.
Therefore, the Agency is proposing to include heavy metal analysis as
part of the sampling analyses to be conducted.
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\25\ Barwise, A. J. G. and Whitehead, E. V. (1980). Separation
and Structure of Petroporphyrins. In: Advances in Organic
Geochemistry 1979. (A. G. Douglas and J. R. Maxwell, eds.),
Pergamon, New York, pp. 181-92.
\26\ Barwise, A. J. G. (1990). Role of Nickel and Vanadium in
Petroleum Classification. Energy & Fuels, 4, 647-52.
\27\ All, M.F., Bukharl, A., and Saleem, M., (1983) Trace Metals
in Crude Oils from Saudi Arabia, Ind. Eng. Chem. Prod. Res. Dev.
1983, Vol 22, pp. 691-694.
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Turbidity. Turbidity is a general measure of water
clarity. Turbidity is determined by measuring how much material
suspended in water decreases the passage of light through the
water.\28\ Suspended materials may include soil particles (clay, silt,
and sand), algae, plankton, microbes, and other substances. This
measure provides a quick assessment of suspended materials in receiving
waters from other water bodies and is useful in determining the
presence of materials that could interfere with oil particle size
determinations. Alternatively, the Agency is requesting comments on
whether there are other physical measurements in the water that would
provide similar timely information, or that can serve as validation for
turbidity values collected in situ.
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\28\ http://water.epa.gov/type/rsl/monitoring/vms55.cfm.
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Water temperature. Water temperature typically is measured
using an electronic thermometer on the conductivity-temperature-depth
(CTD) instrument. When combined with salinity and pressure, temperature
measurements are used to calculate water density, which may change
along the vertical profile. Along with the horizontal subsurface
currents and the rise velocity of the dispersed oil, the ambient
density gradient is an important factor in determining the behavior of
dispersed oil in the water column. Water temperature is also an
important variable that may influence the effectiveness of dispersant
applications. For example, cold temperatures may, among other
environmental factors, impact the effectiveness of dispersants as it
affects certain oil properties (e.g., viscosity). Colder temperatures
also may affect the degree of oil weathering (e.g., evaporation), and
the amount of dispersant/oil mixing energy (wave action) needed to
effectively disperse oil relative to warmer temperatures.
pH. The pH is a simple standard measurement used to
analyze water quality that can affect chemical or biological processes
in water. pH also determines the solubility and biological availability
of chemical constituents such as heavy metals.
Conductivity. Conductivity is measured by passing a
current through the water in a CTD instrument, which is then compared
against known salinities to obtain the water salinity. When combined
with temperature, and pressure, salinity measurements are

[[Page 3398]]

used to calculate water density, which may change significantly along
the vertical profile. Along with the horizontal subsurface currents and
the rise velocity of the dispersed oil, the ambient density gradient is
an important factor in determining the behavior of dispersed oil in the
water column.

The Agency requests comment on the proposed approach to water column
sampling. Alternatives must include a rationale in order for the Agency
to consider them for final action.
(c) Oil Distribution Analyses
The proposal requires that the responsible party, in consultation
with the OSC and using best available technologies, characterize the
dispersant effectiveness and oil distribution, considering the
condition of the oil, dispersant, and dispersed oil components from the
discharge location. EPA believes this is necessary to inform sampling
locations by assessing the horizontal and vertical boundaries of the
dispersed oil plume and the direction of likely transport. The majority
of the sampling can then be focused on known or suspected locations and
depths of the dispersed oil. Based on the initial water sampling
results to characterize the boundaries of the dispersed oil, the
sampling design can be tailored to optimize sampling. The Agency
proposes that the responsible party characterize the dispersant
effectiveness to determine the changes in the condition of the oil due
to weathering, which can include changes in oil viscosity due to water
uptake (e.g., mousse). Weathered oil that mixes with water may result
in significant emulsification (e.g., water-in-oil emulsions), which in
turn may decrease the dispersant's chemical effectiveness and diminish
biodegradability. Therefore, the characterization of dispersant
effectiveness should provide a reasonable estimate to the extent (e.g.,
distance from the discharge source) in which the dispersant can be
applied to the oil and still be effective. The Agency believes this
will result in better dispersant applications and minimize excessive
dispersant use. The Agency requests comment on this approach.
Alternatives posed must include a rationale for the Agency to consider
them for final action.
(d) Ecological Characterization
The Agency proposes that the responsible party characterize the
ecological receptors (e.g. aquatic species, wildlife, and/or other
biological resources), their habitats, and exposure pathways that may
be present in the discharge area, in consultation with the OSC.
Exposure pathways, such as ingestion, refer to the way in which
ecological receptors may come into contact with discharged oil and
result in exposure that would be detrimental to ecological receptors.
The Agency believes that the ecological characterization should include
those species that may be in sensitive life stages, transient or
migratory species, breeding or breeding-related activities (e.g.,
embryo and larvae development), and threatened and/or endangered
species that may be exposed to oil, dispersed oil, and dispersant,
which in turn will assist the OSC in managing response actions,
including those actions that were determined not to be needed. In
developing the characterization of ecological receptors, the
responsible party may refer to relevant sources of information such as
applicable expedited decision-making plans, environmental assessments
or statements, Federal and state environmental databases (e.g., ACP--
Fish and Wildlife and Sensitive Environments Annex; NOAA--Environmental
Sensitivity Indices; NOAA--NMFS Southeast Area Monitoring and
Assessment Program; EPA--National Coastal Assessment \29\) or through
studies conducted by universities or other research-oriented
institutions.
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\29\ http://www.epa.gov/emap/nca/.
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The proposal requires the responsible party to consult with the OSC
to determine an acute toxicity level of concern for the dispersed oil
using available dose/response information relevant to potentially
exposed species. The envisioned approach would be to monitor acute
toxicity in the water column concurrently with dispersed oil sampling
for fluorometry, particle size, and water quality (e.g., dissolved
oxygen). The TPH concentrations in water samples taken throughout the
water column could then be compared to TPH-based ecotoxicity benchmarks
(EBs). Water samples collected for comparison of aqueous TPH
concentrations to EBs would be analyzed and reported within the
timeframe necessary to make operational decisions (e.g., within 24
hours of collection). Sampling could also be performed in areas without
dispersant application to distinguish toxicity associated with
physically dispersed oil from that of chemically dispersed oil.
While EBs may have already been established during the development
of contingency plans, they can also be derived at the time of an
incident. One approach is to use a species sensitivity distribution
(SSD),\30\ which allows for species relevant to the location of the
discharge to be considered. An SSD is a probability distribution of the
sensitivity of a group of species to a toxicant.\31\ SSDs could be
developed for representative oils (e.g., crude oils) using existing
acute toxicity values for mortality or immobility (e.g., 48 and 96 hr
LC50) where sufficient species diversity are available
(e.g., toxicity data for 10 or more species). For example, the EBs
could be computed from the fifth percentile of the SSD as the hazard
concentration 5 percent (HC5), as they are considered protective of 95%
of species, have been used by EPA for developing ambient water quality
criteria, and are generally accepted by the international
community.\32\ Chronic toxicity benchmarks may be derived applying
safety factors to the acute toxicity EBs. The Agency requests comments
on the proposed approach to ecotoxicity assessment, and whether it
should consider making SSDs a requirement for deriving EBs. If
alternative approaches are suggested, the commenter must include an
appropriate rationale in order for the Agency to consider them for
final action.
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\30\ Barron, M.G., Hemmer, M.J., and Jackson, C.R., (2013)
Development of Aquatic Toxicity Benchmarks for Oil Products Using
Species Sensitivity Distributions, Integr Environ Assess Manag, Vol.
9, pp. 610-615.
\31\ Aldenberg, T. and Jaworska, J.S., (2002) Uncertainty of the
Hazardous Concentration and Fraction Affected for Normal Species
Sensitivity Distributions, Ecotox and Environ Safety, Vol. 46, pp.
1-18.
\32\ Barron, M.G., and Wharton, S., (2005) Survey of
Methodologies for Developing Media Screening Values for Ecological
Risk Assessment, Integrated Environmental Assessment and Management,
Vol. 1, pp. 320-332.
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(e) Immediate Reporting
The proposal requires the responsible party to immediately report
to the OSC any deviation of more than 10 percent of the mean hourly
subsurface dispersant use rate for the total dispersant volume
authorized for that 24 hour use, and the reason for the deviation
(e.g., equipment malfunction). The Agency believes that inconsistent
dispersant application rates confound data sampling interpretation due
to variations in the DOR. The proposal, however, provides a margin for
variation within 10 percent of the mean hourly subsurface dispersant
application rate to account for equipment performance. The Agency
believes this margin to adequately account for variations in dispersant

[[Page 3399]]

injection equipment without being overly restrictive. EPA requests
comments on whether it should consider a similar requirement for
dispersant surface application.
The Agency also is proposing to require the immediate reporting of
ecological receptors, including any threatened or endangered species
that may be exposed to dispersed oil based on trajectory modeling and
the estimated acute toxicity level of concern. Results from daily
sampling (e.g., droplet size distribution, TPH) would provide input
data to refine predictions of the likely dispersed oil direction using
trajectory modeling. Further, results may also inform decisions to
alter dispersant application in order to minimize effects on biological
resources.
(f) Daily Reporting
The proposal requires daily reporting of sampling and data analyses
collected within the timeframe necessary to make operational decisions
(e.g., within 24 hours of collection), including documented
observations, photographs, video, and any other information related to
dispersant use, unless an alternate timeframe is authorized by the OSC.
Daily reporting would also include the total amount of dispersant used
for the previous reporting period. Additionally, the proposal would
require a schedule for any data analyses that require time beyond 24
hours due to analytical methods; this schedule is not to exceed 120
hours (i.e., 5 days) unless authorized by the OSC. Timely sample
analyses afford the OSC and other responders with multiple relevant
data that can be analyzed together to inform situational awareness of
dispersant operations and adjust dispersant application if necessary.
The Agency believes that a 120-hour window for analyses requiring
additional time provides an adequate opportunity to conduct all
requested analyses in a timely manner without being overly restrictive.
Finally, the proposal requires the responsible party to report the
estimated daily transport of dispersed and non-dispersed oil, and
associated volatile petroleum hydrocarbons if applicable, and
dispersants, using the best available trajectory modeling. This
information is intended to assist response planners to coordinate
response activities and to schedule monitoring activities based on the
expected transport of oil and dispersed oil.
4. Data and Information Requirements for Product Schedule Listing
The Agency is proposing to revise the data and information
requirements for listing products on the Schedule in Sec. 300.915 of
Subpart J. The proposed amendments revise the efficacy and toxicity
testing protocols and listing criteria for all chemical and biological
agents on the Schedule. Additionally, the Agency proposes revisions to
the requirements for general product information, Confidential Business
Information (CBI) claims, submission package contents, EPA review and
listing procedures, requests for decision review, changes to products,
transitioning products from the current Schedule to the new Schedule,
mandatory product disclaimer, and removal of products from the
Schedule.
(a) General Product Information
The Agency is proposing to consolidate the general submission
requirements applicable to all types of agents that may be listed on
the Schedule in paragraph (a) of Sec. 300.915. Subsequent regulatory
paragraphs in this section are proposed to include requirements
specific to each product category. Additionally, the Agency is
proposing to require some additional information, as applicable,
regarding products that are submitted for Schedule listing
consideration. The proposed general information requirements for all
products are proposed to be revised as follow:
Submitter: Name, physical address, email, telephone
number, identity of submitter (i.e., manufacturer, vendor, importer,
distributor, designated agent for the manufacturer), and documentation
of such identity.
General Product: All name(s), brand(s), and/or
trademark(s) under which the product is to be sold; Safety Data Sheet
(SDS); sample product labels for all name(s), brand(s), and/or
trademark(s); chemical or biological agent categories under which the
product is submitted for listing, including information on the specific
process(es) through which the product affects the oil, and the specific
environment (waters and/or adjoining shorelines) on which it is
intended to be used.
Supplier: Names, physical addresses, emails and telephone
numbers of the primary distributors, vendors, importers, and/or
designated agent acting on behalf of the manufacturer.
Product Storage: Maximum, minimum and optimum temperature,
humidity and other relevant conditions for product storage; impact on
product performance if the product is not stored within recommended
limits; and anticipated shelf life at the recommended storage
conditions.
Product Use: Recommended procedures, including product
concentrations, application ratios, types of application equipment,
conditions for use, and any application restrictions. The procedures
must address variables such as weather, water salinity, water
temperature, types and weathering states of oils or other pollutants,
and product and oil containment, collection, recovery and disposal, and
include supporting documentation and standard methods used to determine
them.
Environmental Fate: Known measured data and supporting
documentation on the persistence, bioconcentration factor,
bioaccumulation factor, and biodegradability of the product and all of
its components.
Physical/Chemical Properties and Formulation: Physical
state and appearance; vapor pressure; flash point; pour point;
viscosity; specific gravity; particle size for solid components; pH;
citation of standard methods used to determine the physical/chemical
properties; identity of all components in the product, including each
specific component name; corresponding Chemical Abstract Service (CAS)
Registry Number; the maximum, minimum, and average weight percent of
each product component; and the intended function of each component
(e.g., solvent, surfactant).
For products that contain microorganisms, enzymes and/or
nutrients: All microorganisms and weight percent by current genus and
species, including any reclassifications; all enzymes and their
International Union of Biochemistry (I.U.B.) number(s); Enzyme
Classification (EC) code numbers; the source of each enzyme, units, and
specific oil-degrading activity; name(s) and maximum, minimum, and
average weight percent of the nutrients contained in the product;
citation or description of the methodology used to determine product
components; certification, including data, methodology, and supporting
documentation, indicating that the product does not contain levels that
exceed the National Ambient Water Quality Criteria lowest density value
for the following: Bacterial, fungal, or viral pathogens or
opportunistic pathogens, including, but not limited to, enteric
bacteria such as Salmonella, fecal coliforms, Shigella, Coagulase
positive

[[Page 3400]]

Staphylococci, and Beta Hemolytic Streptococci or enterococci.
National Water Quality Standard Contaminants:
Certification, including data, methodology, and supporting
documentation, indicating that the product does not contain levels that
exceed the National Water Quality Standards lowest aquatic life acute
value for the following contaminants: Metals reasonably expected to be
in the product including arsenic, cadmium, chromium, copper, lead,
mercury, nickel, vanadium, zinc; cyanide; chlorinated hydrocarbons;
pesticides; polychlorinated biphenyls (PCBs); and polynuclear aromatic
hydrocarbons (PAHs).
Certification, including data, methodology, and supporting
documentation, indicating that the product does not contain prohibited
agents (sinking agents, nonylphenol, or nonylphenol ethoxylates).
Testing Laboratory Information: Name, address, contact
name, email, phone number; national or international accreditations.
Laboratory Testing Data and Reports: All applicable
information, data and analysis specified in the testing protocols,
including raw test data and replicates, notes and observations,
calculated mean values and standard deviations, summary of stock
solution preparation, source and preparation of test organisms, test
conditions, and chain of custody forms.
Production capacity: Estimated annual production volume;
average and maximum volume per day; time needed to reach that maximum
production rate (days).
Performance Capabilities/Benefits: Recognition received
from, if applicable; national and/or international product testing or
use data, recognitions (e.g., EPA's Design for the Environment), and/or
certifications, informing the performance capabilities or environmental
benefits of the product.
The proposed revisions group together and simplify the general
submission requirements applicable to all product types. EPA believes
reorganizing the general requirements in a central location will
clarify which requirements are applicable to all submissions, and which
are specific to each product type by including them in separate
sections. While most of the information listed above is currently
required to be submitted under Subpart J, the Agency is proposing
revisions to several of the existing general requirements and several
new data and information requirements. The Agency believes the proposed
revisions and added new requirements will better characterize the
nature of the product and will assist EPA in product listing decisions.
The information will also assist the RRTs in their area planning
activities, and the OSCs in authorizing the appropriate use of chemical
and biological agents. Details on the proposed additions and revisions
are as follow:
(1) Identification and documentation by the submitter of its status
in relationship to the product as the manufacturer, vendor, importer,
distributor, or other designated agent of the manufacturer. This
proposed requirement is intended to clearly establish the point of
contact responsible for the submission, and to avoid any conflicts or
claims from unauthorized entities on products listed or submitted for
consideration.
(2) Chemical or biological agent categories under which the product
is submitted for listing, including information on the specific
process(es) through which the product affects the oil, and the specific
environment(s) (water and/or adjoining shorelines) on which it is
intended to be used. Currently, when a product meets the definitions of
two or more product categories, a submitter must provide technical
product data for each of those product categories. After review of the
submitted technical product data, EPA makes a determination on whether
and under which category the ``mixed product'' should be listed on the
Schedule. It has been Agency policy to list products only under one
category to avoid confusion in the field during a response, and because
the process(es) through which the products affect the oil for different
product categories do not generally overlap or allow for multiple uses
of one product. However, EPA has received comments from responders,
vendors, and manufacturers who believe that it is appropriate for
certain products to be listed under more than one category. The Agency
is proposing to revise the current limitations for mixed products. The
proposal allows for products to be considered under multiple categories
provided they meet all of the listing requirements for each. To this
end, the Agency is also requiring that information be provided
identifying which environments the product is intended to be used for,
in the water and/or on the shoreline. EPA is soliciting comments on the
issue of multiple category product listing.
(3) Copy of the Safety Data Sheet (SDS) required by the
Occupational Safety and Health Administration (OSHA) under their Hazard
Communication Standard (HAZCOM) for the product. EPA recognizes that
chemical and biological agents may contain substances that could cause
harm to oil spill responders who, if unaware of the product's formula,
may not wear the proper personal protective equipment. SDSs describe
the hazards that may be involved with the product and recommend safety
measures that would minimize or avoid adverse consequences that may
result from exposures. The Agency believes SDS information will be
useful to both OSCs and responders when authorizing and using the
product respectively, and that adding this new requirement for a
product SDS is appropriate. While the Agency believes that the relevant
SDS information should be that of the product, we request comment on
the value for responders of requiring an SDS for each individual
component. The Agency requests comments on this new requirement, as
well as whether the submitter should provide any additional information
on potential adverse human health effects based on the product's
formula and application methods not captured in the SDS, and how to
best communicate this information to product end users.
(4) Sample product label for all names, brands, or trademarked
versions of the product that include the manufacture and expiration
dates of the product, as well as the conditions for storage. The Agency
would be allowing flexibility in complying with this requirement by
specifying that the submitter does not need to affix new labels to
comply with this section if existing labels already convey the required
information. This proposed requirement is not intended in any way to
supersede any other federal labeling requirement in place (e.g., OSHA's
HAZCOM). The proposed requirement is intended to assist the OSC in
ensuring that the product used to respond to an incident is still
viable and effective, and the oil spill response organizations (OSROs)
or any other responder that is storing the product to ensure that their
stockpile is viable and available to be authorized for use.
(5) Recommended product use procedures. The Agency is proposing to
revise the requirement for providing information on the recommended
application procedures. While the proposal is maintaining the specific
elements included in the current requirement, the supporting
documentation and information on the standard methods the product
manufacturer used to establish the procedures is requested. EPA
believes that providing detailed information on the recommended product
use

[[Page 3401]]

procedures is necessary to inform the OSC when authorizing these
products. This supporting documentation and specific information on the
methods and standards used to establish them will inform OSCs and other
response personnel in selecting products that can be effectively used
under the operating conditions encountered for any given incident. The
Agency requests comment on the revised data requirement, and whether
there are other elements that should also be included to ensure the
proper use and application of the products.
(6) Environmental fate information. The Agency is proposing to
request any known and available measured data and supporting
documentation on the persistence, bioconcentration factor,
bioaccumulation factor, and biodegradability of the product and all of
its components. The Agency currently has no restriction on use of
persistent bio-accumulative products. The Agency considered
requirements using existing testing protocols and modeling approaches
to establish thresholds for listing based on bioconcentration factors
(BCF) or bioaccumulation factors (BAF). These factors offer ratios of
the concentration of a particular chemical in a biological tissue per
concentration of that chemical in water surrounding that tissue, or in
the environment respectively. The Agency considered a tiered testing
approach, where the submitter would provide known BCF/BAF information
for listing purposes, but would also be required to provide testing
based on application rates authorized for use. That is, the lower
application rates would only require existing information or the use of
existing EPA models, while higher rates would require additional
testing of fish, bivalves, and earthworms, as needed.
Similarly, there are no restrictions on the use of environmentally
persistent products. The Agency considered requiring the submitter to
use estimation techniques/models, such as the EPA model EPI
Suite^TM, which estimates environmental fate properties
(breakdown in water or air, etc.) that can indicate where a chemical
will go in the environment and how long it will stay there. A tiered
testing approach for larger quantity/duration spills as discussed above
for bioconcentration and bioaccumulation was also considered.
EPA believes environmental fate information is necessary to inform
the OSCs when authorizing these products for use, given the potential
for their extended use in significant quantities. However, given that
the Agency can estimate these factors, it is only proposing to require
that available information or data be submitted on the product rather
than specific product testing, as specific product testing for these
factors can add significantly to the testing cost for each product. The
Agency requests comment on whether testing for products'
bioconcentration, bioaccumulation and biodegradation should be required
for listing purposes. Additionally, the Agency requests comment on
whether thresholds for BCF and BAF should be established for listing a
product on the Schedule.
(7) New physical/chemical properties and removal of the
incorporation by reference of the measurement standards. The Agency is
proposing to add three new elements to the physical/chemical property
requirements: Physical state and appearance; vapor pressure; and
particle size for solid components. The Agency believes these basic
data requirements will provide added context when evaluating the
products for listing determinations. These, in combination with the
other general product information requirements, will assist the Agency
in evaluating the expected product behavior, and the process through
which it would affect the oil when used in the intended water and/or
shoreline environment. Additionally, the Agency is proposing to remove
the current incorporation by reference of specific standards to
determine physical/chemical properties, and replacing this with a
requirement for a citation of the standard methodology used to
determine these values. EPA believes that citing the standard
methodology used to determine the required values is sufficient in lieu
of specifying commonly recognized standard methodologies. The Agency
believes it is appropriate to make this change given the new
requirements for accredited laboratories to conduct testing.
(8) Chemical Abstract Service (CAS) Registry Numbers for each
component in a product. The CAS Registry is a collection of information
covering a wide variety of substances identified from the scientific
literature since 1957. CAS Numbers serve as an international resource
for substance identifiers and are used by scientists, industry, and
regulatory bodies because it can be validated quickly and reliably.
This will assist the Agency in better characterizing a product's
components and assessing its specific process for affecting the oil
prior to listing on the Schedule.
(9) Certification that bioremediation agents do not contain, at
levels that exceed the National Ambient Water Quality Criteria lowest
density value, bacterial, fungal, viral or opportunistic pathogens.
While providing information on these product contaminants is currently
required for bioremediation agents, there are no threshold levels for
product listing; a positive result for any of the above pathogens may
raise concern, but would not prevent the product from being listed on
the Schedule. The proposed requirement that these contaminants not
exceed the National Ambient Water Quality Criteria lowest density value
is intended to provide information for listing decisions that ensure
the use of bioremediation agents that will not result in exceeding
established water safety levels. The Agency believes that this
information is necessary to determine if a product is suitable for
listing, particularly for bioremediation agents, which could
potentially be used at recreational beaches. The Agency requests
comments on whether it should establish listing thresholds for products
based on this criteria, and whether the levels selected for
certification are appropriate for this application.
(10) Certification that the product does not contain levels that
exceed the National Water Quality Standards lowest acute value for
aquatic life of the following contaminants: Arsenic, cadmium, chromium,
copper, lead, mercury, nickel, zinc, or any other heavy metal
reasonably expected to be in the product; cyanide; chlorinated
hydrocarbons; pesticides; polychlorinated biphenyls (PCBs); and
polynuclear aromatic hydrocarbons (PAHs). Providing information (i.e.,
upper limit/concentration, detailed analytical methods, and sample
preparation) on most of these contaminants is currently required for
all products, with no established threshold levels for product listing.
The Agency will continue to require information on the methodology and
the data and supporting documentation used to determine the levels of
these contaminants in a product. The Agency, however, will not specify
what analytical testing method the submitter should use to make these
determinations, as it currently does for chlorinated hydrocarbons,
allowing the submitter flexibility in testing their product.
Additionally, the Agency is proposing to require data on several new
contaminants: Pesticides, PCBs, and PAHs. The Agency's concern with
pesticides as contaminants is mostly due to their potential use on
organic sorbents (e.g., peat moss, corn cobs, and cellulose fibers).
The concern for PCBs is for their toxicity and classification as

[[Page 3402]]

persistent organic pollutants, having toxic effects such as endocrine
disruption. PAHs are potent atmospheric pollutants, of concern because
some compounds have been identified as carcinogenic, mutagenic, and
teratogenic. The proposed threshold requirements for all of these
contaminants is intended to provide information for listing decisions
that ensure the use of any product will not result in exceeding
established water safety levels. The Agency requests comments on
whether it should establish a listing threshold for products based on
these criteria, and whether the levels selected for certification are
the appropriate levels for this application. The Agency also requests
comments on whether there are any other contaminants that should be
included for evaluation of a product prior to listing.
(11) Removal of the requirement for laboratories performing the
efficacy and toxicity testing for products to have prior experience
specific to the required methodology in lieu of recognized national or
international accreditations. Currently, laboratories performing
testing for products to be submitted for listing consideration are
required to document previous experience with the specific testing
methodologies in Appendix C to part 300. The Agency believes it is more
appropriate to require that laboratories be nationally or
internationally accredited. Accredited laboratories are expected to be
capable of following a prescribed testing protocol and good general
practices, providing assurance that the test results will be reliable.
Therefore, the Agency is proposing to remove the requirement for
laboratories to have previous experience specific to the methodologies
in Appendix C, and instead require that the laboratories hold
accreditations from recognized national or international organizations.
National and international accreditation organizations include, for
example, the International Organization for Standardization (ISO), and
the Laboratory Accreditation Bureau (recognized in the US through the
National Cooperation for Laboratory Accreditation (NACLA) and the
International Laboratory Accreditation Cooperation (ILAC)). The ISO
17025, Laboratory Competence standard, identifies high technical
competence and management system requirements to guarantee laboratory
test results and calibrations are consistently accurate. NACLA is a
national voluntary organization of regulators, accreditation bodies and
laboratories cooperatively working towards standardization of
laboratory accreditations throughout the industry; ILAC is the
international counterpart collaboration of laboratory and inspection
accreditation bodies. Established to ensure that laboratories are
subject to oversight by an authoritative body, accreditation
organizations have been evaluated by peers as competent and have signed
arrangements to enhance the acceptance of products and services.
Because interested parties can have confidence in the test results and
certifications provided by accredited laboratories, the Agency is
proposing to amend the laboratory requirement and believes that having
no prior experience with a specific methodology should not disqualify a
laboratory that has been accredited by an appropriate authoritative
body. However, the Agency reserves the right to not accept particular
lab data should EPA find cause to doubt the quality and integrity of
the work. EPA also reserves the right to conduct its own testing of any
product.
(12) Estimated annual product production volume, average and
maximum amounts that could be produced per day, and time frame needed
to reach maximum production rate (days). While there is currently no
requirement for production capability information, the Agency believes
it is important for the OSCs and responders to have this information.
The availability of a product may impact decisions of authorization of
use, depending on inventory or production capabilities. This would
prove to be of key importance, for example, in the event of a major
environmental disaster (e.g., a SONS event).
(13) Recognition received from EPA's Design for the Environment
(DfE). EPA's Design for the Environment (DfE) \33\ works in partnership
with industry, environmental groups, and academia to reduce risk to
people and the environment by finding ways to prevent pollution. DfE
evaluates human health and environmental concerns associated with
traditional and alternative chemicals and processes in a range of
industries in order to select safer chemicals and technologies. DfE
focuses its review of formulation ingredients on key environmental and
human health characteristics of concern within functional classes. This
allows formulators to use those ingredients with the lowest hazard in
their functional class, while still formulating high-performing
products. The DfE label means that EPA scientists have evaluated every
ingredient in the product to ensure it meets DfE's stringent criteria.
Products that meet the DfE criteria are safer chemical choices. In an
effort to encourage the development and use of safer technologies, the
Agency is proposing a requirement for the submitter to identify
products that have met and can be labeled DfE certified as part of the
general information, and would include this information in the NCP
Product Schedule Technical Notebook.\34\ This Technical Notebook
presents manufacturer's summary information on the conditions under
which each product is recommended to be used, and is a source of
information for the OSC in the event of a response.
---------------------------------------------------------------------------

\33\ http://www.epa.gov/dfe/.
\34\ http://www.epa.gov/oem/docs/oil/ncp/notebook.pdf.
---------------------------------------------------------------------------

(14) International product certifications, testing or use data
informing the performance capabilities or environmental benefits of the
product. The Agency believes that any additional data available from
other countries may help identify the benefits or concerns for the
listing and/or the authorization of use of a product. The Agency,
however, is not proposing any specific listing criterion or threshold
associated with this broad information request, as some products
(particularly new formulations) may not have any of this additional
data available.
(b) Dispersant Testing and Listing Requirements
The Agency is proposing revisions to the efficacy and toxicity
testing protocols, as well as establishing new thresholds for listing
dispersants on the Schedule in Sec. 300.915(b). The Agency proposes to
define dispersants as typically mixtures of solvents, surfactants, and
additives that promote the formation of small droplets of oil in the
water column by reducing the oil-water interfacial tension. These
droplets are driven into the water column by wave action. Emergency
response personnel need to know whether a dispersant or any other type
of chemical or biological agent on the Schedule could have negative
environmental impacts relative to the oil before decisions are made
about its use in a particular oil discharge situation. Consequently, it
is essential to consider comparative information about the efficacy and
the toxicity of these products. The proposed revisions are in response
to concerns not only for an increase in the frequency of planning for
the use of these agents, but also for their potential use in large
quantities, such as when responding to oil discharges from

[[Page 3403]]

oil tanker accidents and offshore well blowouts, as evidenced during
the Deepwater Horizon incident in 2010.
(1) Dispersant Efficacy
Current Requirements: The current NCP Subpart J requires
dispersants to be tested for saltwater efficacy in order to determine
listing eligibility on the Schedule. Dispersant efficacy is tested
following the Swirling Flask Test (SFT) listed in Appendix C to part
300 of the NCP. This protocol was developed by Environment Canada to
provide a relatively rapid and simple testing procedure for evaluating
dispersant efficacy (i.e., the percentage of oil that is dispersed).
The procedure places seawater, oil, and a dispersant into an Erlenmeyer
flask, which is then placed on a shaker table for a specified period of
time. The flask is modified by the addition of a side spout attached to
the bottom of the flask, which allows the analyst to pour off dispersed
oil from the bottom into a collection vessel for extraction and
measurement. After 20 minutes, a sample of water is poured off and
chemically analyzed for dispersed oil. For products to be listed, they
must attain an efficacy value of 45 percent or greater average
dispersion efficacy of two different crude oils (South Louisiana Crude
(SLC) and Prudhoe Bay Crude (PBC)) at room temperature (20-23 degrees
Celsius ([deg]C)).
Proposed Revisions: The Agency proposes to change the testing
protocol for measuring efficacy and adopt the Baffled Flask Test (BFT)
as the testing protocol for dispersant efficacy. The new BFT procedure
incorporates a redesign of the testing flask by eliminating the side
arm, incorporating baffles in the wall of the flask, and adding a
stopcock at the bottom, which improves reproducibility in the hands of
different operators. This protocol has undergone extensive peer review
\35\ and has been tested in several laboratories, providing
reproducible and repeatable results. The Agency also proposes revisions
to the efficacy listing criteria for dispersants to be listed.
Specifically, the dispersant must demonstrate that the lower 95%
confidence level (LCL95) of six replicate flasks meets the
new proposed efficacy listing criteria at two test temperatures. New
test oils representing a wider range of characteristics are also
proposed for this protocol: Alaska North Slope (ANS) and Intermediate
Fuel Oil (IFO-120) were tested for this proposal. Both oils are to be
tested at two temperatures: 5 [deg]C and 25 [deg]C. Finally, based on
the ANS and IFO-120 testing, the Agency proposes that dispersants
considered for listing must demonstrate that they attain all of the
following dispersant effectiveness (DE) values:

\35\ Venosa, Albert D., National Risk Management Research
Laboratory, US EPA; Sorial, George A., Department of Civil &
Environmental Engineering, University of Cincinnati; King, Dennis
W., Statking Consulting; Round-Robin Testing of a New EPA Dispersant
Effectiveness Protocol, International Oil Spill Conference, 2001.

ANS at 5 [deg]C: DELCL95 >=70%.
ANS at 25 [deg]C: DELCL95 >=75%.
IFO-120 at 5 [deg]C: DELCL95 >=55%.
IFO-120 at 25 [deg]C: DELCL95 >=65%.

The Agency tested eight of the dispersants currently listed on the
Schedule. Three of the eight dispersants clearly differentiated
themselves from the other five dispersants for having the best
DELCL95 efficacy results; they would meet all the proposed
thresholds. For the next best dispersant tested, the results were
substantially lower than those in the top group and would not meet all
the thresholds proposed today. This natural break in the results
provided the Agency with the basis for the proposed threshold criteria.
The Agency is also proposing to replace the SLC and PBC test oils
currently used for efficacy testing with two other oils that represent
a wider range of characteristics. The proposal is based on the results
of tests using ANS and IFO-120 oils with the new protocol. In proposing
two new oils for efficacy testing, the Agency is seeking to ensure that
the efficacy testing uses oils that represent a wider range of oil
gravities throughout the different geographic locations in the country
where dispersants might be used. The oils selected should exhibit
sufficiently different characteristics to produce results that have
statistically significant variation between them. The proposal is to
replace the SLC and PBC oils, both of which were light oils, with a
range of light-to-medium, and heavier oils. The light-to-medium gravity
ANS pipeline blend and the heavier refined product, IFO-120 were
selected for testing the protocol in this proposal. The current
protocol, testing 4 replicates of both the SLC and the PBC oils and
combining their results, provided one threshold criterion after
determining that each of the oils produced statistically similar
results. In contrast, the efficacy test results between the ANS and the
IFO-120 showed statistically significant differences at each
temperature. The Agency believes the use of ANS and IFO-120, or similar
oils that represent a wider range of oil gravities, will provide better
information on the efficacy of the products when used on different
types of oils.
Additionally, the Agency is proposing that efficacy testing be
conducted at two different temperatures, 5 [deg]C and 25 [deg]C, rather
than at an ambient temperature range of 20-23 [deg]C as currently
required. The Agency recognizes the current and future interest in
arctic and deepwater drilling, and the continued oil production in the
southern, more tropical areas of the country. Given the potential range
of locations where dispersants may be used, the Agency believes it is
appropriate to have products tested at temperatures that would reflect
that range. These temperatures are intended to capture dispersant use
scenarios in a wide range of geographic locations and under different
temperatures that may occur in the same geographical location (such as,
for example, the deep sea and surface water in the Gulf of Mexico,
where the temperatures are typically 5 and 25 [deg]C, respectively).
The Agency is also proposing to replace the current SFT with the
BFT, which is designed to be more representative of moderately
turbulent sea conditions where dispersants are more likely to be
successful when used. The revised testing protocol improves test
repeatability and reproducibility within and between laboratories, as
well as greatly reduces both the inherent error of the method and the
human error associated with the current SFT, as discussed below. In
addition, reporting the test results in terms of the product's
LCL95 accounts for between- and within-laboratory error
variability and the inherent error of the method. Only one number is
reported compared to a mean and standard deviation, as the variation
has already been subtracted in the reported number. Specifically:
The new baffled trypsinizing flask design, fitted with a
glass stopcock positioned at the bottom side, promotes less
manipulation that could result in erroneous re-suspension of non-
dispersed oil, as in the SFT. The re-suspension of oil when using the
SFT test protocol was a major source of error. In the SFT, the flask
has a side arm spout, requiring the analyst to pick up the flask and
pour the contents out manually. Through that action, re-suspension of
the dispersed oil can easily take place, leading to potentially
erroneous results. In contrast, in the BFT, the flask contains a
stopcock at the bottom, so the analyst need only open the stopcock to
drain the contents from the flask without the potential of remixing or
re-suspending the dispersed oil.
The BFT provides more turbulent mixing and better enables
more reproducible and repeatable dispersant

[[Page 3404]]

action than the SFT. The mixing energy within the flask is higher and,
as a result of this increased mixing energy, better dispersion is
possible. Turbulence is needed for the proper mixing of dispersant and
oil and for producing the sheer forces needed to create the small
droplet sizes with high surface area-to-volume ratio that promote the
effective dispersion of the oil into the water column. The BFT provides
such mixing and better enables more repeatable and reproducible
dispersant effectiveness than the SFT. The BFT was tested extensively
in a nine-participant round-robin inter-laboratory calibration test on
six commercial dispersant products.\36\ In addition, based on the
mixing energy that can be achieved using the new baffled flask, the
Agency believes a higher efficacy threshold is warranted. As a result
of this increased mixing energy, better dispersion is realized under
conditions more realistic of wave action in the sea.
---------------------------------------------------------------------------

\36\ Venosa, A. D., D. W. King, and G. A. Sorial. 2002. The
Baffled Flask Test for Dispersant Effectiveness: A Round Robin
Evaluation of Reproducibility and Repeatability. Spill Sci. &
Technol. Bulletin 7(5-6):299-308.
---------------------------------------------------------------------------

The variability both between analysts and within analysts
is substantially lower for the BFT compared to the SFT, as measured by
the coefficient of variation (CV). The CV is defined as the standard
deviation divided by the mean and is expressed in terms of percent; the
higher the CV, the greater the variability.^{37 38}
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\37\ Sorial, G. A., A. D. Venosa, K. M. Miller, E. Holder, and
D. W. King. 2004a. Oil Spill Dispersant Effectiveness Protocol--Part
I Impact of Operational Variables. ASCE. J. Env. Eng. Div.,
130(10):1073-1084.
\38\ Sorial, G. A., A. D. Venosa, K. M. Miller, E. Holder, and
D. W. King. 2004b. Oil Spill Dispersant Effectiveness Protocol--Part
II Performance of the Revised Protocol. ASCE ASCE. J. Env. Eng.
Div., 130(10):1085-1093.
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The Agency considered establishing listing thresholds for efficacy
based on the types of oil. The Schedule could list sub-categories of
dispersants based on gravities of the oil (i.e., light-medium or
heavy), so that a dispersant would only be authorized for use on oils
that fall within the range for which it tested effective. Similarly,
the Schedule could list dispersants based on temperature, allowing a
dispersant to be authorized for use only at the temperature for which
it tested effective. However, determining ranges or definitions for
when oil changes from light to medium or heavy, is challenging because
they may be affected by a number of external factors, including
temperature. Likewise, listing dispersants based on temperature would
require an additional degree of complexity to the authorization for
use, as the temperatures may change drastically in some geographical
regions affected by the same oil discharge. Even within more stable
geographical regions, there may be variations at the time of an oil
discharge that could affect the decision to use a dispersant stockpiled
for a different temperature range. While these more specific listing
approaches would provide more information on effective product choices,
the Agency is concerned about how such specific listing approaches may
contribute to OSC confusion in an emergency, the cost of stockpiling
multiple types of dispersants, or the immediate availability of the
appropriate dispersant in an emergency. Furthermore, the Agency is
proposing revisions to Subpart J to authorize RRTs to request
supplementary testing and information to provide greater flexibility in
tailoring testing conditions to address area- and site-specific
concerns. Given these factors, the Agency believes that it is
appropriate that only those dispersants that achieve efficacy for both
types of oils and at both temperatures be listed. Listing only the
products that achieve efficacy for both types of oils at both
temperatures would demonstrate a wide range of efficacy for the
product, and a single listing would facilitate authorizing their use
during a response action. The Agency requests comments on this
approach.
(2) Dispersant Toxicity
Current Requirements: The current NCP Subpart J requires
dispersants to be tested for toxicity to saltwater species. This
information is available to the OSC for their consideration in
authorizing dispersant use. Dispersant toxicity is tested following the
protocols in Appendix C to part 300 of the NCP. The standard toxicity
test for dispersants involves exposing two saltwater species, the
inland silverside fish (Menidia beryllina or M. beryllina) and the
mysid shrimp (Americamysis bahia or A. bahia), to five concentrations
of the test product and No. 2 fuel oil, alone and in a 1:10 mixture of
product to oil. Reference toxicity tests are conducted using dodecyl
sodium sulfate (DSS) as a reference toxicant. The test length is 96
hours for M. beryllina and 48 hours for A. bahia. The concentration of
test product causing 50% lethality to the test organisms
(LC50) is calculated at the end of the exposure period.
Proposed Revisions: The Agency proposes to revise the toxicity
testing requirements for dispersants, including the testing protocol
and the use of the test results. The proposal would require acute
toxicity testing for the dispersant alone, and the dispersant mixed
with both oils used for efficacy testing; the proposal is based on the
ANS and IFO-120 oils. While the Agency currently provides the toxicity
testing results to the OSC to assist in authorization of use
determinations, it is proposing to use these testing results to
determine eligibility for listing on the Schedule.
Specifically, the Agency is proposing to require evaluations of
dispersant toxicity using acute toxicity tests following existing USEPA
effluent testing guidelines,^{39 40} modified for use with
dispersant product or dispersant product/oil mixtures, as detailed in
Appendix C to part 300. Measured toxicity values for dispersant product
and dispersant product/oil mixtures are proposed to include static
acute toxicity tests using A. bahia and M. beryllina. Developmental
toxicity using a sea urchin assay, and sub-chronic effects using A.
bahia and M. beryllina are also proposed to be conducted, but with
dispersant product only. The Agency is proposing the following toxicity
thresholds for listing dispersants on the Schedule:
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\39\ USEPA 2002a Methods for Measuring the Acute Toxicity of
Effluents and Receiving Waters to Freshwater and Marine Organisms,
Fifth edition. (Acute Methods Manual), Office of Water, Cincinnati,
OH. EPA-821-R-02-012.
\40\ USEPA 2002b. Short-term Methods for Estimating the Chronic
toxicity of Effluents and Receiving Waters to Marine and Estuarine
Organisms, Third Edition. (Saltwater Chronic Methods manual). Office
of Water, Cincinnati, OH. EPA-821-R-02-014.
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Lethal concentration for 50% of the test species
(LC50) at the lower 95% confidence interval for all acute
toxicity tests greater than 10 ppm;
Inhibition concentration for 50% of the test species
(IC50) at the lower 95% confidence interval greater than 10
ppm;
No Observed Effect Concentration (NOEC) equal to or
greater than 1 ppm for sub-chronic toxicity.
Test Oils and Oil Acute Toxicity Values. The Agency proposes to
replace the No. 2 fuel oil currently used for toxicity testing with two
test oils that better represent a wider range of characteristics and
that may be encountered during an incident. The proposal is based on
ANS and IFO-120, as previously discussed. In addition to making the
test oils consistent with the dispersant efficacy tests, testing oils
of different gravities also provides a better estimation of dispersant/
oil toxicity associated with differing oil constituencies, and
ultimately a better representation of the potential overall toxicity of
a product.
The Agency proposes to conduct the oil-only acute toxicity tests
for the two reference oils, with both A. bahia and

[[Page 3405]]

M. beryllina, and provide this data for comparisons to dispersant and
dispersant-oil mixture acute toxicity tests. EPA will make all of the
reference oil toxicity test results available to the public on its Web
site, including raw data and calculated median LC50 values.
By providing this information, the Agency is reducing the number of
required toxicity tests the submitter would need to conduct.
Alternatively, the Agency considered requiring submitters to conduct
the oil acute toxicity testing as it would provide an opportunity to
detect anomalies in the submitted data. The Agency is requesting
comments on whether the submitter should be required to conduct the
oil-only acute toxicity testing for the two test oils.
Dispersant and Dispersant-Oil Acute Toxicity Threshold. Using the
EPA toxicity classification scheme,\41\ LC50 values ranging
from 10 ppm to 100 ppm are classified as slightly toxic and above 100
ppm substances are considered acutely nontoxic to aquatic organisms.
For both M. beryllina and A. bahia, the Agency is proposing as the
threshold value the lower bound of the LC50 95% confidence
interval (CI) greater than or equal to 10 ppm for all toxicity tests to
qualify a dispersant to be listed on the Schedule. The rationale for
using the lower bound of the CI is that the CI should not contain any
values less than or equal to 10 ppm since theoretically, the
LC50 can fall anywhere within the CI. By using the lower CI,
the Agency is providing a conservative decision criterion for acute
toxicity, and by proposing a greater than or equal to 10 ppm threshold
level, it is establishing an adequate safety margin without being
overly restrictive.
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\41\ http://www.epa.gov/oppefed1/ecorisk_ders/toera_analysis_eco.htm#Ecotox.
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Dispersant-Oil Mixture Acute Toxicity Protocol. The Agency is
proposing to substitute the existing preparation procedure for the
dispersant-oil mixture (DOM) in Appendix C to Part 300, Section 3
method for the preparation procedure for dispersant-oil mixture using a
modified protocol \42\ first described by Baron and Ka'aihue \43\ and
fully described by Hemmer et al.\44\ These new modified procedures for
preparation of the chemically enhanced water accommodated fractions
(CEWAFs) of dispersant-oil mixtures are used to make exposure
solutions. Evaluations of the dispersant-oil mixture toxicity using
acute toxicity tests follow existing EPA effluent testing
guidelines,^{45 46} modified for use with these exposure
solutions and are detailed in Appendix C to part 300. EPA proposes to
modify the variable loading preparation procedure described in Chemical
Response to Oil Spills: Ecological Research Forum (CROSERF) \47\ to a
variable dilution procedure to standardize the oil-to-water ratio and
provide a consistent chemical concentration in a test series.
Additionally, the modified preparation procedure provides economies in
analytical costs by reducing the need to analyze the composition of
every tested concentration. Chemical analysis for the total petroleum
hydrocarbon (TPH) concentration of the CEWAF stock solution is
required.
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\42\ The modified protocol is based on a variable dilution
modification of the Chemical Response to Oil Spills: Ecological
Research Forum (CROSERF) testing protocol; Aurand, D. and G. Coelho
(Editors). 2005. Cooperative Aquatic Toxicity Testing of Dispersed
Oil and the ``Chemical Response to Oil Spills: Ecological Effects
Research Forum (CROSERF).'' Ecosystem Management & Associates, Inc.
Lusby, MD. Technical Report 07-03.
\43\ Barron, MG, Ka'aihue L. 2003. Critical evaluation of
CROSERF test methods for oil dispersant toxicity testing under
subarctic conditions. Mar Pollut Bull 46:1191-1199.
\44\ Hemmer, MJ, Barron, MG, Greene, R. 2011. Comparative
toxicity of eight oil dispersants, Louisiana sweet crude oil (LSC)
and chemically dispersed LSC to two aquatic species. Environ Toxicol
Chem, 30: 2244-2252.
\45\ USEPA 2002a Methods for Measuring the Acute Toxicity of
Effluents and Receiving Waters to Freshwater and Marine Organisms,
Fifth edition. (Acute Methods Manual), Office of Water, Cincinnati,
OH. EPA-821-R-02-012.
\46\ USEPA 2002b. Short-term Methods for Estimating the Chronic
toxicity of Effluents and Receiving Waters to Marine and Estuarine
Organisms, Third Edition. (Saltwater Chronic Methods manual). Office
of Water, Cincinnati, OH. EPA-821-R-02-014.
\47\ CROSERF was established as a working group of industry,
government, and university scientists to coordinate and disseminate
research on chemical oil spill dispersants. CROSERF participants
developed aquatic toxicity testing protocols during 1994 to 2000
with the foremost objective of standardizing test methods and
reducing inter-laboratory variability.
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Sea Urchin Developmental Assay. The Agency is proposing to require
a sea urchin developmental assay (also referred to as an embryogenesis
assay) to assess the potential for a dispersant product to cause
adverse effects on the developmental process. During the Deep Water
Horizon spill event, the possible adverse effects of oil dispersants on
the developmental processes of fish and invertebrate species were
identified as critical issues of concern. By incorporating the sea
urchin developmental assay, the Agency is using it as a sensitive
surrogate test for pelagic early life stages. This assay would employ
an existing EPA test protocol \48\ routinely used in effluent testing.
As suggested for the dispersant acute toxicity test criteria with A.
bahia and M. beryllina, the Agency is proposing as the threshold value
the lower bound of the developmental IC50 95% confidence
interval greater than or equal to 10 ppm. For this test, the
IC50 is defined as the concentration of dispersant that
inhibits the development of 50% of exposed embryos. As described above
for acute toxicity levels, the Agency is adopting a similar rationale
for IC such that IC50 values ranging from 10 ppm to 100 ppm
are considered to cause slight adverse effects on the developmental
process, and above 100 ppm substances are considered to cause no
adverse effects. By using the lower CI the Agency is providing a
conservative decision criterion for developmental toxicity, and by
proposing a greater than or equal to 10 ppm threshold level it is
establishing an adequate safety margin without being overly
restrictive.
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\48\ USEPA 1996. Short-term Methods for Estimating the Chronic
Toxicity of Effluents and Receiving Waters to West Coast Marine and
Estuarine Organisms. EPA/600/R-95/136.
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Sublethal/Subchronic Studies. The Agency has limited information
concerning the possible sublethal effects of dispersants currently
listed on the Product Schedule. The Agency is proposing requirements
for subchronic assays (duration approximately 7 days) to be performed
with A. bahia and M. beryllina following established EPA short-term
methods for estimating chronic toxicity of effluents.\49\ While the
Agency considered requiring longer-term tests, it believes the 7-day
subchronic tests are reasonable alternatives for estimating chronic
toxicity. This information would also be of value as guidance to
regional responders and OSC's on possible adverse effects on survival
and growth of larval fish and invertebrates caused by longer-term
exposure to dispersants. The Agency is proposing a NOEC equal to or
greater than 1 ppm listing threshold level for sub-chronic effects.
This threshold level provides a tenfold safety factor from the proposed
acute toxicity threshold values. The tenfold safety factor is a common
practice in ecological risk assessment and thus the Agency believes it
provides an adequate safety margin without being overly restrictive.
The Agency is requesting comment on whether it should consider longer-
term tests (e.g., early life stage tests), which may be more relevant
to sublethal effects caused by longer

[[Page 3406]]

duration exposure to low concentrations of a dispersant product.
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\49\ USEPA 2002b. Short-term Methods for Estimating the Chronic
Toxicity of Effluents and Receiving Waters to Marine and Estuarine
Organisms, Third Edition. (Saltwater Chronic Methods manual). Office
of Water, Cincinnati, OH. EPA-821-R-02-014.
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Alternative Options
In addition to the criteria discussed above, the Agency considered
calculating a toxicity threshold based on the ratio of the
LC50 of oil-alone to the LC50 of the dispersant-
oil mixture for M. beryllina and A. bahia to assist in comparing the
relative toxicity of crude oil to chemically dispersed oil. A ratio of
less than or equal to 1 would indicate the toxicity of the dispersant-
oil mixture is less than or equal to the toxicity of the oil-alone. The
Agency considered whether this ratio should be used as a criterion for
inclusion of dispersants on the Schedule or as guidance to emergency
responders. Using a less than or equal to 1 ratio as a guideline would
afford an adequate safety margin without being overly restrictive.
While the ratio would provide a simple, interpretable, and easily
justifiable value for determining acceptable toxicity levels of
dispersant-oil mixtures, it would not be specific to oils in particular
discharge situations. The Agency is requesting comment as to whether
such a value should be calculated, and if so, whether it should be an
additional listing criterion, or provided as information for the
responders to consider in authorizing dispersant use.
The Agency also considered including geographically or ecologically
representative species in the testing protocol. The Agency believes,
however, that this issue is addressed by the proposed revisions to the
supplemental testing and information requirements in section
300.910(g), with the decisions of testing geographically and
ecologically representative species left to the discretion of the RRTs.
While inclusion of species from different phyla and habitats would
provide useful and important information on possible adverse effects of
dispersant products and dispersed oil, the proposed testing protocols
would need to be modified and validated. Further, the Agency is
concerned about balancing the time and cost associated with the
development of these tests on the part of the submitter rather than on
the end users.
The Schedule currently requires no specific toxicity or efficacy
tests for subsea dispersant listing or authorization of use. While the
differences in toxicity values and efficacy may be affected by
application in subsea environments, the Agency believes that the
proposed requirements establish an adequate baseline for listing
dispersants on the Schedule and for authorizing their use by responders
in case of an incident. The Agency is addressing these concerns by
proposing new provisions for dispersant monitoring for all subsea use,
and requests comments on alternative testing and listing approaches to
specifically address subsea concerns.
(3) Limitations of Use
The Agency is proposing a conditional use listing for dispersants.
The proposal specifies that dispersants may only be used in saltwater
environments. Dispersants are typically designed and traditionally used
for responding to oil discharges in saltwater. In general, the
effectiveness of dispersants decreases as the salinity of the water
decreases, given the same hydrophilic-lipophilic balance, and the
effectiveness is minimal in freshwater environments. Surfactants, the
main active ingredient in dispersants, sustain oil droplets in water by
orienting the lipophilic side of its molecule in the oil and the
hydrophilic side in the water. The hydrophilic side of the surfactant
is generally more soluble in waters with higher salinity values,
causing the oil droplets to be more stable in saline water
environments. In waters with no salinity, many dispersants have shown a
very low effectiveness or are sometimes completely ineffective.\50\
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\50\ Fingas, M., (Ed.), 2011, Oil Spill Science and Technology,
Gulf Professional Publishing, pp. 513-518.
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The Agency is also concerned with using dispersants in freshwater
environments because of the limited dilution typically available as
compared with the open sea and because of the existence of water
intakes in rivers, streams, and lakes for use in drinking water
supplies. Using dispersants in freshwater has the potential for
compounding the impacts caused by already discharged petroleum
products, particularly near potable and non-potable subsurface water
intakes. The Agency does recognize, however, that as a last resort,
dispersants may have some limited applicability in freshwater. The
provision for authorization of use under Sec. 300.910(d) would allow
for exceptions to the prohibition on the use of dispersants in
freshwater in cases where there is an immediate threat to human life.
The Agency is requesting comment on this proposed listing limitation.
(c) Surface Washing Agent Testing and Listing Requirements
The Agency is proposing to define Surface washing agents (SWA) as
substances that separate oil from solid surfaces, such as beaches,
rocks, or concrete, through a detergency mechanism that lifts and
floats oil for collection and recovery from the environment with
minimal dissolution, dispersion, or transfer of oil into the water
column. For this agent category, the Agency is proposing to revise the
toxicity testing protocols, to establish efficacy testing protocols,
and to establish both toxicity and efficacy listing thresholds in Sec.
300.915(c). The proposed revisions respond to concerns regarding their
frequent use and the potential for residual impacts after their use.
(1) Surface Washing Agent Efficacy
Current Requirements: There are currently no efficacy testing
requirements in the NCP Subpart J for surface washing agents to
determine listing eligibility on the Schedule.
Proposed Revisions: The Agency is developing a laboratory testing
protocol to evaluate the efficacy of SWAs in removing crude oil from a
solid substrate.\51\ Currently available efficacy testing protocols for
these agents are concerned with assessing the detergency, or cleaning
power, of the agents by quantifying the physical removal of oil from
non-vegetative substrates as a result of their use. The protocols
typically involve the application of oil to a solid substrate (or the
use of pre-oiled substrate), weathering of the oil on the substrate,
application of the agent to the oiled substrate, a contact period for
SWA penetration, and washing of the substrate with water. The fractions
of oil removed in the wash water and/or remaining on the substrate are
quantified. Oil removal efficiencies for surface washing treatments are
typically compared to the washing efficiency of water without surface
washing agents (untreated controls). Disadvantages or potential sources
of error have been identified in the existing protocols that may not
reflect field performance. Of concern are, for example, the use of
substrates (e.g., stainless steel, porcelain) with different wetting
and adhesion properties than natural substrates such as sand or gravel;
short weathering times insufficient for oil attachment; and the absence
of mixing energy during the washing step, which may lead to incomplete
detachment of partially released oil.
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\51\ Koran, K.M., Venosa, A.D., Luedeker, C.C., Dunnigan, K.,
Sorial, G.A., 2009. Development and Testing of a New Protocol for
Evaluating the Effectiveness of Oil Spill Surface Washing Agents.
Mar. Pollut. Bull., 58: 1903-1908.
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The Agency's goal is to develop and evaluate a new bench-scale
testing protocol that would provide a standard for EPA to use in SWA
product

[[Page 3407]]

evaluation prior to listing on the Schedule. Changes over established
protocols the Agency considered include: Using natural substrates to
reflect the most commonly impacted shoreline material; establishing
sufficient weathering time to permit strong attachment of the oil to
the substrate surface; fully quantifiable approaches with known volumes
and precise measurements to allow mass balance; and a standardized and
reproducible methodology to minimize operator error. PBC oil was used
as the representative standard reference oil in developing the protocol
since it had previously been selected as one of two standard oils for
the Agency's published protocols for dispersant and bioremediation
agent testing. However, the Agency is proposing revisions to the
dispersant and bioremediation testing protocols, including replacing
the PBC reference oil. The protocol being developed has not been
tested: With the IFO-120 or the ANS oils that are proposed to be used
in the revised dispersant efficacy testing protocol; at multiple
temperatures; or to include freshwater systems. The Agency expects to
develop final recommendations for the testing protocol following round
robin testing after adjusting for the new variables. The Agency would
propose this protocol in the Federal Register through notice and
comment before adopting it as part of Subpart J requirements.
Consequently, because of the additional work needed to finalize its
protocol, the Agency is proposing to allow the use of standard
recognized efficacy testing methodologies for surface washing agents.
An example of such a standard recognized methodology is the American
Society for Testing and Materials (ASTM) Standard Test Method for
Evaluating the Effectiveness of Cleaning Agents.\52\ Another
methodology is Environment Canada's Test Method.\53\ The capability of
a particular surface washing agent depends upon the application
procedures and the characteristics of the surface being cleaned, such
as size, shape, and material. The ASTM test method in particular covers
a procedure for evaluating the capability of the agents, providing a
relatively rough surface to which the oil can adhere. The Environment
Canada method uses a stainless-steel `trough' which is placed at a
specified angle. The target oil is placed on an area on the trough. The
treating agent is then applied in droplets to the surface of the oil
and after 10 minutes at 5-minute intervals, rinses of water are applied
to the trough. After drying, the trough is weighed and the removal
calculated from the weight loss. Repeatability is within 5%. The Agency
is requesting comment on available methodologies and its published
protocol to incorporate as the testing protocol for these agents. The
Agency also requests comment on whether the rule should identify the
specific methodologies to be used until EPA develops and adopts a new
testing protocol for SWA efficacy testing.
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\52\ ASTM Standard Test Method for Evaluating the Effectiveness
of Cleaning Agents. Designation: G122--96 (Reapproved 2008). ASTM
International, 100 Barr Harbour Dr., P.O. Box C-700 West
Conshohocken, Pennsylvania 19428-2959, United States
\53\ Fingas, Merv and Fieldhouse, Ben; ``Surface-washing Agents
or Beach Cleaners'' (2010). Chapter 21 Surface-Washing Agents or
Beach Cleaners. In Oil Spill Science and Technology (p716). London:
Gulf Professional Publishing.
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The Agency is also proposing an efficacy threshold of 30% in either
fresh or salt water or both depending on the intended product use. This
is based on the efficacy data published in ``Surface-washing Agents or
Beach Cleaners.'' \48\ Numerous surface washing agent products,
including several from the Schedule were tested using the Environment
Canada methodology. The average efficacy of the surface washing agents
tested is approximately 30%. The Agency requests comments on this
approach and other efficacy test data available.
(2) Surface Washing Agent Toxicity
Current Requirements: The current NCP Subpart J requires surface
washing agents to be tested for saltwater species toxicity. Surface
washing agent toxicity is tested following the dispersant toxicity
testing protocols in Appendix C to part 300 of the NCP.
Proposed Revisions: The Agency is proposing revisions to the
toxicity testing requirements for surface washing agents, including the
testing protocol. While the Agency currently provides the toxicity
testing results to the OSC to assist in authorization of use
determinations, it is proposing to use these toxicity testing results
to determine listing eligibility on the Schedule.
The proposed revisions to the testing protocols for surface washing
agents are detailed in Appendix C to part 300. The proposed acute
toxicity test protocol for surface washing agents is based on EPA's
protocol, Methods for Measuring the Acute Toxicity of Effluents and
Receiving Waters for Freshwater and Marine Organisms.\54\ The Agency
proposes to require surface washing agents be tested for acute toxicity
using fresh water species Ceriodaphnia dubia and Pimephales promelas,
or saltwater species Americamysis bahia and Menidia beryllina, or both,
depending on the intended product use. The concentration of test
product causing 50% lethality to the test organisms (LC50)
and lower and upper 95% confidence intervals (LCI95 and
ULCI95) are calculated at the end of the exposure period. To
be listed on the Schedule, surface washing agents must demonstrate an
acute lethal concentration for 50% of the test species
(LC50) at the lower 95% confidence interval greater than 10
ppm in either fresh or salt water, consistent with the acute toxicity
thresholds proposed for dispersants. EPA's toxicity classification
scheme \55\ classifies LC50 values ranging from 10 ppm to
100 ppm as slightly toxic and values above 100 ppm substances are
considered practically nontoxic to aquatic organisms. By proposing this
threshold level, the Agency is establishing an adequate safety margin
without being overly restrictive. The Agency requests comments on the
proposed acute toxicity methods (or any others available) and
thresholds for surface washing agents.
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\54\ http://water.epa.gov/scitech/methods/cwa/wet/upload/2007_07_10_methods_wet_disk2_atx1-6.pdf.
\55\ USEPA 2010. http://www.epa.gov/oppefed1/ecorisk_ders/toera_analysiseco.htm#Ecotox.
---------------------------------------------------------------------------

The Agency is proposing provisions for conducting acute toxicity
tests with dispersant-oil mixtures, but not for any other agent,
including SWAs. EPA believes that non-dispersant products are not
likely to be used in the same quantities or durations as dispersants
and some may be recovered making a requirement to conduct toxicity
tests of product/oil mixtures unnecessary. There may be concerns,
however, for increased product toxicity because of their interaction
with the oil. Thus, the Agency is requesting comment on the need for
acute toxicity tests conducted with surface washing agents-reference
oil mixtures. A protocol for preparation of product/oil mixtures for
toxicity testing is available for review in the docket.
(3) Limitations
The Agency is proposing a conditional use listing for SWAs. The
proposal specifies that these products may only be used in those water
environments for which the product was tested and for which it met the
listing threshold criteria. The Agency recognizes that products may
yield effective results in certain environments and not in others.
Products that may be

[[Page 3408]]

effective in freshwater environments may not necessarily be so in
saltwater environments, and vice versa. The Agency is proposing this
limitation to allow product manufacturers the flexibility to select
which environment the product is to be tested and authorized for use,
either saltwater, fresh water, or both environments. Therefore, the
product would be listed and could only be authorized for use in those
water environments for which it was tested and for which it met both
the efficacy and toxicity listing criteria.
(d) Bioremediation Testing and Listing Requirements
The Agency is proposing to define bioremediation agents as
biological agents and/or nutrient additives deliberately introduced
into a contaminated environment to increase the rate of biodegradation
and mitigate any deleterious effects caused by the contaminant
constituents. Bioremediation agents include microorganisms, enzymes,
and nutrient additives such as fertilizers containing bioavailable
forms of nitrogen, phosphorus and potassium. For this agent category,
the Agency is proposing to revise the efficacy testing protocols, to
establish toxicity testing protocols, and to establish both efficacy
and toxicity listing thresholds in Sec. 300.915(d).
(1) Bioremediation Agent Efficacy
Current Requirements: Bioremediation agent efficacy is currently
tested following the protocols in Appendix C to part 300 of the NCP.
The current bioremediation agent efficacy testing protocol is designed
to determine a product's ability to biodegrade oil by quantifying
changes in the oil composition resulting from biodegradation using
natural seawater as the test water. The protocol tests the
bioremediation agent for microbial activity and quantifies the
disappearance of saturated hydrocarbons and PAHs in weathered oil; for
purposes of the proposal the Agency tested the protocol using ANS
521.\56\ The sample preparation procedure extracts the oil phase into
dichloromethane (DCM), with a subsequent solvent exchange into hexane.
The analytical technique uses a high-resolution gas chromatograph/mass
spectrometer (GC/MS); GC/MS provides for a high degree of chemical
separation and spectral resolution. Concurrently with the chemical
analysis, a microbiological analysis is also performed to determine and
monitor the viability and growth of the microbial cultures being
studied. For commercial products that are strictly microbial agents not
containing their own nutrients, a mineral nutrient solution is provided
if requested by the submitter; no further nutrients are added to
commercial products containing their own nutrients. To be listed on the
Schedule, bioremediation agents must demonstrate a statistically
significant difference between the average degradation of both total
alkanes and total aromatics in the oil achieved by the product after 28
days and the average degradation for the same compounds achieved by the
non-nutrient control in the same time period.
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\56\ Artificially distilled Alaska North Slope crude oil at
521[emsp14][deg]F (272[deg]C) to remove the low molecular weight
hydrocarbons to approximate natural weathering processes that occur
after a spill.
---------------------------------------------------------------------------

Proposed Revisions: The proposal reflects a series of changes to
the current efficacy testing protocol for bioremediation agents. The
protocol includes freshwater testing in addition to the current
saltwater-based test, and uses artificial water for both fresh and
saltwater testing, replacing the natural seawater currently used. The
proposed protocol also eliminates several gravimetric and
microbiological analyses and testing endpoints not used in the proposed
listing determinations. Additionally, the proposed protocol limits the
levels at which external nutrients may be added, which allows the
addition for product formulations without nutrients, or for product
formulations that have nutrient concentrations at insufficient levels
for the experimental setup. Finally, the methodology streamlines the
statistical analysis. The proposed revisions address concerns with the
existing methodology as discussed below, expanding its application to
include freshwater environments, improving the consistency and
comparability of the test results, and generally streamlining the
protocol.
Protocol. The proposed efficacy testing protocol is designed to
determine a bioremediation agent's ability to biodegrade weathered
crude oil in the exposure water (saltwater or freshwater) by
quantifying changes in the oil composition resulting from
biodegradation. It consists of a series of six product and control
flasks containing artificial seawater or artificial freshwater and
weathered crude oil in which biodegradation of the crude oil
hydrocarbons is monitored for 28 days. Product flasks at day 28 are
compared to product flasks at day 0 to determine if a specified
reduction both in total resolved alkanes and total resolved aromatics
was achieved in that time period. Product flasks contain exposure
water, weathered oil, and product in concentrations specified by the
manufacturer. Positive control flasks must contain exposure water, oil,
nutrients, and the standard culture supplied by the Agency. A negative
control, consisting of artificial exposure water, product, weathered
crude oil, nutrients, and a sterilant is also used to ensure that the
observed degradation of hydrocarbons was not caused by abiotic losses
or interaction with the product. The Agency is requesting comment on
whether an additional protocol specific to products containing enzymes
only would be appropriate; this would consist only of exposure water,
weathered oil and the enzymatic product in the concentrations specified
by the manufacturer. The proposed protocol quantifies the degradation
(or disappearance) of alkane hydrocarbons and aromatic hydrocarbons.
The sample preparation procedure extracts the oil phase into the
solvent dichloromethane (DCM; also known as methylene chloride) with a
subsequent solvent exchange into hexane. The test method targets the
relatively easy to degrade normal alkanes and the more resistant and
toxic aromatics. The analytical technique uses a high resolution GC/MS
because of its high degree of chemical separation and spectral
resolution. GC/MS has long been used to study the weathering and fate
of oil spilled into the environment. It gives unambiguous results for
determining biodegradation efficacy. For quantitative analyses, the
instrument is operated in the selected ion monitoring mode (SIM) of
detection at a scan rate of > 5 scans per second to maximize the linear
quantitative range and precision of the instrument.
Fresh and Saltwater Environments. The existing bioremediation test
is exclusively for saline environments with no equivalent test for
freshwater environments. Further, the existing test uses natural
seawater and has been found to give variable results due to the
compositional variability of seawater both chemically and
microbiologically. The Agency proposes to replace the natural seawater
with a standardized artificial saltwater formula called GP2, whose
components and concentrations are generally recognized, and which is
easily made. The use of artificial saltwater allows for better test
reproducibility. Additionally, the Agency proposes to expand the
requirement for efficacy testing to include freshwater, which allows
for a better evaluation of the use of these agents in this environment.
Similarly to

[[Page 3409]]

the artificial saltwater, artificial minimal salts freshwater would be
used with known ingredients (Bushnell and Haas; Journal of
Bacteriology, Vol. 41: 653, 1941). Because the Agency is adding a
freshwater test, it is also allowing the submitter to test a product
for freshwater only, saltwater only, or both. The Schedule listing
would specify in which environment the product was tested and
authorized for use. Products could be listed for use on saltwater only,
on freshwater only, or for use on both environments, giving the option
to the submitter to market its products accordingly.
GC/MS Testing Endpoints. GC/MS has long been used to study the
weathering and fate of oil spilled into the environment. However, GC/MS
being the primary tool used in the analysis makes this test expensive.
The current protocol includes several measured variables in both the
product flasks and the non-nutrient control flasks, including the
gravimetric residual oil weight analysis, a Most Probable Number
microbiological analysis, and the GC/MS analysis at 3 different time
points, days 0, 7, and 28. The Agency is proposing to eliminate all of
these analyses except the day 0 and 28 GC/MS analysis of both the non-
nutrient control and the product flasks. The Agency believes this is
appropriate because the other measurements are not used in determining
whether a product meets the listing criterion. Additionally, the
statistical analysis has been greatly simplified, and a new decision
rule is proposed for listing determinations rather than relying on a
statistical significance test.
Gravimetric Weight Analysis: Originally, the gravimetric
weight analysis was used as a preliminary test to avoid having to
perform a GC/MS analysis. Products that failed to significantly reduce
the gravimetric weight of the oil within 28 days were considered not
effective, thereby eliminating the need to conduct the more expensive
GC/MS analysis. However, numerous compounds can give rise to positive
interferences with the gravimetric weight analysis, such as biomass
lipids and other biogenic materials, thereby rendering the gravimetric
analysis suspect. Furthermore, numerous factors can confound the
interpretation of gravimetric weight changes in oil over time. This has
led to confusion as some manufacturers have mistakenly concluded their
product passed the testing protocol simply by complying with the
gravimetric weight loss measurement. By eliminating the gravimetric
analysis altogether, EPA is streamlining the testing process, resulting
in less confusion and a modest analytical cost savings for the
manufacturer.
Most Probable Number Enumeration (Microbiological
Analysis), Nutrient Control, and Day-Seven Sampling Event: Results of
these test endpoints, while currently required, would not be used in
determining whether a product meets the proposed listing requirements.
Therefore, the Agency is proposing to eliminate these test requirements
from the proposed protocol.
28 day Sampling Event: Generally, results of
biodegradation may occur in less than 28 days, particularly for alkanes
for which biodegradation often takes place in a much shorter time
period. However, 28 days are needed to make sure that the aromatic
components, which biodegrade more slowly, have been reduced
significantly; testing protocols that accommodate aromatics are of
particular importance because of their potential ecological toxicity.
While the Agency could propose different time frames in determining
whether the product met the reduction criterion for alkanes and
aromatics, it believes that such an approach would be confusing.
Therefore, the 28 day time period is being proposed for both fractions
for simplicity and to provide sufficient time for degradation of the
aromatics.
Protocol Verification. The Agency proposes to provide a standard
culture for performing laboratories to use as a positive control
benchmark. A positive control is needed as an indication that the test
was performed properly. The Agency is proposing to use as the standard
culture an oil-degrading bacteria isolated from Disk Island in Prince
William Sound in 1990. This culture is an excellent degrader of alkanes
and aromatics in saltwater and freshwater, although it performs better
in saltwater, especially in degrading the aromatics. This culture has
the ability to degrade ANS 521 oil, with known efficacy values for both
fresh and saltwater. The proposed positive control consists of
triplicate flasks containing sterile artificial seawater or freshwater,
nutrients (salts of nitrogen and phosphorus), the weathered ANS 521
oil, and the standard culture. The performing laboratory must achieve
the known reduction in alkane and aromatic fractions in these positive
control flasks in order to certify they successfully conducted the test
procedure. Additionally, data from the positive control are required to
be submitted with the product test results. The Agency is not
proposing, however, that the positive control be repeated every time a
product test is performed. Rather, the certifying laboratory would be
required to report the results of the positive control tests conducted
within a year prior to the product testing, as part of the product
submission package. Additionally, this positive control culture would
be used as a standard microbial inoculum to test abiotic products, such
as nutrients and enzymes.
Added Nutrients. The current protocol allows the manufacturer to
request the addition of nutrients to support a culture's ability to
degrade the crude oil hydrocarbons. This addition is currently allowed
for commercial products that are strictly microbial agents and do not
contain any nutrients; the addition of nutrients is not allowed for
commercial products containing its own nutrients. A modified salt
solution of nitrogen and phosphorus is used as the mineral nutrient.
All microbial cultures need nutrients to survive and grow. In the
natural environment, biodegradation is not completely limited by
nutrient availability given that a low level flow of nutrients is
continuous. To maximize biodegradation rates, the addition of nutrients
is typically recommended in the field with a bioremediation product
unless nutrients are already high (i.e., >5 mg/L). However, in a closed
laboratory flask, the amount of nitrogen and phosphorus supplied by a
typical product might easily become limiting quickly as biodegradation
takes place because they are supplied only once at the beginning of the
test. If nutrient limitation occurs, further reduction of hydrocarbons
would likely be inhibited, and this may cause the product to fail the
listing criteria. To address this problem, the Agency proposes
modifying the protocol by allowing the addition of nutrients to any
product containing living microbes that does not contain said nutrients
in sufficient quantities to allow a fair evaluation. However, the
additional quantities allowed are limited to total concentrations of
nitrogen and phosphorus that do not to exceed the equivalent amounts
used in the positive control. Capping the amount of nutrients that can
be added to all products will yield more consistent results and more
effective comparisons among products.
Efficacy Thresholds. The Agency is proposing to revise the listing
criteria by replacing the current ``statistically significant
difference'' test with defined values for the percent reduction of
total alkane and aromatic concentrations. For a bioremediation agent to
be listed on

[[Page 3410]]

the Schedule, the Agency proposes the percent reduction of the total
alkane fraction (sum of all alkane concentrations determined by GC/MS)
to be greater than 95% at day 28, and that the percent reduction of the
total aromatic fraction (sum of all aromatic concentrations determined
by GC/MS) must be greater than 70% at day 28, both based on the one-
tailed Upper 95% Confidence Limit (UCL95) for salt water.
For freshwater, the Agency proposes the percent reduction of the total
alkane fraction (sum of all alkane concentrations determined by GC/MS)
to be greater than 95% at day 28, and that the percent reduction of the
total aromatic fraction (sum of all aromatic concentrations determined
by GC/MS) must be greater than 40% at day 28, both based on the one-
tailed Upper 95% Confidence Limit (UCL95).
Basis of Efficacy Thresholds. According to Haines et al.
(2005),\57\ the positive control culture was able to biodegrade total
alkanes in saltwater by 98.9% and total aromatics by 79.8% in 28 days,
based on the UCL90. In freshwater, the percent reduction
values were 97.9% and 37.8%, respectively, again based on the
UCL90. Thus, the proposed listing thresholds for the percent
reduction of total alkanes and total aromatics from the GC/MS analysis
are based on the findings of Haines et al. (95% for alkanes vs. 98.9%
in saltwater and 97.9% in freshwater, and 70% for aromatics in
saltwater and 40% in freshwater vs. 79.8% in saltwater and 37.8% in
freshwater). As for the positive control, the Agency believes a
reasonable target in saltwater would be 95% for total alkanes in both
types of exposure waters. For aromatics reduction, 70% is considered
reasonable in saltwater and 40% in freshwater, based on Haines et al.
EPA is using UCL95 values rather than the UCL90
values from Haines because EPA's latest research uses 6 replicates for
the test protocol which increases precision. The proposed criteria
demonstrate that the product can cause a substantial degradation of the
alkane and aromatic fractions of weathered crude oil compared to a
control, as determined solely by GC/MS analysis.
---------------------------------------------------------------------------

\57\ Haines, J.R., E.J. Kleiner, K.A. McClellan, K.M. Koran,
E.L. Holder, D.W. King, and A.D. Venosa. 2005. ``Laboratory
evaluation of oil spill bioremediation products in salt and
freshwater systems.'' J. Ind. Micorbiol. Biotechnol. 32:171-185.
---------------------------------------------------------------------------

Of note, these proposed thresholds for listing bioremediation
products on the Schedule are similar to those established for Canadian
efficacy testing, which are reductions of 30% for total aliphatics and
10% for total aromatics. The 30% reduction in total aliphatics
(including all resolvable and non-resolvable but GC-detectable
aliphatics) is approximately equivalent to an 80% reduction in total
GC/MS-resolvable target n-alkanes, based on Canadian data. The 10%
reduction in total aromatics is approximately equivalent to a 50%
reduction of the 5-aromatic homologue group consisting of naphthalene,
fluorene, dibenzothiophene, phenanthrene, and chrysene and their
alkylated homologs. The U.S. aromatic series includes 2 other 4-ring
aromatics in addition to those 5 aromatic series considered by
Blenkinsopp et al.\58\ Thus, the U.S. and Canadian protocols are
similar in terms of decision criteria. The Agency requests comments on
all the proposed changes and listing thresholds.
---------------------------------------------------------------------------

\58\ Blenkinsopp, S, G Sergy, Z Wang, MF Fingas, J Foght and DWS
Westlake. 1995. Oil spill bioremediation agents-Canadian efficacy
test protocols. Proceedings of the 1995 International Oil Spill
Conference, Feb 27-March 2, Long Beach, CA. American Petroleum
Institute, Washington, DC. pp. 91-96.
---------------------------------------------------------------------------

(2) Bioremediation Agent Toxicity
Current Requirements: The Agency currently has no bioremediation
agent toxicity testing requirements for purposes of listing these
agents on the Schedule. Section 5 of Appendix C is reserved for this
purpose. The Agency has, however, on a case-by-case basis, requested
manufacturers to test bioremediation agents for toxicity if the product
contains surfactants or other ingredients that may be harmful to the
environment.
Proposed Revisions: The Agency is proposing an acute toxicity
testing protocol for bioremediation agents to include both fresh and
saltwater. The Agency will use these testing results to determine
listing eligibility on the Schedule. The proposed testing protocols for
bioremediation agents are detailed in Appendix C. The proposed acute
toxicity test protocol for bioremediation agents is based on EPA's
protocol, Methods for Measuring the Acute Toxicity of Effluents and
Receiving Waters for Freshwater and Marine Organisms. The Agency
proposes to require bioremediation agents be tested for acute toxicity
for the product alone using fresh water species Ceriodaphnia dubia and
Pimephales promelas, and saltwater species Americamysis bahia and
Menidia beryllina. The concentration of test product causing 50%
lethality to the test organisms (LC50) lower and upper 95%
confidence intervals (LCI95 and ULCI95) are
calculated at the end of the exposure period. To be listed on the
Schedule, bioremediation agents must demonstrate an acute lethal
concentration for 50% of the test species (LC50) at the
lower 95% confidence interval greater than 10 ppm in either fresh or
salt water, consistent with the acute toxicity thresholds proposed for
dispersants. EPA's toxicity classification scheme \59\ classifies
LC50 values ranging from 10 ppm to 100 ppm as slightly
toxic, and values above 100 ppm substances are considered practically
nontoxic to aquatic organisms. By proposing this threshold level the
Agency is establishing an adequate safety margin without being overly
restrictive. The Agency requests comments on the proposed acute
toxicity methods (or any others available) and thresholds for
bioremediation agents.
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\59\ USEPA 2010. http://www.epa.gov/oppefed1/ecorisk_ders/toera_analysiseco.htm#Ecotox.
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Similarly to surface washing agents, the Agency is not proposing
provisions for conducting acute toxicity tests with bioremediation
agent-oil mixtures. The Agency is requesting comment on the need for
acute toxicity tests conducted with bioremediation agents-reference oil
mixtures. A protocol for preparation of product/oil mixtures for
toxicity testing is available for review in the docket.
(3) Listing of Non-Proprietary Nutrients
The Agency recognizes there may be oil discharge situations where
it is determined that the addition of nutrients in the form of salts of
nitrogen, phosphorus and potassium (i.e., fertilizers) to stimulate or
enhance bioremediation may be the most effective and environmentally
favorable mitigation method. However, non-proprietary commercially
available formulations of nutrients are not specifically listed on the
Schedule, even though as nutrient additives they are subject to Subpart
J requirements. Currently, an OSC may only authorize the use of an
agent not listed on the Schedule when its use is necessary to prevent
or substantially reduce a hazard to human life. Further, RRTs are not
currently able to preauthorize the use of nutrients unless they are
listed on the Schedule. To address these concerns, the Agency proposes
to include on the Schedule a specific list of the following generic
non-proprietary nutrients: Ammonium nitrate, ammonium phosphate, sodium
nitrate, potassium nitrate, urea, sodium triphosphate (or
tripolyphosphate), sodium phosphate, potassium phosphate (mono- or
dibasic), triple super phosphate, or any combination thereof. For these
non-proprietary commercial nutrients, the Agency believes there is no
need for submission of readily available

[[Page 3411]]

information. Thus, the proposal requires no technical product data or
further action on the part of a manufacturer prior to authorizing their
use in response to a discharge event. However, this listing will be
limited to products commonly formulated entirely of those mineral
nutrients and synthetically-derived urea listed. For products that may
contain additional proprietary components or have unique proprietary
formulations, the requirement for the submitter to provide the toxicity
and efficacy data under the bioremediation agent category will apply.
The Agency considered proposing a definition of ``fertilizer'' to
specifically capture the listed bioremediation agents proposed to be
exempted. However, fertilizer is a term commonly used to describe
organic nutrients, which may contain substances that do not play a role
in mitigating oil discharges, and that may have deleterious effects on
the environment. Some non-proprietary fertilizers, for example,
comprised of activated sewage sludge or manure, could contain unwanted
pathogens and trace metals that could further stress the environment if
used in response to an oil discharge. Thus, instead of an exemption
based on a fertilizer definition, EPA proposes to restrict the
exemption under the bioremediation category only to those nutrients
listed above in order to avoid any confusion. The Agency requests
comments on this approach.
(e) Solidifier Testing and Listing Requirements
The proposal defines solidifiers as substances that cause oil to
become a coherent mass, preventing oil from dissolving or dispersing
into the water column, and which are collected and recovered from the
environment. For this agent category, the Agency proposes to revise the
toxicity testing protocol and to establish a listing threshold for
toxicity in Sec. 300.915(e). Although solidifiers are intended to be
removed from the environment, the proposed revisions and new toxicity
listing threshold respond to concerns regarding the general increase in
the use of chemical and biological agents as tools available for oil
discharge responses.
(1) Solidifier Efficacy
There are currently no efficacy testing requirements in the NCP
Subpart J for solidifiers to determine listing eligibility on the
Schedule. These agents would have been captured by the current MOSCA
agent category, which currently has no efficacy testing requirements,
and which the Agency is proposing to eliminate. While the Agency is
aware of existing protocols to determine the effectiveness of
solidifiers, its focus has been on reviewing the protocols for
dispersants and bioremediation agents, given that their specific
process for affecting the oil allows them to be left in the
environment, whereas solidifiers are intended for removal from the
environment. Therefore, the Agency is not proposing an efficacy testing
methodology for solidifiers, but is requesting comment on available
methodologies and/or performance criteria (e.g., buoyancy) it can
consider.
(2) Solidifier Toxicity
Current Requirements: The current NCP Subpart J requires
solidifiers to be tested for saltwater species toxicity. Solidifier
toxicity is tested following the dispersant toxicity testing protocols
in Appendix C to part 300 of the NCP.
Proposed Revisions: The proposal revises the toxicity testing
requirements for solidifiers, including the testing protocol. While the
Agency currently provides the toxicity testing results to the OSC to
assist in authorization of use determinations, it is proposing to use
these results to determine listing eligibility on the Schedule.
The proposed revisions to the testing protocols for solidifiers are
detailed in Appendix C to part 300. The proposed acute toxicity test
protocol for solidifiers is based on EPA's protocol, Methods for
Measuring the Acute Toxicity of Effluents and Receiving Waters for
Freshwater and Marine Organisms. The Agency proposes to require
solidifiers be tested for acute toxicity for the product alone using
fresh water species Ceriodaphnia dubia and Pimephales promelas, or
saltwater species Americamysis bahia and Menidia beryllina, or both,
depending on the intended product use. The concentration of test
product causing 50% lethality to the test organisms (LC50)
and lower and upper 95% confidence intervals (LCI95 and
ULCI95) are calculated at the end of the exposure period. To
be listed on the Schedule, solidifiers must demonstrate an acute lethal
concentration for 50% of the test species (LC50) at the
lower 95% confidence interval greater than 10 ppm in either fresh or
salt water, consistent with the acute toxicity thresholds proposed for
dispersants. EPA's toxicity classification scheme \60\ considers
LC50 values ranging from 10 ppm to 100 ppm as slightly toxic
and values above 100 ppm substances practically nontoxic to aquatic
organisms. By proposing this threshold level, the Agency is
establishing an adequate safety margin without being overly
restrictive. The Agency requests comments on the proposed acute
toxicity methods (or any others available) and thresholds for
solidifiers.
---------------------------------------------------------------------------

\60\ USEPA 2010. http://www.epa.gov/oppefed1/ecorisk_ders/toera_analysis_eco.htm#Ecotox.
---------------------------------------------------------------------------

Similarly to surface washing agents, the Agency is not proposing
provisions for conducting acute toxicity tests with solidifiers-oil
mixtures. The Agency is requesting comment on the need for acute
toxicity tests conducted with solidifiers-reference oil mixtures. A
protocol for preparation of product/oil mixtures for toxicity testing
is available for review in the docket.
(3) Limitations
The Agency is proposing a conditional use listing for solidifiers.
The proposal specifies that the listing of these products is limited to
use only in those water environments for which the product was tested
and for which it met the listing threshold criteria. The Agency
recognizes that products may yield effective results in certain
environments and not in others. Products that may be effective in
freshwater may not necessarily be so in saltwater, and vice versa. The
Agency is proposing this limitation to allow product manufacturers the
flexibility to select which environment the product is to be tested and
could be authorized for use, either saltwater, fresh water, or both.
Therefore, the product would be listed and may only be authorized for
use in those water environments for which it was tested and for which
it met the listing criteria.
(f) Herding Agent Testing and Listing Requirements
The proposal defines herding agents as substances that are used to
control the spreading of oil across the water surface. For this agent
category, the Agency proposes to revise the toxicity testing protocol
and to establish a listing threshold for toxicity in Sec. 300.915(f).
While these agents are intended to be removed from the environment, the
proposed revisions and new toxicity listing threshold respond to
concerns regarding the general increase in the use of chemical and
biological agents as tools available for oil discharge responses.
Currently, there is a test requirement for distinguishing surface
collecting agents from other chemical agents (Sec. 300.915(c)(9), Test
to Distinguish Between Surface Collecting Agents and Other Chemical
Agents). Because the proposal eliminates surface collecting agents as a
category and redefines herding agents to better reflect its specific
process for affecting the oil, and

[[Page 3412]]

given that the agents will need to be identified in order for the
required testing to be submitted, the Agency is eliminating this
requirement.
(1) Herding Agent Efficacy
There are currently no efficacy testing requirements in the NCP
Subpart J for herding agents to determine listing eligibility on the
Schedule. These agents would have been captured by the current surface
collecting agent category, which currently has no efficacy testing
requirements, and which the proposal eliminates. The Agency is not
proposing an efficacy testing methodology for herding agents, but is
requesting comment on available methodologies and/or performance
criteria it can consider.
(2) Herding Agent Toxicity
Current Requirements: The current NCP Subpart J requires herding
agents to be tested for saltwater species toxicity. Herding agent
toxicity is tested following the dispersant toxicity testing protocols
in Appendix C to part 300 of the NCP.
Proposed Revisions: The proposal revises the toxicity testing
requirements for herding agents, including the testing protocol. While
the Agency currently provides the toxicity testing results to the OSC
to assist in authorization of use determinations, we are proposing to
use these results to determine listing eligibility on the Schedule.
The proposed revisions to the testing protocols for herding agents
follow the same procedures as described for surface washing agents and
are detailed in Appendix C to part 300. The acute toxicity test
protocol for herding agents is based on EPA's protocol, Methods for
Measuring the Acute Toxicity of Effluents and Receiving Waters for
Freshwater and Marine Organisms. The Agency proposes to require herding
agents to be tested for acute toxicity for the product alone using
fresh water species Ceriodaphnia dubia and Pimephales promelas, or
saltwater species Americamysis bahia and Menidia beryllina, or both,
depending on the intended product use. The concentration of test
product causing 50% lethality to the test organisms (LC50) and lower
and upper 95% confidence intervals (LCI95 and ULCI95) are calculated at
the end of the exposure period. To be listed on the Schedule, herding
agents must demonstrate an acute lethal concentration for 50% of the
test species (LC50) at the lower 95% confidence interval
greater than 10 ppm in either fresh or salt water, consistent with the
acute toxicity thresholds proposed for dispersants. EPA's toxicity
classification scheme \61\ considers LC50 values ranging
from 10 ppm to 100 ppm as slightly toxic and values above 100 ppm
substances practically nontoxic to aquatic organisms. By proposing this
threshold level, the Agency is establishing an adequate safety margin
without being overly restrictive. The Agency requests comments on the
proposed acute toxicity methods (or any others available) and
thresholds for herding agents.
---------------------------------------------------------------------------

\61\ USEPA 2010. http://www.epa.gov/oppefed1/ecorisk_ders/toera_analysis_eco.htm#Ecotox.
---------------------------------------------------------------------------

Herding agents form a monolayer of surfactants on the water surface
that result in the contraction of the oil slick.^{62 63}
Herding agent composition may include hydrocarbons, fluorosurfactants
and/or silicone-based surfactants, which suggests that a stock solution
prepared using a WAF procedure similar to solidifiers may be
appropriate. The Agency is requesting comment on the procedure for
preparing the stock solution for herding agents for the acute toxicity
tests proposed in Appendix C. Any alternative procedure for preparing
the stock solution must include an appropriate rationale in order for
the Agency to be able to consider it for final action.
---------------------------------------------------------------------------

\62\ Buist, I., Potter, S., Nedwed, T., (2011) Herding Agents to
Thicken Oil Spills in Drift Ice for In Situ Burning: New
Developments, IOSC, http://ioscproceedings.org/doi/abs/10.7901/2169-3358-2011-1-230.
\63\ Buist, I., Nedwed, T., (2011) Using Herders for Rapid In
Situ Burning Of Oil Spills on Open Water, IOSC, http://ioscproceedings.org/doi/abs/10.7901/2169-3358-2011-1-231.
---------------------------------------------------------------------------

Similarly to surface washing agents, the Agency is not proposing
provisions for conducting acute toxicity tests with herding agents-oil
mixtures. The Agency is requesting comment on the need for acute
toxicity tests conducted with herding agents-reference oil mixtures. A
protocol for preparation of product/oil mixtures for toxicity testing
is available for review in the docket.
(3) Limitations
The Agency is proposing a conditional use listing for herding
agents. The proposal specifies that these products may only be used in
those water environments for which the product was tested and for which
it met the listing threshold criteria. The Agency recognizes that
products may yield effective results in certain environments and not in
others. Products that may be effective in freshwater may not
necessarily be so in saltwater, and vice versa. The Agency is proposing
this limitation to allow product manufacturers the flexibility to
select which environment the product is to be tested and could be
authorized for use, either saltwater, fresh water, or both. Therefore,
the product would be listed and may only be authorized for use in those
water environments for which it was tested and for which it met the
listing criteria.
(g) Sorbent Requirements
The proposal defines sorbents as inert, insoluble substances that
readily absorb and/or adsorb oil or hazardous substances. Sorbents
would exclude those contaminated with substances that would interact
with the environment beyond their absorption/adsorption capabilities
(e.g., an invasive species). The proposed definition states that
sorbents are generally collected and removed from the environment and
may be used in their natural bulk form, or as manufactured products in
particulate form, sheets, rolls, pillows, or booms. The list of sorbent
materials in the proposed definition includes: Natural organic
substances (e.g., feathers, cork, peat moss, and cellulose fibers such
as bagasse, corncobs, and straw); (2) inorganic/mineral compounds
(e.g., volcanic ash, perlite, vermiculite, zeolite, clay); and (3)
synthetic compounds (e.g., polypropylene, polyethylene, polyurethane,
polyester). The Agency proposes to identify a list of known sorbent
materials, and make it publicly available so that emergency responders
can be aware and make use of such sorbents on oil discharges. The
Agency is also proposing a process for submitters to request to include
other products as sorbents if they can certify they meet the inert,
insoluble criteria.
Current Requirements: Sorbents are currently not listed on the
Schedule, but rather a list characterizing these materials is included
in section 300.915(g). The current rule allows the OSC to request
written certification from the manufacturers that their particular
sorbent product is comprised solely of those materials identified in
the rule. When a sorbent consists of materials that are not
specifically listed in the current rule, the Agency issues written
certifications, and sometimes requires testing and evaluation for
possible listing on the Schedule.
Proposed Revisions: The Agency proposes to provide a Sorbent
Product List that includes certain publicly available non-proprietary
sorbent materials. The Agency also proposes to allow submitters to
request that other products be included in this list as sorbents if
they provide the technical information required, including data to
support the claim that their product meets the sorbent definition. The
Agency recognizes that a sorbent

[[Page 3413]]

material may consist of one or more substances not specifically
identified in the proposed non-proprietary listing. For products
consisting of one or more substances not specifically identified in the
proposed listing, the Agency proposes submission requirements that
include general and product characterization information required under
paragraphs (a)(1) through (8), and paragraph (a)(13) of proposed Sec.
300.915. These include name and contact information, identification as
manufacturer or designated agent, product name/brand/trademark(s),
contact information for primary distributors or importers, product SDS,
conditions for product storage, product shelf life, and product label
samples. The proposal would additionally require the certification
statements required under paragraphs (a)(14)(iv), (a)(15), and (a)(16)
of proposed Sec. 300.915. The submitter would be required to certify
that the product does not contain specified bacterial, fungal, or viral
pathogens or opportunistic pathogens above National Ambient Water
Quality Criteria lowest density values; that the product does not
contain specified contaminants above National Water Quality Standards
levels; and that the product does not contain any of the prohibited
agents. Finally, the submitter would be required to include information
to support the claim that the product meets the sorbent definition,
including data such as its relative solubility and non-reactivity in
fresh and/or salt water. The Agency will review the submission and make
a determination to include the product as a sorbent on the Sorbent
Product List. The Agency requests comments on this approach.
Testing Options
The current Subpart J has no toxicity or efficacy testing
requirements for sorbents. There are two ASTM standards for performance
testing that could be applicable to sorbents: The ASTM F716-09 Standard
Test Methods for Sorbent Performance of Absorbents, and the ASTM F726-
12 Standard Test Method for Sorbent Performance of Adsorbents. These
methods include laboratory tests that describe the performance of these
products in removing oils that are not emulsified and other floating,
immiscible liquids from the surface of water. While these methods are
to be individually used as a basis for comparison of either absorbents
or adsorbents in a consistent manner, they are not useful for a cross
comparison of absorbents with adsorbents, even though according to ASTM
F716-09 all absorbents exhibit adsorbent properties. Further, these
agents are comprised of inert and insoluble materials that are
generally removed from the environment after use, minimizing their
potential harm. Thus, the Agency is not proposing to include efficacy
or toxicity testing requirements for these agents, but is requesting
comments on whether testing information should be included as part of
the submission requirements for other materials or products to be
included as part of the Sorbent Product List.
5. Submission of Confidential Business Information (CBI)
Currently, manufacturers may assert a claim of confidential
business information (CBI) for any information in their product package
submissions to EPA. Typically, manufacturers claim as CBI the chemical
identity (e.g., chemical name and chemical abstracts number [CAS]) and
concentration (weight percent) of each chemical component in the
product along with information about the concentrations of those
components in the product. The manufacturer may also claim certain
other information in the technical product data, including technical
data for sorbents, as CBI. EPA safeguards CBI information under the
requirements in 40 CFR part 2, subpart B. The proposal addresses the
CBI provisions for product submission under Subpart J in Sec. 300.950.
Due to the amount of dispersant used during the Deepwater Horizon
incident, and the need for the public's right-to-know about chemicals
intentionally discharged into the environment, EPA wanted to make
public information about the chemicals in the dispersant used, the
results of air and water monitoring for these chemicals, and the
concerns for human and environmental impact. A number of stakeholders
wanted to know the chemical makeup of not only the dispersant used
during the incident, but also of all other dispersants on the Schedule.
This resulted in both a number of Freedom of Information Act (FOIA)
requests and a Notice of Intent to Sue for Failure to Perform
Nondiscretionary Duties under the CWA, requesting that the Agency
release CBI for all dispersants on the Schedule.
EPA worked with the manufacturer for the dispersant used on the
Gulf in response to the Deepwater Horizon incident to make the product
chemical information publicly available (see http://www.epa.gov/bpspill/). The Agency also compiled a comprehensive aggregate list of
the chemicals used in all listed dispersants. During this process, some
manufacturers recognized the need to make information available to the
public, but also argued the need to protect proprietary business
information from competitors. Companies provided information on the
magnitude of resources expended to develop a product and test it for
listing on the Schedule; however, they argued that disclosing the
chemical components, CAS numbers, and/or concentrations for their
product would allow domestic and international competitors to freely
duplicate or reverse engineer their product and potentially drive them
out of the market. EPA is aware that over 90% of businesses on the
current Schedule are small, and that for some companies the product
they developed for the Schedule is their only business. While companies
could protect their product via the U.S. patent process, they would be
required to release components and concentrations information, which
would be made public. Manufacturers voiced concern that not only others
may use that information to tailor competitive products, but that the
U.S. patent process would offer no protection against international
competitors.
EPA believes that when chemical agents are used on oil discharges,
it is critically important for the public and all other stakeholders to
have information regarding the chemicals being added to the
environment, along with information about their toxicity and fate. This
is particularly true for major discharge events where larger quantities
of chemical or biological agents may be authorized for use. Prompt and
accurate information will allow the public to evaluate and understand
the potential human and environmental effects of these chemical agents.
While EPA understands it is essential for companies to protect their
investment in developing unique products, it is proposing limitations
to what submitters are allowed to claim as CBI in an effort to balance
public access to information with proprietary business needs. The
proposal provides that if a company submits a product for listing on
the Schedule, then it will only be allowed to claim CBI for the
concentrations of all chemical components, microbiological cultures,
enzymes, or nutrients; all other information submitted to EPA for
listing a product on the Schedule will not be considered CBI and will
be made public. While providing confidential treatment for the
concentrations of product components, the proposal allows public access
to the identity of chemical components and relevant health and
environmental effects

[[Page 3414]]

information. All other information required for a product submission
(e.g., company data, distributors, general product properties,
recommended use procedures, the product category, contaminants,
production capacities, product testing data) would already be publicly
available for commercial products, and would not constitute proprietary
business information or provide a business advantage. The Agency
requests comments on whether this approach safeguards against
duplication or reverse engineering of products by competitors and
whether other information in Subpart J should be considered as CBI.
Alternatively, the Agency considered maintaining the current
approach of allowing CBI claims for any information in their
submission. When the incident arises where affected stakeholders or the
public wants access to specific information, the Agency would request
that the company substantiate its claims and make a determination
whether to honor the claim or release the information to the public as
provided in 40 CFR part 2, subpart B. The Agency also considered
modifying the current approach by making the component identity and
concentration information public without further notice or action for
major discharge events or SONS, or for events where a given amount of
chemical or biological agent would be allowed for use. Finally, another
option for modifying the current approach would be to allow
manufacturers to waive CBI claims only for certain chemical components
for monitoring purposes (e.g. manufacturer identifies a ``marker''
component as a condition for listing) was also considered. The Agency
is rejecting the current approach because it does not believe that,
even with the modifications considered, it offers the appropriate
balance between the public interest and business needs.
EPA also considered developing an aggregate list of components used
in categories of chemical and biological agents for public disclosure.
For example, a list of all the chemicals used in listed dispersants, a
separate list for those substances used in surface washing agents, etc.
This would allow information to be disassociated with specific products
and protected from reverse engineering or duplication of products by
competitors, while providing public access. The concern with this
approach is how to update the aggregate list for new products without
potentially revealing the components added to the list for that new
product. Further, in the event of a major discharge or SONS, the
interest will be for information and monitoring data specific to the
product being used. Consequently, EPA is not adopting this approach,
but requests comments on these and other options to handle CBI while
balancing all interests.
6. Addition of a Product to the Schedule
The proposal establishes the requirements for submitters to request
a product be listed on the Schedule in Sec. 300.955. It provides
administrative information, such as the address where to submit the
package, as well as details of the requirements for a complete
submission package. Additionally, it addresses how a submitter may
request a listing determination review and the requirements when there
are changes in a listed product. Finally, the proposal addresses the
process the Agency will follow to review all new submissions, requests
for review of decisions and product changes, as well as how it will
transition from the current Schedule to a new one that reflects the new
and amended testing and data requirement.
Submission. The proposal updates the address where the package is
to be submitted.
Package contents. The proposal specifies a complete package must
include, as follows:
A company letter certifying all testing was conducted on
representative product samples at a nationally or internationally
accredited laboratory, that it was conducted in accordance with all
technical rule requirements, and that all test results and product
technical data and information reported are true and accurate;
A numbered Table of Contents showing all required
information and data submitted;
All required data and information (both general and
product category specific) in the order the requirements appear in the
rule; and
A separate inner envelope labeled: ``CONFIDENTIAL BUSINESS
INFORMATION--TO BE OPENED BY THE PRODUCT SCHEDULE MANAGER ONLY'', if
applicable.
Because of their intended function in responding to oil discharges,
products listed on the Schedule will certainly impact the environment.
It is important that the information provided by the submitter is true
and accurate, as it serves as the basis for evaluating those potential
environmental impacts. The Agency believes that it is appropriate for
the submitter to be held accountable for the technical data and
information provided to make these listing determinations. Thus, the
proposal requires the submitter to certify the accuracy of the
information submitted, and will reject any submission that is
determined to be incomplete or non-compliant, misleading, or
inaccurate.
The requirements for a Table of Contents and for the information to
be organized as it appears in the regulation are intended to make the
Agency review process as efficient as possible. These requirements will
assist the Agency in conducting a quick and accurate review, both
during the transition period, as well as for future submissions, by
generally simplifying the review process.
While the Agency needs to process packages containing information
claimed to be CBI with additional safeguards, it is the responsibility
of the submitter to ensure that this information comes to the Agency
clearly identified as such. Therefore, the proposal requires a separate
and clearly marked envelope for CBI to ensure proper handling.
EPA Review. The proposal maintains most of the existing Agency
process for reviewing product submissions. A revision to the current
process increases the number of days allowed for the Agency to complete
its product review from the current 60 days to 90 days from the date of
receipt. This proposed change considers the additional technical data
and information proposed to be required, as well as the Agency's past
experience with submission packages based on the current requirements.
EPA will first review the package for completeness and compliance
with all data and information requirements and will contact the
submitter to verify information, or to request clarification or
additional information, including a product sample, as necessary. The
Agency will make product listing determinations based on a technical
evaluation of all data and information submitted, any relevant
information on impacts or potential impacts of the product or any of
its components on human health or the environment, and on the intended
use of the product. The Agency reserves the right to make a
determination on whether the product will be listed, and under which
category. For products that may meet more than one category (e.g., a
product that meets both the bioremediation and dispersant agent
criteria), the Agency requests comments on whether there should be any
product listing limitations beyond those identified for each individual
product category. Within the 90-day timeframe, the Agency will notify
the submitter, in writing, of its decision to either list the product
on the Schedule and under which category or categories, or of its
decision and supporting rationale to reject the submission. Submitters
may

[[Page 3415]]

revise submission packages to address test results, data, or
information deficiencies and resubmit them. Because the Agency will
need a complete set of data and technical information to make a listing
determination, the 90-day review time period will start anew once a
complete package is resubmitted.
Request for review of decision. The proposal is not substantively
changing the process for a submitter to request that the Agency review
its determination on a product. If the Agency rejects a product for
listing on the Schedule, the proposal continues to allow for a
submitter to appeal to the EPA Administrator to review its
determination to reject the product listing. The proposal maintains the
requirement that such a request be in writing, within 30 days of
receipt of the written notification of EPA's decision not to list the
product on the Schedule. The request to review the Agency's
determination must include a clear and concise statement with
supporting facts and technical analysis that demonstrates why the
submitter believes the Agency's assessment of the product was
incorrect. The proposal allows the Administrator to request additional
information or a meeting opportunity. Within 60 days of receipt of any
such request, or within 60 days of receipt of any requested additional
information, the proposal requires the Administrator or her designee to
notify the submitter in writing of the review decision, maintaining the
current timeframe.
Changes to a product listing. The Agency proposes to revise the
provisions for notification of changes to a product listing. Submitters
must notify EPA in writing within 30 days of any changes to the general
product information submitted for listing on the Schedule so the OSCs
have timely updated information. The proposal revises the notification
requirement to include details of the specific changes to information
submitted under Sec. 300.915(a)(1) through (8) and Sec.
300.915(a)(19) through (21) for a product on the Schedule, including
the reasons for such changes and the supporting data and information,
and maintains the provision allowing EPA to request additional
information and clarification regarding these changes. For any changes
to the chemical components and/or their concentrations, the proposed
revisions would require retesting of the product according to the
requirements for the product category, and the resubmission of a
complete new package for a new review and consideration for a listing
determination by the Agency of the reformulated product. While the
Agency currently has and is retaining the option of requiring
additional testing, it believes that when the chemical components or
concentrations of a product change, an automatic retesting requirement
is merited. The Agency believes this requirement is appropriate when
the identity of the product itself changes; the only way of evaluating
the potential effects of these changes on the efficacy and toxicity of
a new product formulation is to retest it. The Agency considered
whether it was necessary to explicitly provide the flexibility to waive
this requirement under extraordinary circumstances (i.e., a SONS
event). However, OSCs already have broad authority to use agents in
areas impacted or threatened by a release or discharge, whether the
agent is identified or not on the Schedule, to prevent or substantially
reduce an immediate threat to human life. In addition, the Agency
considered whether there is a chemical concentration threshold that
could accommodate minor adjustments to a product. For example, a
producer may make a slight variation in a product formula to account
for a food grade or technical grade chemical component. Such a
threshold might be that if concentration changes vary by no more than
1%, no retesting is necessary. However, the Agency has no basis for
such a threshold and requests comment on this approach with appropriate
technical details. Because of this, and the concern for the potential
impact reformulated products may have on the environment, the Agency is
proposing to require retesting whenever the chemical components or
concentrations of a product change. However, the Agency is requesting
comments on whether it should require the retesting of all products
that have a change in composition, even if the only change is of
chemical components that may considered inert.
Transitioning Listed Products from the Current Schedule to the New
Schedule. The Agency believes it important that products on the current
Schedule continue to be available during the transition period to a new
Schedule that reflects the amended requirements. During this transition
period, all products on the current Schedule will remain conditionally
listed and the Agency will rely on it for planning and response
activities. Because of the proposed revisions to test protocols and
listing criteria, and because of the additional test requirements, the
Agency proposes that all products currently on the Schedule be
retested, and that the new data and information be submitted to the
Agency for reevaluation of the current listings within 24 months of the
effective date of a final rule. The Agency believes this provides
adequate time for submitters to prepare and submit new packages to EPA
and for the Agency to review and make decisions on these products. For
a product to be transitioned from the current Schedule to the new
Schedule, manufacturers would be required to submit a new, complete
package according to the amended test and listing criteria, and EPA
would need to make a favorable finding to list the product on the new
Schedule, either as currently listed or with modifications. Products on
the current Schedule for which a new submission is not received, or
that upon review of their submissions do not meet the revised listing
criteria, would be removed from the Schedule at the end of the 24-month
transition period. While the Agency is reviewing the new submission
packages, planning and response authorities are encouraged to consider
those products that based on existing data would meet the revised
listing criteria. While the existing data may be limited and likely
developed with different protocols, considering the new requirements in
selecting products for planning and response activities would provide
an increased level of environmental protection. The Agency notes,
however, that this is not a requirement, and that the proposal would
allow any product on the current Schedule to be authorized for use
following the current protocols, until the 24-month transition period
is over. The Agency is requesting comments on the practicability of
this transition process, and whether the 24-month period allows
sufficient time for retesting of products on the current Schedule, and
for EPA to review and make listing determinations on the submissions
for the new Schedule. The Agency also requests comments on potential
R&D costs of modifying existing products to meet the new requirements
that could be incurred during this transition.
7. Mandatory Product Disclaimer
The current requirements provide that the listing of a product on
the Schedule does not constitute approval or endorsement of the
product. To avoid possible misinterpretation or misrepresentation, the
Agency currently requires that any label, advertisement, or technical
literature that refers to the placement of the product on the Schedule
must either reproduce in its entirety EPA's written notification that
it will add the product to the Schedule

[[Page 3416]]

currently in Sec. 300.920(a)(2) or (b)(2), or include the disclaimer
currently set forth in Sec. 300.920(e). It remains the Agency's
position that listing a product on the Schedule does not constitute
approval or endorsement of that product, nor a recommendation of its
use. The Agency continues to believe that it is important to avoid any
possible misinterpretation or misrepresentation of this policy. Thus,
the requirement for a disclaimer to be included on any label,
advertisement, or technical literature for the product is maintained.
However, the proposal removes the alternative to reproduce in its
entirety EPA's written notification that it will add the product to the
Schedule currently in Sec. 300.920(a)(2) or (b)(2). The Agency
believes it will be able to update the Schedule list within a
reasonable timeframe given the advances in information technology, and
thus the option of producing the EPA letter of notification for a
product listing should no longer be necessary. The Agency is proposing
to modify the disclaimer language as follows:

[PRODUCT NAME] is listed on the National Contingency Plan (NCP)
Product Schedule. This listing does NOT mean that EPA approves,
recommends, licenses, or certifies the use of [PRODUCT NAME] on an
oil discharge. This listing means only that data have been submitted
to EPA as required by Subpart J of the NCP. Only a Federal On-Scene
Coordinator (OSC) may authorize use of this product according to the
NCP.

The proposed revisions set forth in Sec. 300.965 are intended to
clarify that the use of these products is conditional to OSC
authorization following the requirements set forth under the NCP
regulations. The disclaimer language must continue to be conspicuously
displayed in its entirety, and must be fully reproduced on all product
literatures, labels, and electronic media, including Web site pages. As
discussed in the next section, a product can be removed from the
Schedule if the submitter does not comply with the disclaimer
requirements, or makes any improper attempt to demonstrate the approval
or endorsement of a product. The Agency requests comments on the
proposed revisions.
8. Removal of a Product From the Schedule
Products that are not properly used in the field may cause harm to
human health and the environment, and may constitute violations of the
CWA, and other federal, state, or local laws. Misleading, inaccurate,
or incorrect statements within a product submittal package or within
language that refers to the listing of a product on the Schedule may
result in their improper or incorrect use. Falsification of federal
documents, unsupported toxicity or efficacy claims, submission of
incorrect product composition or use information, or withholding
technical product data are some examples of these acts. To minimize
potential misuse of listed products, the Agency believes it is
appropriate to further clarify the criteria for the removal of a
product from the Schedule. In Sec. 300.970 the proposal specifically
includes, but does not limit, as causes for removal from the Schedule:
Any misleading, inaccurate, or incorrect statements within the product
submission to EPA or to any person or private or public entity
regarding the composition or use of the product to remove or control
oil discharges, including on labels, advertisements, or technical
literature; any alterations to the chemical components, concentrations,
or use conditions of the product without proper notification to EPA as
required by Sec. 300.955(e); the failure to print the disclaimer
provided in Sec. 300.965 on all labels, advertisements, or technical
literature; or any new or previously unknown relevant information
concerning the impacts or potential impacts of the product to human
health or the environment. It also establishes a process for removal if
the Agency obtains evidence of cause for removal. EPA would notify the
submitter in writing, at the address of record, of its reasons for
removal of the product from the Schedule. The proposal would allow for
an appeals process similar to the one set forth for listing
determinations. Appeals must be received within 30 days of receipt of
EPA's removal notification and must contain a clear and concise
statement with supporting facts and technical analysis demonstrating
why the submitter believes EPA's decision was incorrect. Written
notification from the Administrator will be sent to the submitter
within 60 days of any appeal, or within 60 days of receipt of any
requested additional information. However, if no appeal is received
within the 30 days of receipt of EPA's removal notification, the
product would be delisted without further notice. The Agency requests
comments on the proposed clarification of criteria for removal of
products from the Schedule, and on the associated appeals process.
9. Appendix C to Part 300
The Agency is proposing to revise the current Appendix C--Swirling
Flask Dispersant Efficacy Test, Revised Standard Dispersant Toxicity
Test, and Bioremediation Agent Efficacy Test as Appendix C--
Requirements for Product Testing Protocols and Summary Test Data:
Dispersant Baffled Flask Efficacy and Toxicity Tests; Standard Acute
Toxicity Test for Bioremediation Agents, Surface Washing Agents,
Herding Agents, and Solidifiers; and Bioremediation Agent Efficacy
Test. The proposed revisions reflect the proposed new and revised
testing protocols for listing agents on the Schedule. The details of
the technical changes and rationale are discussed for each agent in
section V.C.4 of this preamble--Data and Information Requirements for
Product Schedule Listing. The appendix reflects the proposed technical
considerations and listing requirements. The Agency is requesting
comment on the protocols and their technical rationale. The Agency is
also requesting comment on its organization and ease of use.
10. Appendix E to Part 300
The 1994 revisions to the NCP established Appendix E, Oil Spill
Response, which separates the oil spill response requirements of the
NCP from the hazardous substance release requirements (59 FR 47414).
The purpose of creating this appendix was to compile general oil
discharge response requirements into one document to aid responsible
parties and responders with their duties under the national response
system. The Agency's intent was to provide guidance, and not to alter
in any way the meaning or policy stated in other sections or subparts
of the NCP. However, some minor variations between the Appendix E
provisions and the analogous provisions of the NCP rule language were
necessary to ensure that the appendix addressed only oil discharges;
hazardous substance releases continue to be addressed in the NCP rule
but are not addressed in Appendix E.
The Agency proposes to remove Appendix E. While having all of the
information pertaining to oil discharges compiled in one location may
offer useful guidance, it is not necessary that this guidance be
codified as a regulatory appendix to the NCP. The provisions in the
appendix do not alter any NCP requirement; however, they do contain
variations from the main NCP requirements in order to have the appendix
be relevant solely to oil discharges. While EPA carefully reviewed the
appendix and the relevant sections of the NCP at the time it was
established to ensure consistency in policy, instructions, guidance and
requirements, there were intentional minor variations. These may result
in having responses to oil discharges

[[Page 3417]]

subject to two sets of what appear to be potentially conflicting
requirements, causing unnecessary confusion.
Because all requirements in Appendix E are part of the NCP, any
revisions to the NCP necessitate revisions to this appendix. This adds
burden not only for the Agency in revising and ensuring consistency,
but also for the regulated community in reviewing redundant and
duplicative requirements. While it may be a useful tool to have all of
the oil discharge specific requirements in one location, the Agency has
reconsidered its position and believes that this is more appropriately
achieved through a separate guidance document, one that does not codify
duplicative regulatory requirements. The Agency requests comments on
the proposal to remove Appendix E from the NCP regulation, and whether
it should continue to offer similar guidance through other formats.

VI. Summary of Proposed Rule Provisions

This section summarizes the proposed changes to 40 CFR parts 110
and 300. Subpart J has been renumbered to include new, consolidated,
and revised sections. Some of the rule sections have been retained,
removed, or moved in their entirety. The Table below provides an
overview of the existing rule and proposed rule citations for a quick
reference of the proposed changes.
Section 110.4, Dispersants, would be revised to link the rule with
the new and amended regulatory definitions for Subpart J product
categories.
Section 300.5, Definitions, would be revised to include new,
amended, and deleted definitions.
Subpart J--Use of Dispersants, Chemicals, and Bioremediations
Agents, heading would be revised to reflect new and amended regulatory
definitions for product categories.
Section 300.900, General, paragraphs (a) and (c) would be revised
to reflect new and amended regulatory definitions for product
categories.
Section 300.905, NCP Product Schedule, would be removed.
Section 300.910, Authorization of Use, would be revised and new
paragraphs added to clarify planning and preauthorization
responsibilities.
Paragraph (a) would be revised to clarify the
requirements, including process, responsibilities, and factors to
consider for preauthorization; and add new requirements for
preauthorization plan review, concurrence, and withdrawal procedures.
Paragraph (b) would be revised to clarify the requirements
for using a listed product not addressed by a preauthorization plan and
add new parameters for use considerations.
Paragraph (c) would be revised to clarify the requirements
for authorizing the use of burning agents by an OSC for authorized in-
situ burns.
Paragraph (d) would be revised to clarify the exception
requirements and add specific time frames for notification of continued
agent use.
Paragraph (e) would be revised to expand the prohibition
to include nonylphenol (NP) or nonylphenol ethoxylates (NPEs) as
components of chemical or biological agents.
Paragraph (f) would be revised to add new regulatory
requirements for agent storage and use. Existing paragraph (f)
requirements would be moved to new paragraph (g), Supplemental Testing,
Monitoring, and Information.
New paragraph (g), Supplemental Testing, Monitoring, and
Information, would revise the regulatory text to clarify the
requirements for supplemental testing, monitoring and information.
New paragraph (h), Recovery of Oil and Agents from the
Environment, would add regulatory requirements for recovery of oil and
agents from the environment.
New paragraph (i), Reporting of Agent Use, would add
regulatory requirements for notification of agent use on an oil
discharge.
New section 300.913, Monitoring the Use of Dispersants, would add
regulatory requirements for monitoring certain prolonged surface and
subsurface use of dispersants.
Section 300.915, Data Requirements, would be revised to consolidate
general submission requirements applicable to all product categories.
The section would be restructured to include new testing and listing
requirements for specific product categories.
Paragraph (a), Dispersants, would be revised to
consolidate general testing and listing requirements from existing
paragraphs (a), (b), (d), and (f). The paragraph would include
revisions and new requirements for the identification of and testing
for all product categories designated for listing. Existing paragraph
(a) requirements specific to dispersants would be moved to new section
300.915(b), Dispersant Testing and Listing Requirements. The paragraph
would also be revised to add new toxicity and efficacy testing
requirements, limitations for use, and new criteria for listing a
dispersant to the Schedule. Existing paragraph (b) would be moved to
new paragraph (c), Surface Washing Agent Testing and Listing
Requirements.
Paragraph (b), Surface Washing Agents, would be moved to
new paragraph (c), Surface Washing Agent Testing and Listing
Requirements. The paragraph would be revised to add new toxicity and
efficacy testing requirements, limitations for use, and new criteria
for listing a surface washing agent to the Schedule. Existing paragraph
(c), Surface Collecting Agents, would be deleted.
Paragraph (d), Bioremediation Agents, would be revised to
add new toxicity and efficacy testing requirements, limitations for
use, and new criteria for listing a bioremediation agent to the
Schedule. Existing paragraphs (d)(9) and (10) were moved to new
paragraph (a), General Product Information.
Paragraph (e) would be revised to add new regulatory
requirements for submission and listing of a solidifier. Existing
paragraph (e), Burning Agents, would be deleted.
Paragraph (f) would be revised to add new toxicity testing
requirements, limitations of use, and criteria for listing a herding
agent on the Schedule. Existing paragraph (f), Miscellaneous Oil Spill
Control Agents, would be deleted.
Paragraph (g), Sorbents, would be revised to add new
exceptions for listing a sorbent to the Schedule.
Section 300.920, Addition of Products to Schedule, would be moved
to new section 300.955, Addition of a Product to the Schedule.
Paragraph (a) would be revised to include submission
instructions for all product categories. Existing paragraphs (a)(1)
through (3) regulatory text specific to dispersant applications would
be moved to new Sec. Sec. 300.915(b) and 300.955(c) and (d).
Paragraph (b) would be revised to add new regulatory text
for preparation of complete submission packages. Existing paragraph (b)
regulatory text would be moved to new Sec. 300.955(c) and (d).
Paragraph (c) would be revised to add regulatory text for
EPA's review of submission packages and decision criteria for listing.
Existing paragraph (c) would be moved to new Sec. 300.950, Submission
of Confidential Business Information (CBI).
Paragraph (d) would be revised to add regulatory text for
requesting a listing decision review. Existing paragraph (d) would be
moved to new Sec. 300.955(e), Changes to a Listed Product.
Paragraph (e) would be revised to add new regulatory text
for notification of changes to a listed product. Existing paragraph (e)
would be moved to new

[[Page 3418]]

Sec. 300.965, Mandatory Product Disclaimer.
New paragraph (f) would add new regulatory requirements
for transitioning products on the current Schedule to the new Schedule.
New Sec. 300.950, Confidential Business Information (CBI), would
revise and clarify the allowable CBI claims in a submission package.
New Sec. 300.965, Mandatory Product Disclaimer, would clarify the
regulatory text for including a disclaimer statement on all product
labels and literature.
New Sec. 300.970, Removal of a Product from the Schedule, would
add basis for removal of products from the Schedule, EPA notification
of decision, and appeals process.
Revised Appendix C to Part 300--Requirements for Product Testing
Protocols and Summary Test Data: Dispersant Baffled Flask Efficacy and
Toxicity Tests; Standard Acute Toxicity Test for Bioremediation Agents,
Surface Washing Agents, Herding Agents, and Solidifiers; and
Bioremediation Agent Efficacy Test.
Removed Appendix E to Part 300--Oil Spill Response.

40 CFR Part 100 Discharge of Oil--Distribution Table
------------------------------------------------------------------------
Current citation Proposed rule citation
------------------------------------------------------------------------
110.4 Dispersants...................... 110.4 Chemical and Biological
Agents.
------------------------------------------------------------------------

40 CFR Part 300--National Oil and Hazardous Substances Pollution
Contingency Plan--Distribution Table
------------------------------------------------------------------------
Current citations Proposed rule citations
------------------------------------------------------------------------
Sec. 300.5 Definitions............... Sec. 300.5 Definitions.
Subpart J--Use of Dispersants and Other Subpart J--Use of Dispersants,
Chemicals. and Other Chemical and
Biological Agents.
Sec. 300.900 General................. Sec. 300.900 General.
Sec. 300.900(a)...................... Sec. 300.900(a)
Sec. 300.900(c)...................... Sec. 300.900(c)
Sec. 300.905 NCP Product Schedule.... Deleted.
Sec. 300.910 Authorization of Use.... Sec. 300.910 Authorization
for Agent Use.
Sec. 300.910(a)...................... Sec. 300.910(a) Use of Agents
Identified on the Schedule on
Oil Discharges Addressed by a
Preauthorization Plan.
Sec. 300.910(b)...................... Sec. 300.910(b) Use of Agents
Identified on the Schedule on
Oil Discharges Not Addressed
by a Preauthorization Plan.
Sec. 300.910(c)...................... Sec. 300.910(c) Burning
Agents.
Sec. 300.910(d)...................... Sec. 300.910(d) Exceptions.
Sec. 300.910(e)...................... Sec. 300.910(e) Prohibited
Agents.
Sec. 300.910(f)...................... Sec. 300.910(g) Supplemental
Testing, Monitoring, and
Information.
Sec. 300.910(f) Storage and
Use of Agents.
Sec. 300.910(h) Recovery of
Oil and Agents from the
Environment.
Sec. 300.910(i) Reporting of
Agent Use.
Sec. 300.913 Monitoring the
Use of Dispersants.
Sec. 300.913(a).
Sec. 300.913(b).
Sec. 300.913(c).
Sec. 300.913(d).
Sec. 300.913(e).
Sec. 300.913(f).
Sec. 300.915 Data Requirements....... Sec. 300.915 Data and
Information Requirements for
Product Schedule Listing.
Sec. 300.915(a)(1) through (12) Sec. 300.915(a)(1) through
Dispersants. (21) General Product
Information.
Sec. 300.915(b) Dispersant
Testing and Listing
Requirements.
Sec. 300.915(b) Surface Washing Sec. 300.915(a)(1) through
Agents. (21) General Product
Information.
Sec. 300.915(c) Surface
Washing Agent Testing and
Listing Requirements.
Sec. 300.915(c) Surface Collecting Deleted.
Agents.
$300.915(d) Bioremediation Agents...... Sec. 300.915(a)(1) through
(21) General Product
Information.
Sec. 300.915(d)
Bioremediation Agent Testing
and Listing Requirements.
Sec. 300.915(e) Burning Agents....... Deleted.
Sec. 300.915(f) Miscellaneous Oil Deleted.
Spill Control Agents.
Sec. 300.915(g) Sorbents............. Sec. 300.915(g) Sorbent
Listing Requirements.
Sec. 300.915(h) Mixed Products....... Deleted.
Sec. 300.915(e) Solidifier
Testing and Listing
Requirements, including Sec.
300.915(a)(1) through (21)
General Product Information.
Sec. 300.915(f) Herding Agent
Testing and Listing
Requirements, including Sec.
300.915(a)(1) through (21)
General Product Information.
Sec. 300.920 Addition of Products to Sec. 300.955 Addition of a
Schedule. Product to the Schedule.
Sec. 300.920(a)(1) Dispersants....... Sec. 300.955(a) Submission.
Sec. 300.915(b) Dispersant
Testing and Listing
Requirements.
Sec. 300.920(a)(2)................... Sec. 300.955(c) EPA Review.
Sec. 300.920(a)(3)................... Sec. 300.955(d) Request for
Review of Decision.
Sec. 300.955(b) Package
Contents.
Sec. 300.920(b)(1) Surface Washing Sec. 300.955(a) Submission.
Agents, Surface Collecting Agents,
Bioremediation Agents, and
Miscellaneous Oil Spill Control Agents.

[[Page 3419]]

Sec. 300.920(b)(2)................... Sec. 300.955(c) EPA Review.
Sec. 300.920(c)...................... Sec. 300.950 Submission of
Confidential Business
Information (CBI).
Sec. 300.920(d)...................... Sec. 300.955(e) Changes to a
Listed Product.
Sec. 300.955(f) Transitioning
Listed Products from the
Current Schedule to the New
Schedule.
Sec. 300.920(e)...................... Sec. 300.965 Mandatory
Product Disclaimer.
Sec. 300.970 Removal of a
Product from the Schedule.
------------------------------------------------------------------------

VII. Statutory and Executive Order Reviews

A. Executive Order 12866: Regulatory Planning and Review and Executive
Order 13563: Improving Regulation and Regulatory Review

Under Executive Order 12866 (58 FR 51735, October 4, 1993), this
action is a ``significant regulatory action.'' This action raises novel
legal or policy issues arising out of legal mandates, the President's
priorities, or the principles set forth in the Executive Order.
Accordingly, EPA submitted this action to the Office of Management and
Budget (OMB) for review under Executive Orders 12866 and 13563 (76 FR
3821, January 21, 2011) and any changes made in response to OMB
recommendations have been documented in the docket for this action.
In addition, EPA prepared an analysis of the potential costs and
benefits associated with this action. This analysis is contained in the
Regulatory Impact Analysis for Proposed Revisions to the National Oil
and Hazardous Substances Pollution Contingency Plan Regulations. A copy
of the analysis is available in the docket for this action and the
analysis is briefly summarized here.
The Agency expects the proposed rule would not cause a significant
economic impact on a substantial number of small businesses. The total
incremental costs are estimated as $667,610 to $694,343 annually at 3%
and 7% ($2011) annualization rates, respectively. The benefits of this
action are assessed qualitatively and include, for example, greater
clarity of regulatory requirements, as well as less toxic products. The
resulting ratio of compliance cost to annual sales revenue for the
proposed rule for existing and new product manufacturers would be less
than one percent in most instances.

B. Paperwork Reduction Act

The information collection requirements in this proposed rule have
been submitted for approval to the Office of Management and Budget
(OMB) under the Paperwork Reduction Act, 44 U.S.C. 3501 et seq. The
Information Collection Request (ICR) document prepared by EPA has been
assigned EPA ICR number 1664.10. You can find a copy of the ICR in the
docket for this rule, and it is briefly summarized here. The ICR
supporting this proposed rule is largely self-implementing. The
information collection is to ensure that: (1) The Agency has the
necessary information to make Schedule listing determinations specific
to the different product categories; (2) product use by owners or
operators of facilities or vessels, or response personnel, in response
to oil discharges is performed in accordance with all applicable
requirements; and (3) the Agency can verify compliance as needed.
Section 300.950 of the NCP contains provisions for confidentiality.
EPA has carefully considered the burden imposed upon the regulated
community by the proposed regulations. EPA believes that the activities
required are necessary and, to the extent possible, has attempted to
minimize the burden imposed. The minimum requirements specified in the
proposed rule are intended to ensure that, when needed, products are
used properly in the field to respond to an oil discharge in a manner
protective of human health and the environment.
Respondents/affected entities: Manufacturers of oil spill
mitigating agents (products)/Oil spill responsible parties.
Respondent's obligation to respond: Mandatory (40 CFR Part 300,
Subpart J).
Estimated number of respondents: 65.
Frequency of response: Initially.
Total estimated burden: 721 hours (per year). Burden is defined at
5 CFR 1320.3(b).
Total estimated cost: $584,504 (per year), includes $575,400
operation & maintenance costs.
An agency may not conduct or sponsor, and a person is not required
to respond to, a collection of information unless it displays a
currently valid OMB control number. The OMB control numbers for EPA's
regulations in 40 CFR are listed in 40 CFR part 9.
Submit your comments on the Agency's need for this information, the
accuracy of the provided burden estimates, and any suggested methods
for minimizing respondent burden to the EPA using the docket identified
at the beginning of this rule. You may also send your ICR-related
comments to OMB's Office of Information and Regulatory Affairs via
email to oria_submisssions@omb.eop.gov, Attention: Desk Officer for
EPA. Since OMB is required to make a decision concerning the ICR
between 30 and 60 days after receipt, OMB must receive comments no
later than February 23, 2015. The EPA will respond to any ICR-related
comments in the final rule.

C. Regulatory Flexibility Act (RFA)

The Regulatory Flexibility Act (RFA) generally requires an agency
to prepare a regulatory flexibility analysis of any rule subject to
notice and comment rulemaking requirements under the Administrative
Procedure Act or any other statute unless the agency certifies that the
rule will not have a significant economic impact on a substantial
number of small entities. Small entities include small businesses,
small organizations, and small governmental jurisdictions.
For purposes of assessing the impacts of the proposed rule on small
entities, small entity is defined as: (1) As defined by the Small
Business Administration's (SBA) regulations at 13 CFR 121.201; (2) a
small governmental jurisdiction that is a government of a city, county,
town, school district or special district with a population of less
than 50,000; or (3) a small organization that is any not-for-profit
enterprise that is independently owned and operated and is not dominant
in its field.
After considering the economic impacts of this proposed rule on
small entities, I certify that this action will not have a significant
economic impact on a substantial number of small entities. The small
entities directly regulated by this proposed rule are product

[[Page 3420]]

manufacturers and laboratories and state and local governments that are
involved in product development, testing and use for oil discharge
response. EPA conducted a small business analysis consistent with the
Agency's 2006 small business guidance. The Agency's analysis indicates
that about 95 percent of manufacturers are small businesses. In
conducting the small business analysis, the agency compared the
incremental annualized compliance costs to the annual sales revenue for
the smallest entities. The results indicate that 90 percent of the
smallest manufacturers have annualized compliance costs that are less
than 1 percent of their annual sales revenue, and that no manufacturers
are expected to have incremental costs that exceed 3 percent of annual
sales. The small business analysis is available for review in the
Regulatory Impact Analysis (RIA). Therefore, we have determined that
this proposed rule does not have a significant impact on a substantial
number of small entities.
Nonetheless, EPA has tried to reduce the impact of this rule on
small entities in developing the regulatory requirements that balance
the costs and burden, while addressing the environmental protection
concerns. We continue to be interested in the potential impacts of this
proposed rule on small business entities and welcome comments on the
issues related to such impacts.

D. Unfunded Mandates Reform Act

This action contains no Federal mandates under the provisions of
Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), 2 U.S.C.
1531-1538 for State, local, or tribal governments or the private
sector. This proposed rule imposes no new enforceable duty on any
state, local or tribal governments or the private sector. UMRA excludes
from the definition of ``Federal intergovernmental mandate'' and
``Federal private sector mandate'' duties that arise from conditions of
Federal assistance. UMRA generally excludes from the definition of
``Federal intergovernmental mandate'' duties that arise from
participation in a voluntary Federal program. UMRA also excludes from
the definition of ``Federal private sector mandate'' duties that arise
from participation in a voluntary Federal program. Since the decision
on whether to request that a product be included on the Schedule is
voluntary, the Agency has determined that this proposed rule is not
subject to the requirements of sections 202 or 205 of UMRA. This action
is also not subject to the requirements of section 203 of UMRA because
it contains no regulatory requirements that might significantly or
uniquely affect small governments.

E. Executive Order 13132: Federalism

This action does not have federalism implications. It will not have
substantial direct effects on the States, on the relationship between
the national government and the States, or on the distribution of power
and responsibilities among the various levels of government, as
specified in Executive Order 13132. This proposal does not alter the
general procedures already defined in the NCP of how state, local, and
federal agencies cooperate in responding to oil spills and how to
consult with the OSC and RRT when considering the use of products on
the Schedule. Thus, Executive Order 13132 does not apply to this
action. In the spirit of Executive Order 13132, and consistent with EPA
policy to promote communications between EPA and State and local
governments, EPA specifically solicits comment on this proposed action
from State and local officials.

F. Executive Order 13175: Consultation and Coordination With Indian
Tribal Governments

Subject to Executive Order 13175 (65 FR 67249, November 9, 2000),
EPA may not issue a regulation that has tribal implications, that
imposes substantial direct compliance costs, and that is not required
by statute, unless the Federal government provides the funds necessary
to pay the direct compliance costs incurred by tribal governments, or
EPA consults with tribal officials early in the process of developing
the proposed regulation and develops a tribal summary impact statement.
EPA has concluded that this action may have tribal implications.
However, it will neither impose substantial direct compliance costs on
tribal governments, nor preempt Tribal law, similarly to the effect on
states. EPA will be consulting with tribal officials as it develops
this regulation to permit them to have meaningful and timely input into
its development. Consultation will include conference calls, webinars,
and meetings with interested tribal representatives to ensure that
their concerns are addressed before the rule is finalized. In the
spirit of Executive Order 13175 and consistent with EPA policy to
promote communications between EPA and tribal governments, EPA
specifically solicits comment on this proposed rule from tribal
officials.

G. Executive Order 13045: Protection of Children From Environmental
Health Risks and Safety Risks

EPA interprets EO 13045 (62 FR 19885, April 23, 1997) as applying
only to those regulatory actions that concern health or safety risks,
such that the analysis required under section 5-501 of the EO has the
potential to influence the regulation. This action is not subject to EO
13045 because it does not establish environmental standards, such as
limits on levels of pollutants in the water, that are intended to
directly mitigate health or safety risks.

H. Executive Order 13211: Actions That Significantly Affect Energy
Supply, Distribution or Use

This proposed rule is not a ``significant energy action'' as
defined in Executive Order 13211, ``Actions Concerning Regulations that
Significantly Affect Energy Supply, Distribution, or Use'' (66 FR
28355, May 22, 2001) because it is not likely to have a significant
adverse effect on the supply, distribution, or use of energy. The
proposal focuses on maintaining the availability of certain response
tools that can be considered when responding to oil discharges,
minimizing any potential adverse impacts from their use, and resulting
in greater overall environmental protection. Thus, the proposed rule
would not cause reductions in the supply or production of oil, fuel,
coal, or electricity; nor would it result in increased energy prices,
increased cost of energy distribution, or an increased dependence on
foreign supplies of energy.

I. National Technology Transfer and Advancement Act

Section 12(d) of the National Technology Transfer and Advancement
Act of 1995 (``NTTAA''), Public Law 104-113, 12(d) (15 U.S.C. 272 note)
directs EPA to use voluntary consensus standards in its regulatory
activities unless to do so would be inconsistent with applicable law or
otherwise impractical. Voluntary consensus standards are technical
standards (e.g., materials specifications, test methods, sampling
procedures, and business practices) that are developed or adopted by
voluntary consensus standards bodies. NTTAA directs EPA to provide
Congress, through OMB, explanations when the Agency decides not to use
available and applicable voluntary consensus standards.
This rulemaking involves technical standards. The Agency conducted
a search to identify potentially applicable

[[Page 3421]]

voluntary consensus standards for efficacy testing. However, we
identified no such standards. Therefore, EPA developed the Baffled
Flask Efficacy Test and the Bioremediation Efficacy Test required in
Appendix C of this proposed rule. Voluntary consensus standards
developed by ASTM are recommended for several product property data
points, such as pH, flash point and pour point. The product toxicity
testing relies on existing protocols that are universally accepted. EPA
welcomes comments on this aspect of the proposed rulemaking and,
specifically, invites the public to identify potentially-applicable
voluntary consensus standards for product efficacy and to explain why
such standards should be used in this regulation.

J. Executive Order 12898: Environmental Justice

Executive Order 12898, ``Federal Actions to Address Environmental
Justice in Minority Populations and Low-Income Populations'' (59 FR
7629 (February 11, 1994)) establishes federal executive policy on
environmental justice. Its main provision directs federal agencies, to
the greatest extent practicable and permitted by law, to make
environmental justice part of their mission by identifying and
addressing, as appropriate, disproportionately high and adverse human
health or environmental effects of their programs, policies, and
activities on minority populations and low-income populations in the
United States.
EPA is committed to addressing environmental justice concerns and
has assumed a leadership role in environmental justice initiatives to
enhance environmental quality for all citizens of the United States.
The Agency's goals are to ensure that no segment of the population,
regardless of race, color, national origin, income, or net worth bears
disproportionately high and adverse human health and environmental
impacts as a result of EPA's policies, programs, and activities. In
response to Executive Order 12898, EPA's Office of Solid Waste and
Emergency Response (OSWER) formed an Environmental Justice Task Force
to analyze the array of environmental justice issues specific to waste
programs and to develop an overall strategy to identify and address
these issues (OSWER Directive No. 9200.3-17). To address this goal, EPA
conducted a qualitative analysis of the environmental justice issues
under this proposed rule.
Under the NCP, RRTs and ACs are required to address, as part of
their planning activities, the desirability of using appropriate
chemical or biological agents, or other spill mitigating devices. In
addition, the OSC, under authority granted by the NCP, must respond to
an oil spill in a diligent and effective manner to protect human health
and the environment. If chemical or biological agents are needed, the
OSC must coordinate with the RRT and ACs before their use is
authorized. In all cases, the RRT, ACs and OSC will address a broad
array of oil spill response and mitigation issues, including the
potential for environmental justice concerns. Historically, EPA has not
found any evidence that the use of chemical or biological agents on the
Schedule on oil spills in the U.S. has had any disproportionate effect
on any environmental justice communities. However, EPA will continue to
monitor the implementation of the rule to ensure the planned or actual
use of chemical or biological agents has no disproportionate effect on
any EJ communities.
EPA has determined that this proposed rule will not have
disproportionately high and adverse human health or environmental
effects on minority or low-income populations because it increases the
level of environmental protection for all affected populations without
having any disproportionately high and adverse human health or
environmental effects on any population, including any minority or low-
income population. Specifically, the proposed rule provides additional
safeguards before any product can be listed on the Schedule, as well as
allows OSCs and RRTs to request additional information to ensure that
the use of any chemical or biological agent, or any other spill
mitigating substance, in responding to oil discharges is protective of
human health and the environment. This proposed rule is consistent with
EPA's Environmental Justice Strategy and the OSWER Environmental
Justice Action Agenda.

List of Subjects

40 CFR Part 110

Environmental protection, Oil pollution, and Reporting and
recordkeeping requirements.

40 CFR Part 300

Air pollution control, Area contingency planning, Bioremediation,
Chemicals, Dispersants, Environmental protection, Hazardous materials,
Hazardous substances, Intergovernmental relations, Natural resources,
Oil spills, Oil spill mitigating devices, Regional response teams,
Sorbents, and Surface washing agents.

Dated: January 9, 2015.
Gina McCarthy,
Administrator.
For the reasons set out in the preamble, the Environmental
Protection Agency proposes to amend 40 CFR parts 110 and 300 to read as
follows:

PART 110--DISCHARGE OF OIL

0
1. The authority citation for part 110 continues to read as follows:

Authority: 33 U.S.C. 1321(b)(3) and (b)(4) and 1361(a); E.O.
11735, 38 FR 21243, 3 CFR parts 1971-1975 Comp., p. 793.

0
2. Revise Sec. 110.4 and its section heading to read as follows:

Sec. 110.4 Chemical or biological agents.

Addition of any chemical or biological agent, as defined in Sec.
300.5, to oil to be discharged that would circumvent the provisions of
this part is prohibited.

PART 300--NATIONAL OIL AND HAZARDOUS SUBSTANCES POLLUTION
CONTINGENCY PLAN

0
3. The authority citation for part 300 continues to read as follows:

Authority: 33 U.S.C. 1321(c)(2); 42 U.S.C. 9601-9657; E.O.
13626, 77 FR 56749, 3 CFR, 2013 Comp., p. 306; E.O. 12777, 56 FR
54757, 3 CFR, 1991 Comp., p. 351; E.O. 12580, 52 FR 2923, 3 CFR,
1987 Comp., p. 193.

Subpart A--Introduction

0
4. Amend Sec. 300.5 by:
0
a. Adding in alphabetical order the definitions of ``Bioaccumulation'',
``Bioconcentration'', ``Biodegradation'', ``Biological agents'', and
``Bioremediation'';
0
b. Revising the definitions of ``Bioremediation agents'', ``Burning
agents'', ``Chemical agents'', and ``Dispersants'';
0
c. Adding in alphabetical order the definition of ``Herding agents'';
0
d. Removing the definitions for ``Miscellaneous oil spill control
agent'';
0
e. Adding in alphabetical order the definition of ``Products'';
0
f. Revising the definition of ``Sinking agents'';
0
g. Adding in alphabetical order the definition of ``Solidifiers''; and
0
h. Revising the definition of ``Sorbents''
0
i. Removing the definition for ``Surface collecting agents''.
0
j. Revising the definition title ``Surface washing agent'' and its
definition;
The revisions and additions read as follows:

[[Page 3422]]

Sec. 300.5 Definitions.

* * * * *
Bioaccumulation is the process of accumulation of chemicals in the
tissue of organisms through any route, including respiration,
ingestion, or direct contact with the ambient or contaminated medium.
Bioconcentration is the accumulation of chemicals in the tissues of
organisms from water alone.
Biodegradation is a process by which microorganisms metabolically
decompose contaminants into biomass and simpler compounds such as
carbon dioxide, water, and innocuous end products.
Biological agents are microorganisms (typically bacteria, fungi, or
algae) or biological catalysts, such as enzymes, able to enhance the
biodegradation of a contaminated environment.
Bioremediation is the process of enhancing the ability of
microorganisms to convert contaminants into biomass and innocuous end
products by the addition of materials into a contaminated environment
to accelerate the natural biodegradation process.
Bioremediation agents are biological agents and/or nutrient
additives deliberately introduced into a contaminated environment to
increase the rate of biodegradation and mitigate any deleterious
effects caused by the contaminant constituents. Bioremediation agents
include microorganisms, enzymes, and nutrient additives such as
fertilizers containing bioavailable forms of nitrogen, phosphorus and
potassium.
Burning agents are additives that improve the combustibility of the
materials to which they are applied through physical or chemical means.
* * * * *
Chemical agents are elements, compounds, or mixtures designed to
facilitate the removal of oil from a contaminated environment and
mitigate any deleterious effects. Chemical agent categories include
burning agents, dispersants, herding agents, sinking agents,
solidifiers, surface washing agents, and bioremediation agents that
consist of nutrient additives.
* * * * *
Dispersants are typically mixtures of solvents, surfactants, and
additives that promote the formation of small droplets of oil in the
water column by reducing the oil-water interfacial tension.
* * * * *
Herding agents are substances that are used to control the
spreading of the oil across the water surface.
* * * * *
Products are chemical or biological agents manufactured using a
unique composition or formulation.
* * * * *
Sinking agents are substances deliberately introduced into an oil
discharge for the purpose of submerging the oil to the bottom of a
water body.
* * * * *
Solidifiers are substances that through a chemical reaction cause
oil to become a cohesive mass, preventing oil from dissolving or
dispersing into the water column, and which are collected and recovered
from the environment.
Sorbents are inert, insoluble substances that readily absorb and/or
adsorb oil or hazardous substances, and that are not combined with or
act as a chemical or biological agent. Sorbents are generally collected
and recovered from the environment. Sorbents may be used in their
natural bulk form, or as manufactured products in particulate form,
sheets, rolls, pillows, or booms. Sorbents consist of:
(1) Natural organic substances (e.g., feathers, cork, peat moss,
and cellulose fibers such as bagasse, corncobs, and straw);
(2) Inorganic/mineral compounds (e.g., volcanic ash, perlite,
vermiculite, zeolite, clay); and
(3) Synthetic compounds (e.g., polypropylene, polyethylene,
polyurethane, polyester).
* * * * *
Surface washing agents are substances that separate oil from solid
surfaces, such as beaches, rocks, metals, or concrete, through a
detergency mechanism that lifts and floats oil for collection and
recovery from the environment with minimal dissolution, dispersion, or
transfer of oil into the water column.
* * * * *

Subpart J--Use of Dispersants, and Other Chemical and Biological
Agents

0
5. Revise the heading of Subpart J as set out above.
0
6. Amend Sec. 300.900 by revising paragraphs (a) and (c), and by
adding paragraph (d) to read as follows:

Sec. 300.900 General.

(a) Section 311(d)(2)(G) of the Clean Water Act (CWA) requires EPA
to prepare a schedule identifying dispersants, other chemicals, other
spill mitigating devices and substances if any, that may be used in
carrying out the NCP; and the waters and quantities in which they may
be used. This subpart establishes a schedule identifying chemical and
biological agents, and procedures that, when taken together, identify
the waters and quantities in which such dispersants, other chemicals,
or other spill mitigating devices and substances may be used.
* * * * *
(c) This subpart applies to the use of chemical and biological
agents as defined in Subpart A of this part, or other substances that
may be used to remove, control, or otherwise mitigate oil discharges.
(d) [Reserved]

Sec. 300.905 [Removed]

0
7. Remove Sec. 300.905.
0
8. Revise Sec. 300.910 and the section heading to read as follows:

Sec. 300.910 Authorization for agent use.

Use of chemical or biological agents in response to oil discharges
to waters of the U.S. or adjoining shorelines must be authorized by the
OSC in accordance with the provisions of this section:
(a) Use of Agents Identified on the Schedule on Oil Discharges
Addressed by a Preauthorization Plan. RRTs and Area Committees shall
address in a preauthorization plan, as part of their planning
activities, whether the use of chemical and biological agents listed on
the Schedule on certain oil discharges is appropriate. RRTs and Area
Committees shall, as appropriate, include applicable approved
preauthorization plans in RCPs and ACPs. When a preauthorization plan
is approved in advance for the use of certain agents under specified
discharge situations, then the OSC may authorize the use of agents on
the Schedule for their intended purpose without obtaining the incident
specific concurrences described in paragraph (b) of this section.
(1) Preauthorization Plan Development. For discharge situations
identified where such agents may be used, the preauthorization plan
must specify limits for the quantities and the duration of use, and use
parameters for water depth, distance to shoreline, and proximity to
populated areas. In meeting the provisions of this paragraph,
preauthorization plans should document how regional factors are
addressed including likely sources and types of oil that might be
discharged, various discharge scenarios, the existence and location of
environmentally sensitive resources or restricted areas that might be
impacted by discharged oil, and logistical factors including inventory,
storage locations and manufacturing capability of available agents,
availability of equipment needed for agent use, availability of
adequately trained

[[Page 3423]]

operators, and means to monitor agent use in the environment.
(2) Preauthorization Plan Approval. The EPA representative to the
RRT, the Department of Commerce and the Department of the Interior
natural resource trustees and, as appropriate the RRT representative
from the state(s) with jurisdiction over waters and adjoining
shorelines within the preauthorization plan area shall review and
either approve, approve with modification, or disapprove the
preauthorization plans developed by the RRT and/or the Area Committees.
Withdrawal of concurrence means the preauthorization plan becomes
invalid and the authorization of use for chemical or biological agents
must be performed according to paragraph (b) of this section. The RRTs
and Area Committees shall address the withdrawal and the RRT shall
notify the NRT of the final status of the preauthorization plan within
30 days from withdrawal.
(3) Preauthorization Plans Reviews. The RRT and/or the Area
Committees must review, and revise as needed, preauthorization plans at
least every 5 years; after a major discharge or after a Spill of
National Significance (SONS); to address revisions of the Schedule; to
reflect new listings of threatened and/or endangered species; and to
address any other change that may impact the conditions under which the
use of chemical and biological agents is preauthorized. The designated
EPA RRT representative, the Department of Commerce and the Department
of the Interior natural resource trustees, and the RRT representative
from the state(s) with jurisdiction over the waters of the area to
which a preauthorization plan applies shall review and either approve,
approve with modification, or disapprove any revisions to the
preauthorization plans.
(b) Use of Agents Identified on the Schedule on Oil Discharges Not
Addressed by a Preauthorization Plan. For discharge situations that are
not addressed by the preauthorization plan developed pursuant to
paragraph (a) of this section, the OSC may authorize the use of
appropriate chemical or biological agents identified on the Schedule
for their intended purpose on an oil discharge with the concurrence of
the designated EPA RRT representative and, as appropriate, the
concurrence of the RRT representatives from the state(s) with
jurisdiction over the waters and adjoining shorelines threatened by the
release or discharge, and in consultation with the Department of
Commerce and the Department of the Interior natural resource trustees.
In meeting the provisions of this paragraph, the OSC must consider and
document the parameters for the use of agents including the quantities
to be used, the duration of use, the depth of water, the distance to
shoreline and proximity to populated areas, and should address factors
such as environmentally sensitive resources or restricted areas that
might be impacted, agent inventory and storage locations, agent
manufacturing capability, availability of equipment needed for agent
use, availability of adequately trained operators and appropriate means
to monitor agent use in the environment.
(c) Burning Agents. For authorized in-situ burns, the OSC may
authorize the use of burning agents.
(d) Exception. The OSC may authorize the use of any chemical or
biological agent, whether it is identified or not on the Schedule,
without obtaining the immediate concurrence of the designated EPA RRT
representative and, as appropriate, the RRT representatives from the
state(s) with jurisdiction over the waters and adjoining shorelines
threatened by the release or discharge, when, in the judgment of the
OSC, the use of the agent is necessary to prevent or substantially
reduce a threat to human life. If an OSC authorizes the use of an agent
pursuant to this paragraph, he or she shall immediately notify, and
document the circumstances requiring and the reasons for use of the
agent to the EPA RRT representative and, as appropriate, the RRT
representatives from the affected state(s) and, the Department of
Commerce/Department of the Interior natural resources trustees. Use of
any agent beyond 48 hours under this exception shall be in accordance
with paragraphs (a) or (b) of this section.
(e) Prohibited Agents. Notwithstanding paragraph (d) of this
section, the OSC may not authorize the use of the following:
(1) Sinking agents, or any other chemical agent, biological agent,
or any substance that acts as a sinking agent when mixed with oil; and
(2) Chemical or biological agents that have either nonylphenol (NP)
or nonylphenol ethoxylates (NPEs) as components.
(f) Storage and Use of Agents. The OSC may authorize for use only
products that are certified by the responsible party to have been
stored under the conditions provided by the submitter under Sec.
300.915(a)(6) and whose date of use does not exceed the expiration date
listed on the container's label at the time of the incident. The
responsible party must provide the OSC product documentation, developed
in consultation with the submitter of the product to the Schedule,
prior to OSC authorization of product use affirming it has maintained
its integrity, including no changes in its composition, efficacy, and
toxicity. The owner or operator of a facility or vessel must ensure
samples of the expired product lot are tested following the applicable
testing protocols in Appendix C, and that they are representative of
all storage conditions at any end user location. If testing
demonstrates the expired product has maintained its integrity, the
product may be used for an additional 5 years from the date of the
testing described above. The responsible party, or its representative,
must re-label the tested product lots and maintain test results and
document all of the information under Sec. 300.915(a)(17) and (a)(18)
until used. The owner or operator of a facility or vessel must ensure
the testing of re-labeled products every 5 years.
(g) Supplemental Testing, Monitoring and Information. The RRT may
require supplementary toxicity and efficacy testing, or available data
or information that addresses site, area, or ecosystem specific
concerns relative to the use of a product for both planning and
authorization of use. During a discharge incident, the RRT may request
that the OSC require a responsible party to conduct additional
monitoring associated with the use of a product. Such additional
monitoring data may include supplemental toxicity and efficacy testing
or submission of available data or information that addresses the
discharge area or ecosystem specific concerns relative to the use of a
product or that aids the OSC and/or the RRT in operational decisions.
(h) Recovery of Agents from the Environment. Depending on factors
such as the safety of response personnel and harm to the environment,
and as directed by the OSC, the responsible party shall ensure that any
removal action adequately contains, collects, stores and disposes of
agents that are intended to be recovered from the environment.
(i) Reporting of Agent Use. Unless already included in the OSC
report required under Sec. 300.165 of this part, within 30 days of
completion of agent operations, the authorizing OSC shall provide the
RRT the following information on chemical and biological agents used in
response to an oil discharge: product name, quantity and concentration
used, duration of use, locations, and any data collected and analysis
of efficacy or environmental effects.
0
9. Add Sec. 300.913 to read as follows:

[[Page 3424]]

Sec. 300.913 Monitoring the use of dispersants.

As directed by the OSC, the responsible party must monitor any
subsurface use of dispersant in response to an oil discharge, surface
use of dispersant in response to oil discharges of more than 100,000
U.S. gallons occurring within 24 hours, and surface use of dispersant
for more than 96 hours in response to an oil discharge, and submit a
Quality Assurance Project Plan for approval to the OSC covering the
collection of all environmental data. When these dispersant use
conditions are met, and for the duration of dispersant operations, the
responsible party shall:
(a) Document the characteristics of the source oil; best estimate
of the oil discharge flow rate, periodically reevaluated as conditions
dictate, including a description of the method, associated
uncertainties, and materials; dispersant(s) product used, rationale for
dispersant product choice(s) including the results of any efficacy and
toxicity tests specific to area or site conditions, recommended
dispersant-to-oil ratio (DOR); and the application method and
procedures, including a description of the equipment to be used, hourly
application rates, capacities, and total amount of dispersant needed.
For subsurface discharges also document the best estimate of the
discharge flow rate of any associated volatile petroleum hydrocarbons,
periodically reevaluated as conditions dictate, including a description
of the method, associated uncertainties, and materials.
(b) In areas not affected by the discharge of oil, collect a
representative set of background water column samples following
standard operating and quality assurance procedures, at the closest
safe distance from the discharge as determined by the OSC and in any
direction of likely transport considering surface and subsurface
currents and oil properties for the variables listed below. In the
dispersed oil plume, collect daily water column samples following
standard operating and quality assurance procedures, at such depths and
locations where dispersed oil is likely to be present and analyze for:
(1) In-situ oil droplet size distribution, including mass or volume
mean diameter for droplet sizes ranging from 2.5 to 2,000 [mu]m, with
the majority of data collected between the 2.5 and 100 [mu]m size;
(2) In-situ fluorometry and fluorescence signatures targeted to the
type of oil discharged and referenced against the source oil;
(3) Dissolved oxygen (DO);
(4) Total petroleum hydrocarbons, individual resolvable
constituents including volatile organic compounds, aliphatic
hydrocarbons, monocyclic, polycyclic, and other aromatic hydrocarbons
including alkylated homologs, and hopane and sterane biomarker
compounds;
(5) Carbon dioxide (CO2) (subsurface only);
(6) Methane, if present (subsurface only);
(7) Heavy metals, including nickel and vanadium;
(8) Turbidity;
(9) Water temperature;
(10) pH; and
(11) Conductivity.
(c) In consultation with the OSC, and using best available
technologies, characterize the dispersant effectiveness and oil
distribution, considering the condition of oil, dispersant, and
dispersed oil components from the discharge location;
(d) In consultation with the OSC, characterize the ecological
receptors (e.g. aquatic species, wildlife, and/or other biological
resources) and their habitats that may be present in the discharge area
and their exposure pathways. Include those species that may be in
sensitive life stages, transient or migratory species, breeding or
breeding-related activities (e.g., embryo and larvae development), and
threatened and/or endangered species that may be exposed to the oil
that is not dispersed, the dispersed oil, and the dispersant alone.
Estimate an acute toxicity level of concern for the dispersed oil using
available dose/response information relevant to potentially exposed
species.
(e) Immediately report to the OSC any:
(1) Deviation of more than 10 percent from the mean hourly
dispersant use rate for subsurface application, based on the dispersant
volume authorized for 24 hours use, and the reason for the deviation;
and
(2) Ecological receptors, including any threatened or endangered
species that may be exposed based on dispersed plume trajectory
modeling and level of concern information.
(f) Report daily to the OSC water sampling and data analyses
collected in Sec. 300.913(b) and include:
(1) Specific hourly dispersant application rate and the total
amount of dispersant used for the previous reporting period established
by the OSC with concurrence from the EPA representative to the RRT;
(2) All collected data and analyses of those data within a
timeframe necessary to make operational decisions (e.g., within 24
hours of collection), including documented observations, photographs,
video, and any other information related to dispersant use, unless an
alternate timeframe is authorized by the OSC;
(3) For analyses that take more than 24 hours due to analytical
methods, provide such data and results within 5 days, unless an
alternate timeframe is authorized by the OSC; and
(4) Estimates of the daily transport of dispersed and non-dispersed
oil and associated volatile petroleum hydrocarbons, and dispersants,
using the best available trajectory modeling.
0
10. Revise Sec. 300.915 and the section heading to read as follows:

Sec. 300.915 Data and information requirements for Product Schedule
listing.

If you are submitting an application for listing a product to the
Schedule, you must provide EPA the information required under Sec.
300.955. Your submission must contain:
(a) General Information for any Product Category. (1) Your name,
physical address, email, and telephone number;
(2) Your identity as the manufacturer of the product, a vendor,
importer, or distributor of the product, and/or a designated agent
acting on behalf of the manufacturer. Provide documentation of such
identity;
(3) All name(s), brand(s), and/or trademark(s) under which the
product is to be sold;
(4) Names, physical addresses, emails and telephone numbers of the
primary distributors, vendors, importers, and/or designated agent
acting on behalf of the manufacturer;
(5) A Safety Data Sheet (SDS) for the product;
(6) The maximum, minimum and optimum temperature, humidity and
other relevant conditions for product storage and a brief description
of the consequences to performance if the product is not stored within
these limits;
(7) The anticipated shelf life of the product at the storage
conditions noted in paragraph (a)(6) of this section and documentation
for this determination;
(8) A sample product label for all name(s), brand(s), and/or
trademark(s) under which the product is to be sold that includes
manufacture and expiration dates, and conditions for storage. You may
use an existing label provided it already contains the required dates
and storage information;
(9) The chemical or biological agent category under which you want
the product to be considered for listing on the Schedule, including
detailed information on the specific process(es)

[[Page 3425]]

through which the product affects the oil, and the specific
environment(s) (waters and/or adjoining shorelines) on which it is
intended to be used. If your product meets the definition of more than
one chemical or biological agent category and you want it considered
for listing on the Schedule in more than one category, you must
identify all applicable categories and provide the test data to meet
the listing criteria appropriate to each category;
(10) Recommended product use procedures, including product
concentrations, use ratios, types of application equipment, conditions
for use, and any application restrictions. These procedures must
address, as appropriate, variables such as weather, water salinity,
water temperature, types and weathering states of oils or other
pollutants, and product and oil containment, collection, recovery and
disposal, and include supporting documentation and standard methods
used to determine them;
(11) Environmental fate information, including any known measured
data and supporting documentation, on the persistence, bioconcentration
factor, bioaccumulation factor, and biodegradability of the product and
all of its components in the environment;
(12) The physical/chemical properties of the product, as
appropriate, and a citation for the standard methods used to determine
them, including:
(i) Physical state and appearance;
(ii) Vapor pressure;
(iii) Flash point;
(iv) Pour point;
(v) Viscosity;
(vi) Specific gravity;
(vii) Particle size for solid components; and
(viii) pH.
(13) The identity and concentration of all components in the
product, including each specific component name; corresponding Chemical
Abstract Service (CAS) Registry Number; the maximum, minimum, and
average weight percent of each component in the product; and the
intended function of each component (e.g., solvent, surfactant);
(14) For products that contain microorganisms, enzymes and/or
nutrients, provide the following along with a citation or a description
of the methodology used to determine:
(i) The name of all microorganisms by current genus and species,
including any reclassifications, and any physical, chemical, or
biological technique used to manipulate the genetic composition and the
weight percent of each genus in the product;
(ii) The name of all enzymes and their International Union of
Biochemistry (I.U.B.) number(s); Enzyme Classification (EC) code
numbers; the source of each enzyme; units; and specific oil-degrading
activity;
(iii) The name(s), maximum, minimum, and average weight percent of
the nutrients contained in the product; and
(iv) Certification, including data, methodology, and supporting
documentation, indicating that the product does not contain, at levels
that exceed the National Ambient Water Quality Criteria lowest density
value, bacterial, fungal, or viral pathogens or opportunistic pathogens
including, but not limited to: enteric bacteria such as Salmonella,
fecal coliforms, Shigella, or Coagulase positive Staphylococci, and
Beta Hemolytic Streptococci and enterococci.
(15) Certification, including data, methodology, and supporting
documentation, indicating that the product does not contain, at levels
above National Water Quality Standards lowest acute value for aquatic
life:
(i) Arsenic, cadmium, chromium, copper, lead, mercury, nickel,
vanadium, zinc, and any other heavy metal reasonably expected to be in
the product;
(ii) Cyanide;
(iii) Chlorinated hydrocarbons;
(iv) Pesticides;
(v) Polychlorinated Biphenyls (PCBs); and
(vi) Polynuclear aromatic hydrocarbons (PAHs).
(16) Certification, including data, methodology, and supporting
documentation, indicating that the product does not contain any of the
prohibited agents identified in Sec. 300.910(e);
(17) Information about the laboratory that conducted the required
tests, including:
(i) Name of the laboratory, address, contact name, email, and phone
number; and
(ii) The national and/or international accreditations held by the
laboratory.
(18) All test data and calculations, including:
(i) Raw data and replicates, including positive controls;
(ii) Notes and observations collected during tests;
(iii) Calculated mean values and standard deviations;
(iv) Reports, including a summary of stock solution preparation;
(v) Source and preparation of test organisms;
(vi) Test conditions; and
(vii) Chain of custody forms.
(19) An estimate of the annual product production volume, the
average and maximum amount that could be produced per day, and the time
frame needed to reach that maximum production rate (days);
(20) Recognition received from EPA's Design for the Environment
(DfE) if applicable; and
(21) International product testing or use data or certifications,
if available, informing the performance capabilities or environmental
benefits of the product.
(b) Dispersant Testing and Listing Requirements--(1) Dispersant
Efficacy test and listing criteria. Test the dispersant product for
efficacy using the Baffled Flask Test (BFT) method in Appendix C to
part 300. To be listed on the Schedule, the dispersant must demonstrate
for each oil and temperature a Dispersant Effectiveness (DE) at the 95%
lower confidence level (LCL95) greater than or equal to:
(i) 55% for Intermediate Fuel Oil 120 (IFO-120) at 5 [deg]C;
(ii) 65% for IFO-120 at 25 [deg]C;
(iii) 70% for Alaska North Slope (ANS) crude oil at 5 [deg]C; and
(iv) 75% for ANS at 25 [deg]C.
(2) Dispersant Toxicity tests and listing criteria. Use the methods
specified in Appendix C to part 300 to test the dispersant alone, the
dispersant mixed with ANS, and the dispersant mixed with IFO-120 for
acute toxicity, using Americamysis bahia and Menidia beryllina. Use the
methods specified in Appendix C to part 300 to test the dispersant
alone for developmental toxicity using a sea urchin assay and for sub-
chronic effects using Americamysis bahia and Menidia beryllina. To be
listed on the Schedule, the lethal concentration for 50% of the test
species (LC50) at the lower 95% confidence interval for all
acute toxicity tests must be greater than 10 ppm; the inhibition
concentration for 50% of the test species (IC50) at the
lower 95% confidence interval must be greater than 10 ppm; and the sub-
chronic No Observed Effect Concentration (NOEC) must be equal to or
greater than 1 ppm.
(3) Limitations. Product listing would be for use only in saltwater
environments.
(c) Surface Washing Agent Testing and Listing Requirements--
(1) Surface Washing Agent Efficacy test and listing criteria. To be
listed on the Schedule, using a recognized standard methodology, the
surface washing agent must meet an efficacy of greater than or equal to
30% in either fresh or saltwater or both depending on the intended
product use.

[[Page 3426]]

(2) Surface Washing Agent Toxicity test and listing criteria. Using
the toxicity test methodology in Appendix C to part 300, test the
surface washing agent for acute toxicity against fresh water species
Ceriodaphnia dubia and Pimephales promelas, or saltwater species
Americamysis bahia and Menidia beryllina, or both, depending on the
intended product use. To be listed on the Schedule, the surface washing
agent must demonstrate an LC50 at the lower 95% confidence
interval of greater than 10 ppm in either fresh or saltwater for all
tested species.
(3) Limitations. Based on testing, product listing would be for use
only in the fresh and/or saltwater environments for which it was tested
and for which it met the efficacy and toxicity listing criteria.
(d) Bioremediation Agent Testing and Listing Requirements--(1)
Bioremediation Agent Efficacy test and listing criteria. To be listed
on the Schedule, a bioremediation agent must successfully degrade both
alkanes and aromatics as determined by gas chromatography/mass
spectrometry (GC/MS) in salt or fresh water or both, depending on the
intended product use, following the test method specified in Appendix C
to part 300. The percentage reduction of total alkanes (aliphatic
fraction) from the GC/MS analysis must be greater than or equal to 95%
at day 28, based on the ninety-fifth percentile Upper Confidence Limit
(UCL95) for both salt and freshwater. The percentage
reduction of total aromatics (aromatic fraction) must be greater than
or equal to 70% at day 28 for saltwater and greater than or equal to
40% for freshwater based on the UCL95.
(2) Bioremediation Agent Toxicity test and listing criteria. The
bioremediation agent must be tested for acute toxicity in saltwater,
freshwater or both, depending on the intended product use, following
the method specified in Appendix C to part 300. To be listed on the
Schedule, the bioremediation agent must demonstrate an LC50
at the lower 95% confidence interval of greater than 10 ppm in either
fresh or saltwater for all tested species.
(3) Limitations. Based on testing, product listing would be for use
only in the fresh and/or saltwater environments for which it was tested
and for which it met the efficacy and toxicity listing criteria.
(4) Exceptions. If the product consists solely of: ammonium
nitrate, ammonium phosphate, ammonium sulfate, calcium ammonium
nitrate, sodium nitrate, potassium nitrate, synthetically-derived urea,
sodium triphosphate (or tripolyphosphate), sodium phosphate, potassium
phosphate (mono- or dibasic), triple super phosphate, potassium
sulphate, or any combination thereof, no technical product data are
required, are generically listed as non-proprietary nutrients on the
Schedule, and no further action is necessary.
(e) Solidifier Testing and Listing Requirements. (1) Solidifiers
must be tested for acute toxicity in saltwater, freshwater or both,
depending on the intended product use, following the method specified
in Appendix C to part 300. To be listed on the Schedule, the solidifier
must demonstrate an LC50 at the lower 95% confidence
interval of greater than 10 ppm in either fresh or saltwater for all
tested species.
(2) Limitations. Based on testing, product listing would be for use
only in the fresh and/or saltwater environments for which it was tested
and for which it met the toxicity listing criteria.
(f) Herding Agent Testing and Listing Requirements. (1) Herding
agents must be tested for acute toxicity in saltwater, freshwater, or
both, depending on the intended product use, following the method
specified in Appendix C to part 300. The herding agent must demonstrate
an LC50 at the lower 95% confidence interval of greater than
10 ppm in either fresh or saltwater for all tested species.
(2) Limitations. Based on testing, product listing would be for use
only in fresh and/or saltwater environments for which it was tested and
for which it met the toxicity listing criteria.
(g) Sorbent Requirements. Known sorbent materials and products will
be identified on a publicly available Sorbent Product List for the use
of such products when responding to an oil discharge as follows:
(1) For sorbent products that consist solely of the following
materials, or any combination thereof, no technical data are required
and no further action is necessary for use as a sorbent:
(i) Feathers, cork, peat moss, and cellulose fibers such as
bagasse, corncobs, and straw;
(ii) Volcanic ash, perlite, vermiculite, zeolite, and clay; and
(iii) Polypropylene, polyethylene, polyurethane, and polyester.
(2) If the product consists of one or more natural organic
substances, inorganic/mineral compounds, and/or synthetic compounds not
specifically identified in paragraph (g)(1) of this section but you
believe the product meets the definition of a sorbent then, as
applicable under Sec. 300.955(a) and (b), you must submit the
following information for consideration for listing it as a sorbent on
the Sorbent Product List:
(i) The information required under paragraphs (a)(1) through (8),
and paragraph (a)(13) of this section;
(ii) The certifications required under paragraphs (a)(14)(iv),
(a)(15), and (a)(16) of this section; and
(iii) Information, including data, to support the claim your
product meets the sorbent definition under Sec. 300.5.

Sec. 300.920 [Removed]

0
11. Remove Sec. 300.920.
0
12. Add Sec. 300.950 to subpart J to read as follows:

Sec. 300.950 Submission of Confidential Business Information (CBI).

(a) Except as provided in paragraph (b) of this section, all
product information submitted to EPA as required under Sec. 300.915
will be disclosed to the public.
(b) You may only claim the concentration and the maximum, minimum,
and average weight percent of each chemical component or microorganism
in your product, as identified in Sec. 300.915(a)(13) or (14), to be
CBI. EPA will handle such claims in accordance with 40 CFR part 2,
subpart B.
(1) You must make your CBI claim at the time you submit your
information to EPA to be listed on the Schedule.
(2) You must redact the CBI from all submitted information but
include the CBI separately with your submission package. Clearly
identify and mark the information as ``Confidential Business
Information'' and place it in a separate inner envelope in your
submission package labeled with ``CONFIDENTIAL BUSINESS INFORMATION--TO
BE OPENED BY THE PRODUCT SCHEDULE MANAGER ONLY.''
0
13. Add Sec. 300.955 to subpart J to read as follows:

Sec. 300.955 Addition of a product to the Schedule.

(a) Submission. Submit your complete package to: U.S. Environmental
Protection Agency, 1200 Pennsylvania Ave. NW., Mail Code: 5104A, Room
1448, William J. Clinton North, Washington, DC 20460, Attention:
Product Schedule Manager.
(b) Package contents. Your package shall include, in this order:
(1) A cover letter on company letterhead signed and dated by you
certifying that:
(i) All testing was conducted on representative product samples;
(ii) Testing was conducted at a nationally or internationally
accredited laboratory in accordance with the

[[Page 3427]]

methods specified in Appendix C to part 300, and other applicable
methods as appropriate; and
(iii) All test results and product technical data and information
are true and accurate.
(2) A numbered Table of Contents showing the information and data
submitted under Sec. 300.915(a) through (g);
(3) All required data and information arranged in the same order as
specified in Sec. 300.915(a) through (g); and
(4) A separate envelope containing Confidential Business
Information as specified in Sec. 300.950(b), if applicable.
(c) EPA Review. EPA shall, within 90 days of receiving a submission
package:
(1) Review the package for completeness and compliance with all
data and information requirements in Sec. Sec. 300.915, 300.950, and
this section, verify information, and request clarification or
additional information as necessary;
(2) Make a product listing determination based on a technical
evaluation of all data and information submitted, relevant information
on impacts or potential impacts of the product or any of its components
on human health or the environment, and the intended use of the
product. EPA reserves the right to make a determination on whether the
product will be listed, and under which category; and
(3) Notify you, in writing, of its decision to list the product on
the Schedule and in which category or categories, or of its decision
and supporting rationale to reject the submission. If your submission
is rejected:
(i) You may revise the submission package to address test results,
data, or information deficiencies and resubmit it.
(ii) EPA's 90-day review will not start until a complete package is
resubmitted.
(d) Request for review of decision. If your product is rejected for
listing on the Schedule, you may request that the EPA Administrator
review the determination. Your request must be in writing within 30
days of receipt of notification of EPA's decision not to list the
product on the Schedule. Your request must contain a clear and concise
statement with supporting facts and technical analysis demonstrating
why you believe EPA's decision was incorrect.
(1) The EPA Administrator or designee may request additional
information from you and may offer an opportunity for you to meet with
EPA.
(2) The EPA Administrator or his designee will notify you in
writing of the decision within 60 days of receipt of your request, or
within 60 days of receipt of requested additional information.
(e) Changes to a product listing. You must notify EPA in writing
within 30 days of any changes to information submitted under Sec.
300.915(a)(1) through (8) and Sec. 300.915(a)(19) through (21) for a
product on the Schedule. In the notification, you must detail the
specific changes, the reasons for such changes and supporting data and
information. EPA may request additional information and clarification
regarding these changes. If you change the chemical components and/or
concentrations, you must retest the reformulated product according to
the requirements for the product category and submit a complete new
package for a review and consideration for listing on the Schedule by
EPA.
(f) Transitioning Listed Products from the Current Schedule to the
New Schedule. All products on the current Schedule as of [EFFECTIVE
DATE OF FINAL RULE] will remain conditionally listed until [DATE 24
MONTHS FROM THE EFFECTIVE DATE OF FINAL RULE] at which time all
products that have not submitted and been listed in the new Schedule
based on the amended test and listing criteria will be removed. Your
product will be transitioned from the current Schedule to the new
Schedule prior to [DATE 24 MONTHS FROM THE EFFECTIVE DATE OF FINAL
RULE] after you submit a new, complete package according to the amended
test and listing criteria and EPA makes a favorable finding to list the
product on the new Schedule.
0
14. Add Sec. 300.965 to subpart J to read as follows:

Sec. 300.965 Mandatory product disclaimer.

The listing of a product on the Schedule does not constitute
approval or recommendation of the product. To avoid possible
misinterpretation or misrepresentation, any label, advertisement, or
technical literature for the product must display in its entirety the
disclaimer shown below. The disclaimer must be conspicuous and must be
fully reproduced on all product literatures, labels, and electronic
media including Web site pages.
DISCLAIMER [PRODUCT NAME] is listed on the National Contingency
Plan (NCP) Product Schedule. This listing does NOT mean that EPA
approves, recommends, licenses, or certifies the use of [PRODUCT NAME]
on an oil discharge. This listing means only that data have been
submitted to EPA as required by Subpart J of the NCP. Only a Federal
On-Scene Coordinator (OSC) may authorize use of this product according
to the NCP.
0
15. Add Sec. 300.970 to subpart J to read as follows:

Sec. 300.970 Removal of a product from the Schedule.

(a) The EPA Administrator may remove your product from the Schedule
for reasons including, but not limited to:
(1) Misleading, inaccurate, or incorrect statements within the
product submission to EPA or to any person or private or public entity
regarding the composition or use of the product to remove or control
oil discharges, including on labels, advertisements, or technical
literature; or
(2) Alterations to the chemical components, concentrations, or use
conditions of the product without proper notification to EPA as
required by Sec. 300.955(e); or
(3) Failure to print the disclaimer provided in Sec. 300.965 on
all labels, advertisements, or technical literature, or
(4) New or previously unknown relevant information concerning the
impacts or potential impacts of the product to human health or the
environment.
(b) EPA will notify you in writing, at your address of record, of
its reasons for deciding to remove the product from the Schedule. If
EPA receives no appeal from you in 30 days, the product will be removed
from the Schedule without further notice to you.
(c) You may appeal the decision to remove your product from the
Schedule within 30 days of receipt of EPA's notification. Your appeal
must contain a clear and concise statement with supporting facts and
technical analysis demonstrating why you believe EPA's decision was
incorrect. The EPA Administrator will notify you in writing of his
decision within 60 days of your appeal, or within 60 days of receipt of
any requested additional information.
0
16. Revise Appendix C to Part 300 and appendix heading to read as
follows:

Appendix C to Part 300--Requirements for Product Testing Protocols and
Summary Test Data: Dispersant Baffled Flask Efficacy and Toxicity
Tests; Standard Acute Toxicity Test for Bioremediation Agents, Surface
Washing Agents, Herding Agents, and Solidifiers; and Bioremediation
Agent Efficacy Test.

Table of Contents

1.0 Applicability and Scope
2.0 Baffled Flask Dispersant Efficacy Test (BFT)
3.0 Dispersant Toxicity Testing

[[Page 3428]]

4.0 Standard Acute Toxicity Testing for Surface Washing Agents,
Bioremediation Agents, Herding Agents, and Solidifiers.
5.0 Bioremediation Agent Efficacy Test Protocol

Illustrations

Figure Number

1. A Baffled Trypsinizing Flask

Tables

Table Number

1. Constituent Concentrations for GP2 Artificial Seawater
2. Test Oil Characteristics
3. Stock Solution Preparation
4. Dispersant Calibration Example for Both Oils
5. Sample Calculation with ANS
6. Toxicity Testing Requirements for Dispersants
7. Summary of Test Conditions--Dispersant Toxicity
8. Toxicity Testing Requirements for Surface Washing Agents, Herding
Agents, Bioremediation Agents and Solidifiers
9. Summary of Test Conditions--Surface Washing Agents, Herding
Agents, Bioremediation Agents and Solidifiers Toxicity
10. Artificial Seawater Nutrient Concentrations
11. Artificial Seawater Nutrient Concentrations for Bioremediation
Agents Having No Nutrients Included
12. Constituent Concentrations for Artificial Freshwater (Bushnell-
Haas)
13. Freshwater Nutrient Concentrations
14. Artificial Freshwater Nutrient Concentration for Bioremediation
Agents Having No Nutrients Included
15. Bioremediation Efficacy Test--Summary of Experimental Setup
16. Bioremediation Efficacy--Summary of Analytical Procedures
17. QA/QC Checks

Standard Operating Procedures Tables

SOP 3-1 Amount of Stock Solutions Required to Make the Working
Standards
SOP 4-1 Ions Associated With Retention Time Groups
SOP 4-2 Instrumental Conditions for Crude Oil Analysis
SOP 4-3 Ion Abundance Criteria for DFTPP
SOP 4-4 Target Compound List
1.0 Applicability and Scope. This Appendix establishes
laboratory protocols required under Subpart J (Use of Dispersants
and Other Chemical and Biological Agents) of 40 CFR part 300
(National Oil and Hazardous Substances Pollution Contingency Plan)
to make listing determinations for the Product Schedule. The
protocols apply, based on product type, to dispersants,
bioremediation agents, surface washing agents, herding agents, and
solidifiers as defined in Subpart A (Introduction) of 40 CFR part
300.

2.0 Baffled Flask Dispersant Efficacy Test (BFT)

2.1 Summary. This laboratory protocol establishes procedures to
evaluate the degree to which a product effectively disperses oil
spilled on the surface of seawater, using a modified 150-mL screw-
cap trypsinizing flask (an Erlenmeyer flask with baffles) with a
glass and Teflon[supreg] stopcock near the bottom to allow removal
of subsurface water samples without disturbing the surface oil
layer. The efficacy of a dispersant is measured using two types of
oils (Intermediate Fuel Oil 120 and Alaska North Slope) at two
temperatures (5 [deg]C and 25 [deg]C). Six replicates are required
at each condition with two method blank replicates at each
temperature. A layer of oil is placed on the surface of artificial
seawater, and the dispersant is added to the slick at a
dispersant:oil ratio (DOR) of 1:25 (4%) by volume. A standard
orbital shaker table provides turbulent mixing at a speed of 250
revolutions per minute (rpm) for 10 minutes, immediately after which
it is maintained stationary for 10 minutes to allow non-dispersed
oil to rise to the water's surface. An undisturbed water sample is
removed from the bottom of the flask through the stopcock, extracted
with dichloromethane (DCM), and analyzed for oil content by UV-
visible absorption spectrophotometry at wavelengths ranging between
340 and 400 nm.
2.2 Apparatus. All equipment must be maintained and calibrated
per standard laboratory procedures.
2.2.1 Modified Trypsinizing Flask. A modified 150 mL glass
screw-capped Erlenmeyer flask with baffles (e.g., Wheaton No. 355394
or equivalent) fitted with a 2 mm bore Teflon[supreg] stopcock and
glass tubing, the center of which is no more than 1.3 cm from the
bottom, as shown in Figure 1.
[GRAPHIC] [TIFF OMITTED] TP22JA15.038

[[Page 3429]]

2.2.2 Orbital Shaker Table. An orbital shaker table with a
variable speed control unit capable of maintaining 250 rpm. The
orbital diameter must be approximately 1.0 inch (2.5 cm) +/- 0.1
inch (0.25 cm).
2.2.3 Spectrophotometer. A UV-visible spectrophotometer capable
of measuring absorbance between 340 and 400 nm (e.g., Shimadzu UV-
1800, Agilent 8453, or equivalent). Use standard transmission-
matched quartz 10-mm path length rectangular cells with PTFE cover
for absorbance measurements.
2.2.4 Glassware. Including: 25-ml graduated mixing cylinders (a
graduated cylinder with a ground glass stopper); 50- and 100-ml
graduated cylinders; 125-mL separatory funnels with Teflon
stopcocks; 10 ml volumetric flasks; 30 ml crimp style glass serum
bottles; 1-, 2-, 5-mL pipettes; other miscellaneous laboratory
items.
2.2.5 Micropipettor. Use a micropipettor capable of dispensing 4
[micro]L of dispersant and 100 [micro]L of oil (e.g., Brinkmann
Eppendorf repeater pipettor with 100 [micro]L and 5 mL syringe tip
attachments or equivalent).
2.2.6 Syringes. 25-, 100-, 250-, 1000-, 2500-, 5000- [micro]l
gas-tight syringes.
2.2.7 Constant temperature rooms or incubators to hold the
shaker at 5 [deg]C and 25 [deg]C.
2.2.8 Analytical Balance.
2.2.9 Chemical fume hood.

2.3 Reagents

2.3.1 Artificial seawater. Use the artificial seawater GP2
formulation shown in Table 1 of this Appendix.
2.3.2 Test oils. Use the two EPA standard reference oils, Alaska
North Slope oil (ANS) and Intermediate Fuel Oil 120 (IFO 120). To
obtain these oils at no charge (except for a minimal shipping fee),
see the instructions at http://www.epa.gov/emergencies/content/ncp/index.htm. Selected properties are summarized in Table 2 of this
Appendix.
2.3.3 Dichloromethane (DCM) (also known as methylene chloride),
pesticide quality.
2.3.4 Positive Control Dispersant. Dispersant sample with a
known, reproducible efficacy. To obtain this control sample at no
cost (except for shipping), see the instructions at http://www.epa.gov/emergencies/content/ncp/index.htm.

2.4 Container Handling and Storage

2.4.1 Glassware. If the glassware has been used with oil before,
rinse with DCM to remove as much of the oil adhering to the sides of
the flask as possible; waste DCM may be used. Soak in warm water
with detergent and individually wash with bristled brushes. First
rinse with tap water, then follow with two de-ionized water rinses.
Dry either on a rack or in a 110 [deg]C drying oven). After drying,
rinse with fresh DCM (use sparingly).
2.4.2 Serum bottles and other non-volumetric glassware. Bake for
at least 4 hours in a muffle furnace at 450 [deg]C.

2.5 Calibration Curve for the UV-visible spectrophotometer

2.5.1 Stock Standard Solution Preparation. Stock standard
solution concentrations are based on the mass measurements after
each addition and density determinations of the oil/dispersant/DCM
solution using a density bottle or a 1-mL gas tight syringe. An
example calculation is given in Table 3 of this Appendix according
to the following equation:
[GRAPHIC] [TIFF OMITTED] TP22JA15.039

Use the reference oils and the specific dispersant being tested
for a particular set of experimental test runs. Prepare the stock
solution of dispersant-oil mixture in DCM, starting with 2 ml of the
oil, then adding 80 [micro]l of the dispersant followed by 18 ml of
DCM. Two sets of standards are needed, one for each oil and
dispersant combination.
2.5.2 Six-point Calibration Curve. For each reference oil, add
specific volumes of its stock standard solution (given in Table 4 of
this Appendix) to 30 ml of artificial seawater in a 125 ml
separatory funnel. Extract the oil/water mixture with triplicate 5
ml volumes of DCM. Follow each DCM addition by 15 seconds of
vigorous shaking, carefully releasing the initial pressure inside
the separatory funnel by partially removing the glass stopper inside
a fume hood after the first few shakes. Then, allow a 2-minute
stationary period for phase separation for each extraction. Drain
the extracts into a 25-mL graduated mixing cylinder. Release any
entrained bubbles of DCM from the water layer by sideways shaking of
the funnel. Use precaution not to drain water into the DCM extract
as it can affect the absorbance readings. Adjust the final volume of
the collected extracts to 20 mL in the mixing cylinder using DCM.
Determine specific masses for oil concentrations in the standards as
volumes of oil/dispersant solution multiplied by the concentration
of the stock solution. An example calculation is given in Table 4 of
this Appendix. Two calibration curves are needed, one for each oil
and dispersant combination.
2.6 Sample Preparation and Testing. See section 2.7 of this
Appendix for a detailed description of the spectrophotometer's
linear calibration procedure.
2.6.1 Six replicates of each oil and test dispersant are
required at each temperature plus two additional tests of method
blanks (artificial seawater without oil and dispersant), one at each
temperature. A completed test consists of 26 baffled flask tests (a
total of six replicates for each of two reference oil/test
dispersant combinations at two temperatures (5 [deg]C and 25
[deg]C), plus two method blanks).
2.6.2 A positive control run of 6 replicates of a dispersant
with known dispersion efficacy (see 2.3.4 above for how to obtain)
is prepared with both oils at both temperatures to verify the
protocol is being correctly performed. The lab must certify that a
positive control was successfully conducted within a year of any
testing submitted for a dispersant listing.
2.6.3 Attach a 3-inch length of Teflon tubing to the stopcock of
each of the 150-mL baffled flasks. Add 120 mL of artificial seawater
to each flask. Put screw cap on flasks and place them at the
appropriate temperature (either 5 [deg]C or 25 [deg]C) for
equilibration.
2.6.4 Calibrate and adjust the shaker table to 250
10 rpm.
2.6.5 Prepare and time separately each baffled flask.
Sequentially add 100 [micro]L of oil and 4 [micro]L of dispersant to
the flask layering them onto the center of the seawater to give a
dispersant-to-oil ratio (DOR) of 1:25. Avoid any oil or dispersant
splashing on the flask walls, as it may reduce efficacy or cause
errors in the calculated results. Discard the sample and repeat the
setup if: (1) Any oil or dispersant splashing occurs during the
additions, or (2) the dispersant contacts the water first rather
than the oil.
2.6.6 For the oil, fill the tip of the pipettor, using a wipe to
remove any oil from the sides of the tip. Holding the pipettor
vertically, dispense several times back into the reservoir to ensure
that the oil flows smoothly. Insert the syringe tip vertically into
the baffled flask, and let the bottom of the pipettor rest on the
neck of the flask. Slowly and carefully dispense the oil one time
onto the center of the water's surface. IFO 120 takes longer to
drip, and ANS will splash if dispensed too fast. The remainder of
the oil can either be returned to the oil bottle or set aside for
use in the next test flask. Note to 2.6.6: If a Brinkmann Eppendorf
repeater pipettor is used for dispensing the oil, attach a 5-mL
syringe tip, and set the dial to 1.
2.6.7 For the dispersant, use the same procedure as for the oil
to dispense onto the center of the oil slick surface. As the
dispersant first contacts the oil, it will usually push the oil to
the sides of the flask. Replace the screw cap onto the flask.
Note to 2.6.7: If a Brinkmann Eppendorf repeater pipettor is
used for dispensing the dispersant, attach a 100-[mu]L syringe tip,
and set the dial to 2.
2.6.8 Carefully place flask securely onto the shaker and agitate
for 10 0.25 minutes at 250 10 rpm.
2.6.9 Remove the flask from the shaker table and allow a
stationary, quiescent period of 10 0.25 minutes to
allow undispersed and/or recoalesced oil droplets to refloat to the
surface.
2.6.10 Carefully open the screw cap, then the stopcock at the
bottom, and discard the first several mL of seawater into a waste
beaker to remove non-mixed water-oil initially trapped in the
stopcock tubing. Collect a volume slightly greater than 30-mL into a
50-mL graduated cylinder. Adjust the collected volume to the 30-mL
mark by

[[Page 3430]]

removing excess with a disposable glass Pasteur pipette. A web-like
emulsion may form at the solvent/water interface during the water
sample extraction. Avoid pulling any emulsion phase into the DCM
extract as it may cloud the DCM-extract leading to error.
2.6.11 Transfer the water-oil sample from the graduated cylinder
into a 125-mL glass separatory funnel fitted with a Teflon stopcock.
2.6.12 Add 5 mL DCM to the separatory funnel. Start shaking,
releasing pressure into the fume hood by loosening the glass
stopper. Shake vigorously at least 20 times for 15 seconds.
2.6.13 Allow the funnel to remain in a stationary position for 2
minutes to allow phase separation of the water and DCM.
2.6.14 Drain the DCM layer from the separatory funnel into a 25
mL mixing cylinder. Avoid pulling any emulsion phase into the DCM
extract as it may cloud the DCM extract.
2.6.15 Repeat the DCM-extraction process two or three additional
times until the DCM is clear. Collect each extract in the graduated
cylinder. After the final extraction, lightly shake the separatory
funnel sideways once or twice to dislodge entrained bubbles of DCM
and drain.
2.6.16 Adjust the final volume to a known quantity, 20 or 25 mL,
in the mixing cylinder. IFO 120 samples may require dilution when
dispersed chemically because of their high absorbance properties.
Using a syringe, dispense 2.5 mL or 5.0 mL of an IFO 120 sample into
a 10-mL volumetric flask, and fill with DCM to make either a 1:4 or
1:2 dilution, respectively. ANS samples adjusted to 25 mL typically
don't require dilution.
2.6.17 If analysis cannot be conducted immediately, store the
extracted DCM samples at 4 [deg]C until time of analysis. Glass-
stoppered mixing cylinders may be used for short-term storage or
prior to bringing the extracts up to volume. After bringing to
volume, transfer the DCM extracts to 25-30 ml crimp-style serum
vials with aluminum/Teflon seals.
2.6.18 Complete all analysis within 10 consecutive days from
when the sample was collected.
2.7 UV-Visible Spectrophotometer Linear Stability Calibration
2.7.1 A six-point calibration of the UV-visible
spectrophotometer is required at least once per day for each oil.
The stability calibration criterion is determined with the six oil
standards identified in Table 4 of this Appendix.
2.7.2 Turn on spectrophotometer and allow it to warm up for at
least 30 minutes before beginning analysis. Blank the instrument for
the wavelengths between 340 and 400 nm with DCM.
2.7.3 If refrigerated, allow all extracts, standards and samples
to warm to room temperature.
2.7.4 Determine the absorbance of the six standards between the
wavelengths of 340 and 400 nm. This can be done by either one of the
following methods:
2.7.4.1 Trapezoidal Rule. Program the spectrophotometer to take
readings every 5[lgr] or 10[lgr] and calculate the area under the
curve using the Trapezoidal rule:
[GRAPHIC] [TIFF OMITTED] TP22JA15.040

where N+1 = number of absorbance measurements to delineate N equally
spaced sections of the curve, and H = the distance ([lgr]) between
each reading. For H = 5, N+1 = 13 measurements, for H = 10, N+1 = 7.
The following formula illustrates readings taken every 10[lgr].
[GRAPHIC] [TIFF OMITTED] TP22JA15.041

When using readings taken every 5[lgr], each absorbance sum is
multiplied by 5.
2.7.4.2 Automatic Integration. Program the spectrophotometer to
automatically integrate the area under the curve between 340 nm and
400 nm.
2.7.4.3 If the wavelengths must be manually set on the
spectrophotometer, the older method of only measuring at 340 [lgr],
370 [lgr], and 400 [lgr] may be used. Then calculate using the
trapezoidal rule for N + 1 = 3, H = 30. While the resulting area
count with the older method is less accurate, the final results are
similar since the inaccuracy is systematic.
2.7.5 After determining the area count for each standard,
determine the response factor (RF) for the oil at each concentration
using the following equation:
[GRAPHIC] [TIFF OMITTED] TP22JA15.042

2.7.6 Spectrophotometer stability for the initial calibration is
acceptable when the RFs of the six standard extracts are less than
10% different from the overall mean value for the six standards, as
calculated in Equation 5 of this Appendix and depicted in the
example in Table 4 of this Appendix.
[GRAPHIC] [TIFF OMITTED] TP22JA15.043

2.7.7 If this criterion is satisfied, begin analysis of sample
extracts. Absorbances greater than or equal to 3.5 are not included
because absorbance saturation occurs at and above this value. If any
of the standard oil extracts fails to satisfy the initial-stability
criterion, the source of the problem (e.g., preparation protocol for
the oil standards, spectrophotometer stability, etc.) must be
corrected before analysis of the sample extracts begins.
2.7.8 Determine the slope of the calibration points by using
linear regression forced zero intercept:
[GRAPHIC] [TIFF OMITTED] TP22JA15.044

[[Page 3431]]

2.8 Spectrophotometric Analysis and Calculations
2.8.1 Once a successful calibration curve for each of the two
reference oils has been created and verified, measure experimental
replicates for each of the reference oils at each temperature
followed by a standard check sample.
2.8.2 The same procedure is followed for the positive controls.
2.8.3 Determine the area for the absorbance values obtained for
the experimental samples by using Equation 2 of this Appendix and
illustrated by Equation 3 of this Appendix.
2.8.4 Calculate the Total Oil dispersed and the percentage of
oil dispersed (%OD) based on the ratio of oil dispersed in the test
system to the total oil added to the system, as follows:
[GRAPHIC] [TIFF OMITTED] TP22JA15.045

where:

VDCM = final volume of the DCM extract (mL)
Vtw = total seawater in Baffled Flask (120 mL)
Vew = volume seawater extracted (30 mL)
[GRAPHIC] [TIFF OMITTED] TP22JA15.046

where:

[rho]Oil = density of the specific test oil, mg/mL and
VOil = Volume (mL of oil added to test flask (100 [mu]L =
0.1 mL))
2.8.5 The %ODs for the six replicates within a particular
treatment are then subjected to an outlier test, the Grubb's Test or
Maximum Normal Residual test (6). A convenient Internet-based
calculator of a Grubbs outlier may be found at: http://www.graphpad.com/quickcalcs/Grubbs1.cfm. If an outlier is detected
(p < 0.05), analyze an additional replicate to obtain the required
six replicates.
2.8.6 Report the Dispersion Efficacy value for each oil and each
temperature, which is the lower 95% confidence level of the 6
independent replicates (DELCL95) for each oil/temperature
combination. Error bars are not needed as reporting the lower
confidence level computationally takes the variability of the
replicates into account as shown in Equation 9 of this Appendix.
[GRAPHIC] [TIFF OMITTED] TP22JA15.047

where %OD = mean percentage oil dispersed for the n = 6 replicates,
S = standard deviation, and t (n-1,1-[alpha])
= 100 * (1-[alpha])^th percentile from the t-distribution
with n-1 degrees of freedom. For 6 replicates, t
n-1,1-[alpha] = 2.015, where [alpha] = 0.05. An example
of the calculations is given in Table 5 of this Appendix.
2.9 Performance Criterion
The dispersant product tested will remain in consideration for
listing on the NCP Product Schedule if the dispersant efficacy
(DELCL95), as calculated in section 2.8.6 of this
Appendix, is:

------------------------------------------------------------------------
Temp DELCL95
Oil ([deg]C) (%)
------------------------------------------------------------------------
ANS.................................................. 5 >= 70
ANS.................................................. 25 >= 75
IFO120............................................... 5 >= 55
IFO120............................................... 25 >= 65
------------------------------------------------------------------------

2.10 Quality Control (QC) Procedures for Oil Concentration
Measurements
2.10.1 Absorbance readings. Perform at least 5% of all UV-
visible spectrophotometric measurements in duplicate as a QC check
on the analytical measurement method. The absorbance values for the
duplicates must agree within 5% of their mean value.
2.10.2 Method blanks. Analytical method blanks involve an
analysis of artificial seawater blanks (artificial seawater without
oil or dispersant in a baffled flask) through testing and analytical
procedures. Analyze method blanks with a frequency of at least two
per completed test. Oil concentrations in method blanks must be less
than detectable limits.
2.10.3 Accuracy. Determine accuracy by using a mid-point
standard calibration check after each set of replicate samples
analyzed. The acceptance criterion is based on a percent recovery of
90-110% using the following equation:
[GRAPHIC] [TIFF OMITTED] TP22JA15.048

2.10.4 Calibration QC checks. Before analyzing samples, the
spectrophotometer must meet an instrument stability calibration
criterion using the oil standards. The instrument stability for
initial calibration is acceptable when the RFs (Equation 5 of this
Appendix) for each of the six standard concentration levels are less
than 10% different from the overall mean value.

Table 1--Constituent Concentrations for GP2 Artificial Seawater
[Based on Spotte et al., 1984]
------------------------------------------------------------------------
Concentration
Constituent (g/L)
------------------------------------------------------------------------
NaCl.................................................... 21.03
Na2SO4.................................................. 3.52
KCl..................................................... 0.61
KBr *................................................... 0.088
Na2B4O7 [middot]10H2O *................................. 0.034
MgCl2 [middot]6H20...................................... 9.50
CaCl2 [middot]2H2O...................................... 1.32
SrCl2 [middot]6H2O *.................................... 0.02
NaHCO2 *................................................ 0.17
------------------------------------------------------------------------
* Use Stock Solution, 1 mL/L GP2 for 100X stock solution for Bromide,
Borate, and Strontium.
10 mL/L GP2 for bicarbonate--10X stock solution as it is not soluble in
a 100X solution.

[[Page 3432]]

Adjust to pH 8.0 prior to autoclaving.

Table 2--Test Oil Characteristics
----------------------------------------------------------------------------------------------------------------
Viscosity @ Category by
Oil Density, mg/mL API gravity 15 [deg]C, Category by API kinematic
@ 15 [deg]C (deg) (cSt) gravity viscosity
----------------------------------------------------------------------------------------------------------------
ANS............................. 884 28.2 40 Medium........... Light
IFO120.......................... 948 17.5 1520 Heavy............ Heavy
----------------------------------------------------------------------------------------------------------------

Table 3--Stock Solution Preparation
------------------------------------------------------------------------
Item Amount
------------------------------------------------------------------------
Mass of Bottle, g.......................................... 29.9666
Mass of Bottle + oil, g.................................... 31.5734
Mass of bottle + disp + oil + DCM, g....................... 55.0425
Mass of oil, g............................................. 1.6068
Mass of disp + oil + DCM, g................................ 25.0759
Mass of 1 mL syringe, g.................................... 14.5563
Mass of 1 mL syringe + solution, g......................... 15.8779
------------------------------------------------------------------------
Density of solution, g/mL.................................. 1.3216
Volume of solution, mL..................................... 18.9740
Conc. Of stock solution, mg/mL............................. 84.6850
------------------------------------------------------------------------

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[[Page 3433]]

[GRAPHIC] [TIFF OMITTED] TP22JA15.049

[[Page 3434]]

2.11 References for Section 2.0
(1) U.S. Environmental Protection Agency (1994), ``Swirling
Flask Dispersant Effectiveness Test,'' Title 40 Code of Federal
Regulations, Pt. 300, Appendix C, pp 47458-47461.
(2) Sorial, G.A., A.D. Venosa, K.M, Koran, E. Holder, and D.W.
King. 2004. ``Oil spill dispersant effectiveness protocol: I. Impact
of operational variables.'' ASCE J. Env. Eng. 130(10):1073-1084.
(3) Sorial, G.A., A.D. Venosa, K.M, Koran, E. Holder, and D.W.
King. 2004. ``Oil spill dispersant effectiveness protocol: II.
Performance of revised protocol.'' ASCE J. Env. Eng. 130(10):1085-
1093.
(4) Venosa, A.D., D.W. King, and G.A. Sorial. 2002. ``The
baffled flask test for dispersant effectiveness: A round robin
evaluation of reproducibility and repeatability.'' Spill Sci. &
Technol. Bulletin 7(5-6):299-308.
(5) Spotte, S., G. Adams, and P.M. Bubucis. 1984. ``GP2 medium
is an synthetic seawater for culture or maintenance of marine
organisms,'' Zoo Biol, 3:229-240.
(6) Grubbs, F. 1969. ``Sample Criteria for Testing Outlying
Observations,'' Annals of Mathematical Statistics, pp. 27-58.

3.0 Dispersant Toxicity Testing

3.1 Summary. This laboratory protocol includes testing for: (1)
Dispersant standard static acute toxicity tests for the mysid
shrimp, Americamysis bahia (48-hr duration) and the inland
silverside, Menidia beryllina (96-hr duration); (2) dispersant/oil
mixture static acute toxicity tests for Americamysis bahia and
Menidia beryllina (48-hr and 96-hr duration, respectively); (3)
dispersant developmental assay for the purple sea urchin,
Strongylocentrotus purpuratus, (72-hr duration); and (4) dispersant
7-day static subchronic tests with Americamysis bahia and Menidia
beryllina (Table 6 of this Appendix).

Table 6--Toxicity Testing Requirements for Dispersants
----------------------------------------------------------------------------------------------------------------
Test procedure
-----------------------------------------------------------------------------------------------------------------
96-hr static 48-hr static 72-hr sea urchin 7-day subchronic:
Test substance acute: Menidia acute: Developmental M. beryllina & A.
beryllina Americamysis Bahia Assay bahia
----------------------------------------------------------------------------------------------------------------
Dispersant only.................. yes............... yes............... yes............... yes.
Dispersant/Reference Oil Mixture. yes............... yes............... no................ no.
----------------------------------------------------------------------------------------------------------------

3.2 Preparation of Stock Solutions

3.2.1 Dispersant. Prepare a 1000 [mu]L/L primary stock solution
prior to test initiation by adding 1.1 mL of dispersant to 1100 mL
of dilution water consisting of salinity adjusted uncontaminated
natural or artificial seawater, in a glass vessel. Using a
laboratory top stirrer equipped with a stainless steel blade, center
the stirrer blade in the mixing vessel one inch off the bottom.
Initially mix the resulting stock solution for approximately five
seconds at speeds of < 10,000 rpm to avoid foaming. Thereafter, set
the speed to provide a 70% vortex. Using a glass pipette, remove
appropriate aliquots of stock solution from between the mixing
vessel wall and edge of the vortex and place directly into the
dilution water within an exposure vessel. Suspend mixing of the
stock solution after the removal of each aliquot. Base the
preparation of exposure solutions on the nominal concentration of
the stock solution and follow procedures outlined in sections 3.5
and 3.6 of this Appendix.
3.2.2 Dispersant-Reference Oil(s) Mixtures. Use IFO 120 and ANS
oils. To obtain these oils at no charge (except for a minimal
shipping fee) see http://www.epa.gov/emergencies/content/ncp/index.htm. Assessment of dispersant-reference oil mixture (DOM)
toxicity is determined for each reference oil using the aqueous
phase of a chemically enhanced-water accommodated fraction (CE-WAF).
Repeat the following procedure for each reference oil tested. Fit a
glass aspirator bottle (approximately 23L) equipped with a hose bib
at the base with a length of silicon tubing containing a hose clamp.
Fill the bottle with 19L of seawater leaving a 20% headspace above
the liquid, place on a magnetic stir plate then add and center a
stir bar. Add the respective crude oil at 25g/L using a silicon tube
attached to a glass funnel that reaches just below the water
surface. Using this method reduces the production of air bubbles on
the oil surface slick. Adjust the stir plate to obtain an oil vortex
of 25% of the total volume of the seawater, then add the dispersant
to be tested at a ratio of 1:10 dispersant:oil (2.5 g/L). Securely
seal the bottle to reduce the loss of volatiles using a silicon
stopper and wraps of Parafilm and stir for 18 hours, then allow the
solution to settle for 6 hours. Maintain the temperature at 25
[deg]C during stirring and settling. Purge the hose at the base of
the bottle of any material followed by removal of the CE-WAF
(aqueous phase) into a clean glass container without disturbing the
surface oil slick. The CE-WAF should be remixed and 1-2 L removed
for chemical analysis of total petroleum hydrocarbons (TPH)
following the procedures outlined in section 3.4 of this Appendix.
The remaining volume will be used for the preparation of exposure
solutions following procedures outlined in section 3.3 of this
Appendix. To reduce time and cost, mix sufficient amounts of
dispersant product-reference oil mixture CE-WAF to allow preparation
of exposure solutions for conducting simultaneous acute tests with
both Americamysis bahia and Menidia beryllina.

3.3 Preparation of Exposure Concentrations

3.3.1 Concentration Selection. Preliminary rangefinder tests may
be necessary using a series of logarithmic concentrations (e.g. 0.1,
1, 10, 100 [mu]l dispersant product/L or mg TPH/L) to determine the
appropriate exposure concentration range necessary to determine
LC50 values and 95% confidence intervals. For definitive
tests, conduct a minimum of five test concentrations using a
geometric ratio between 1.5 and 2.0 (e.g. 2, 4, 8, 16, and 32). Note
that when testing only the dispersant product, the highest test
concentration must not exceed the dispersant's self-dispersibility
limit.
3.3.2 Exposure Concentrations. Exposure solutions are prepared
by adding the appropriate amount of stock solution directly to
dilution water in each test chamber. Mix each exposure solution
using five rotations in one direction followed by five rotations in
the opposite direction using a solid glass stir rod.
3.3.3 Reference Toxicants. Separate toxicity tests must be
performed with a reference toxicant for each species tested. Conduct
additional reference toxicity tests any time a change in the
population or source of a test species occurs. Use sodium dodecyl
sulfate (SDS), also known as dodecyl sodium sulfate (DSS), and
sodium lauryl sulfate (SLS) as the reference toxicant for exposures
conducted with Menidia beryllina and Americamysis bahia. Use copper
chloride as the reference toxicant for exposures conducted with the
sea urchin developmental test. Use reagent grade quality SDS and
copper chloride for tests. Information on procedures for conducting
reference toxicant tests with these species can be found in the
specific EPA methods documents cited in sections 3.5.1, 3.6.1 and
3.7.1 of this Appendix.
3.4 Chemical Analysis of Stock Solutions. Add the 1L sample of
CE-WAF (Section 3.2.2 of this Appendix) solutions directly to amber
glass bottles with Teflon[supreg]-lined cap. Collect a replicate
sample in the event of accidental loss or if reanalysis of the stock
solution becomes necessary. Adjust sample to a pH=2 using 50%
hydrochloric acid, immediately refrigerate and analyze within 48
hours of collection. Analyze samples for C9-C32 TPH by gas
chromatography-flame ionization detection (GC-FID) following EPA SW-
846, Method 8015B-DRO (4). Report TPH concentration of stock
solutions as milligrams TPH/L and use in the calculation of exposure
concentrations for all toxicity tests conducted with CE-WAF.

[[Page 3435]]

3.5 Static Acute Tests With M. beryllina and A. bahia

3.5.1 General. Use EPA's Methods for Measuring the Acute
Toxicity of Effluents and Receiving Waters to Freshwater and Marine
Organisms (EPA-821-R-02-012) (1) for testing each species separately
with dispersant product or a mixture of dispersant product and
reference oil (DOM).
3.5.2 Test Solutions. Modify procedures in EPA-821-R-02-012
specifically dealing with the handling and toxicity testing of
effluents or receiving water samples as follows: Prepare stock
solutions following section 3.2 of this Appendix and exposure
concentrations following section 3.3 of this Appendix.
3.5.3 Number of Treatments, Replicates and Organisms. Conduct a
minimum of three replicates of at least five exposure treatments
plus a minimum of three replicate dilution water controls. Expose
ten organisms per replicate treatment.
3.5.4 Exposure Period. Test duration is 48-hr for Americamysis
bahia and 96-hr for Menidia beryllina. Mortality must be recorded at
each 24 hour period of each test.
3.5.5 Test Acceptability. For each test performed, survival of
control animals must be >90% and test results must allow
determination of statistically valid LC50 and 95%
confidence interval values except in cases where the LC50
is >1000 [mu]l/L or is determined to be greater than the limits of
water solubility of dispersibility.
3.5.6 Static Acute Test Summary. A summary of required test
conditions is provided in Table 7 of this Appendix.

3.6 Sea Urchin Developmental Test With Dispersant Product

3.6.1 General. Use Section 15, ``Purple Urchin,
Strongylocentrotus purpuratus and Sand Dollar, Dendraster
excentricus Larval Development Test Method'' of EPA's Short-Term
Methods for Estimating the Chronic Toxicity of Effluents and
Receiving Waters to West Coast Marine and Estuarine Organisms (EPA/
600/R-95-136) (2).
3.6.2 Test Organism. Tests of dispersant products are to follow
methods for the purple urchin only. Tests with the sand dollar are
not required.
3.6.3 Test Solutions. Modify procedures in EPA/600/R-95-136,
Section 15 specifically dealing with the handling and toxicity
testing of effluents or receiving water samples as follows: Prepare
stock solutions following section 3.2.1 of this Appendix and
exposure concentrations following section 3.3 of this Appendix.
3.6.4 Number of Treatments and Replicates. Conduct a minimum of
four replicates of five exposure treatments plus a minimum of four
replicate dilution water controls.
3.6.5 Exposure Duration and Test Endpoint. Examine the effects
of the dispersant product on normal development of sea urchin
embryos over a period of 72 hours. An IC50 (the exposure
concentration at which normal development is inhibited in 50% of the
embryos) with 95% confidence intervals are to be determined in place
of an IC25. The concentration of dispersant causing
inhibition of development in 50% of exposed embryos
(IC50) with the lower and upper 95% confidence intervals
(LCI95 and ULCI95) must be calculated at the
end of the exposure period. Mortality determinations are not
required.
3.6.6 Test Acceptability. Requirements of the assay are: (i) >=
80% normal larval development in the control treatment, (ii) the
minimum significant difference (MSD) that can be statically detected
relative to the control is <=25%, (iii) test results which support
the determination of a statistically valid IC50 and 95%
confidence interval unless the LC50 is >1000 [mu]l/L or
is greater than the limits of water solubility of dispersibility.
3.6.7 Urchin Developmental Test Summary. A summary of required
test conditions is provided in Table 7 of this Appendix.

3.7 Seven-Day Subchronic Tests With M. beryllina and A. bahia

3.7.1 General. Use Section 13, Method 1006.0, ``Inland
Silverside (Menidia beryllina) Larval Survival and Growth Method,''
and Section 14, Method 1007.0, ``Mysid (Mysidopsis [renamed
Americamysis] bahia) Survival, Growth, and Fecundity Method'' of
EPA's Short-Term Methods for Estimating the Chronic Toxicity of
Effluents and Receiving Waters to Marine and Estuarine Organisms
(EPA-821-R-02-014) (3) for testing of dispersant product.
3.7.2 Test Solutions. Modify procedures in EPA-821-R-02-014,
sections 13 and 14 specifically dealing with the handling and
toxicity testing of effluents or receiving water samples as follows:
Prepare stock solutions following section 3.2.1 of this Appendix and
exposure concentrations following section 3.3 of this Appendix.
Exposure solutions should be renewed every 24 hr for the duration of
the test.
3.7.3 Number of Treatments, Replicates and Organisms. (i)
Menidia beryllina: Conduct a minimum of four replicates of at least
five exposure treatments plus a minimum of four replicate dilution
water controls. Expose ten M. beryllina per replicate treatment.
(ii) Americamysis bahia: Conduct a minimum of eight replicates of at
least five exposure treatments plus a minimum of eight replicate
dilution water controls. Expose five A. bahia per replicate
treatment.
3.7.4 Exposure Duration and Test Endpoint. The test duration is
seven days for both species. Test endpoints for Menidia beryllina
are survival and growth (dry weight) and for Americamysis bahia is
survival, growth (dry weight) and fecundity. Calculate an
LC50 and 95% confidence interval for survival and
IC25 and IC50 with 95% confidence intervals
for growth (and fecundity for A. bahia only). Report the lowest
observed effect concentration (LOEC) and no observed effect
concentration (NOEC) for each endpoint.
3.7.5 Test Acceptability. Requirements of the assay are: (i)
>=80% survival in the control treatment for each species, (ii) dry
weights must meet the specific requirements as stipulated in Method
1006.0 for Menidia beryllina and Method 1007.0 for Americamysis
bahia, (iii) egg production must occur in 50% of female Americamysis
bahia in the replicate control treatments.
3.7.6 Subchronic Test Summary. A summary of required test
conditions for each species is provided in Table 7 of this Appendix.
3.8. Laboratory Report. The laboratory must include, for each
toxicity test report, all applicable information, data and analyses
as follows:
3.8.1 Test Objective: Protocol title and source, endpoint(s);
3.8.2 Product Information: Product name, manufacturer contact
information, lot number, production date, date received/chain of
custody;
3.8.3 Contract Facility: Contact information;
3.8.4 Dilution Water: Source, pretreatment, physical and
chemical characteristics (pH, salinity);
3.8.5 Test Conditions: Date and time of test (start and end),
test chambers type and volume, volume of solution per chamber,
number of organisms per chamber, number of replicate chambers per
treatment, feeding frequency, amount and type of food, test
concentrations, test temperature (mean and range), test salinity
(mean and range);
3.8.6 Test Organisms: Common and scientific name, source contact
information, age and date purchased, acclimation conditions (e.g.,
temperature, salinity, both mean and range), age at test start;
3.8.7 Reference toxicant: Date received, lot number, date of
most recent test, results and current Cumulative Sum Chart, dilution
water used, physical and chemical methods used;
3.8.8 Quality Assurance: Verification of laboratory
accreditation, including subcontractor facilities;
3.8.9 Test Results: Raw data in tabular and graphical form,
daily records of affected organisms in each concentration replicate
and controls, table of required endpoints (i.e., LC50
with 95% confidence interval (CI), IC25 and
IC50 with 95% CI, LOEC and NOEC), statistical methods
used to calculate endpoints, summary tables of test conditions and
QA data;
3.8.10 Analytical Results: Method summary including Limit of
Detection (LOD)/Limit of Quantitation (LOQ), deviations and reasons
if any, sample summary, results including chromatograms and data
qualifiers, QA summary including calibration curves, method blank
and surrogate recovery, analytical results summary; and
3.8.11 Conclusions: Relationship between test endpoints and
threshold limit.

[[Page 3436]]

Table 7--Summary of Test Conditions--Dispersant Toxicity
--------------------------------------------------------------------------------------------------------------------------------------------------------
Subchronic M. Development S.
Acute M. beryllina Acute A. bahia beryllina Subchronic A. bahia purpuratus
--------------------------------------------------------------------------------------------------------------------------------------------------------
Test type.......................... Static non-renewal.... Static non-renewal.... Static renewal Static renewal Static non-renewal.
(daily). (daily).
Test duration...................... 96 hours.............. 48 hours.............. 7 days............... 7 days............... 72 2
hours.
Salinity........................... 20 20 20 20 34
2[permil]. 2[permil]. 2[permil]. 2[permil]. 2[permil].
--------------------------------------------------------------------------------------------------------------------
Temperature........................ 25 1 [deg]C. Test temperatures must not deviate (maximum minus minimum 15 1
temperature) by for than 3 [deg]C during the test. [deg]C.
--------------------------------------------------------------------------------------------------------------------
Light quality...................... Ambient laboratory illumination
--------------------------------------------------------------------------------------------------------------------
Light intensity.................... 10-20 [mu]E/m\2\/s
--------------------------------------------------------------------------------------------------------------------
Photoperiod........................ 16 h light, 8 h darkness, with phase in/out period recommended
--------------------------------------------------------------------------------------------------------------------
Test chamber size \1\.............. 250 mL................ 250 mL................ 600 mL-1 L........... 400 mL............... 30 mL.
Test solution volume \1\........... 200 mL................ 200 mL................ 500-750 mL........... 150 mL............... 10 mL.
Age of test organism \2\........... 9-14 days............. 1-5 days.............. 7-11 days............ 7 days............... 1 hr old fertilized
eggs.
No. organisms per test chamber..... 10.................... 10.................... 10................... 5.................... 25 embryos per mL.
No. of replicate chambers per 3..................... 3..................... 4.................... 8.................... 4.
concentration.
--------------------------------------------------------------------------------------------------------------------
Feeding regime..................... Refer to specific feeding procedures provided in each test method None.
--------------------------------------------------------------------------------------------------------------------
Aeration........................... None, unless DO falls below 4.0 mg/L, then aerate all chambers. Rate:<100 bubbles/minute
--------------------------------------------------------------------------------------------------------------------
Test concentrations................ 5 exposure concentrations and a control (minimum required)
--------------------------------------------------------------------------------------------------------------------
Test acceptability (required)...... >=90% survival in >=90% survival in For controls: >=80% For controls: >=80% >=80% normal shell
controls. controls. survival; average survival; average development in
dry weight >=0.5mg dry weight >=0.20 controls.
where test starts mg; >= 50% of
with 7 day old control females
larvae, or >= 0.43 produce eggs.
mg for larvae
preserved for
<=7days.
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Recommended minimum value.
\2\ Less than or equal to 24-hr range in age.

3.9 References for Section 3.0

(1) U.S. EPA. 2002. Methods for Measuring the Acute Toxicity of
Effluents and Receiving Waters to Freshwater and Marine Organisms.
Fifth Edition. U.S. Environmental Protection Agency, Washington, DC
(EPA-821-R-02-012).
(2) U.S. EPA. 1995. Short-Term Methods for Estimating the Chronic
Toxicity of Effluents and Receiving Waters to West Coast Marine and
Estuarine Organisms. First Edition. U.S. Environmental Protection
Agency, Washington, DC (EPA/600/R-95-136)
(3) U.S. EPA. 2002. Short-Term Methods for Estimating the Chronic
Toxicity of Effluents and Receiving Waters to Marine and Estuarine
Organisms U.S. Environmental Protection Agency, Washington, DC (EPA-
821-R-02-014).
(4) U.S. EPA. 2008. Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods U.S. Environmental Protection Agency,
Washington, DC (SW-846) http://www.epa.gov/osw/hazard/testmethods/sw846/online/index.htm.

4.0 Standard Acute Toxicity Testing of Surface Washing Agents,
Bioremediation Agents, Herding Agents, and Solidifiers.

4.1 Summary. This laboratory protocol includes testing for: (1)
Saltwater standard static acute toxicity tests for test products
with the mysid shrimp, Americamysis bahia (48-hr duration) and the
inland silverside, Menidia beryllina (96-hr duration); and (2)
freshwater standard static acute toxicity tests for test products
with the daphnid, Ceriodaphnia dubia (48-hr duration) and the
fathead minnow, Pimephales promelas (96-hr duration) (see Table 8 of
this Appendix).

TABLE 8--Toxicity Testing Requirements for Surface Washing Agents, Herding Agents, Bioremediation Agents and
Solidfiers
----------------------------------------------------------------------------------------------------------------
Test procedure
------------------------------------------------------------------------------
48-hr static
Application environment 96-hr static 48-hr static 96-hr static acute:
acute: Menidia acute: acute: Pimephales Ceriodaphnia
beryllina Americamysis bahia promelas dubia
----------------------------------------------------------------------------------------------------------------
Saltwater only................... yes............... yes............... no................ no.
Freshwater only.................. no................ no................ yes............... yes.
Freshwater and saltwater use..... yes............... yes............... yes............... yes.
----------------------------------------------------------------------------------------------------------------

[[Page 3437]]

4.2 Dilution Water. Use Section 7 of EPA's Methods for Measuring
the Acute Toxicity of Effluents and Receiving Waters to Freshwater
and Marine Organisms (EPA-821-R-02-012) [1] for preparation of the
appropriate dilution water for each species tested. Use of clean
natural or synthetic seawater for tests conducted with saltwater
species is acceptable.

4.3 Preparation of Stock Solutions

4.3.1 Liquid Surface Washing Agents and/or Herding Agents.
Prepare a 1000 [mu]L/L stock solution prior to test initiation by
adding 1.1 mL of test product to 1100 mL of dilution water in a
glass vessel. Place on a magnetic stir plate then add and center a
stir bar and adjust the stir plate to obtain a vortex of 25% of the
total volume of the liquid. Mix the resulting stock solution for
approximately five minutes at room temperature. Using a glass
pipette, remove appropriate aliquots of stock solution from between
the mixing vessel wall and edge of the vortex and place directly
into the dilution water within an exposure vessel. Base the
preparation of exposure solutions on the nominal concentration of
the stock solution and follow procedures outlined in sections 4.6
and/or 4.7 of this Appendix, as appropriate.
4.3.2 Bioremediation Agents. For products consisting of two or
more liquid and/or solid components, prepare the product following
the manufacturers recommended procedure and ensure the test product
mixture is completely blended. Prepare a 1000 [micro]L/L stock
solution prior to test initiation by adding 1.1 mL of the test
product mixture to 1100 mL of dilution water in a glass vessel.
Place on a magnetic stir plate then add and center a stir bar and
adjust the stir plate to obtain a vortex of 25% of the total volume
of the liquid. Mix the resulting stock solution for approximately
five minutes at room temperature. Using a glass pipette, remove
appropriate aliquots of stock solution from between the mixing
vessel wall and edge of the vortex and place directly into the
dilution water within an exposure vessel. Base the preparation of
exposure solutions on the nominal concentration of the stock
solution and follow procedures outlined in sections 4.5 and/or 4.6
of this Appendix, as appropriate.
4.3.3 Solid Phase Products. Assessment of the toxicity of
solidifiers and other solid phase products are determined using the
aqueous phase of water-accommodated fractions (WAFs) of the test
product. Fit a glass aspirator bottle (approximately 23L) equipped
with a hose bib at the base with a length of silicon tubing
containing a hose clamp. Fill the bottle with 19L of dilution water
leaving a 20% headspace above the liquid, place on a magnetic stir
plate then add and center a stir bar. Add the test product at 25 g/L
and securely seal the bottle using a silicon stopper and wraps of
parafilm. Adjust the stir plate to obtain a vortex of 25% of the
total fluid volume, stir for 18 hours then settle for 6 hours.
Maintain the temperature at 25 [deg]C during stirring and settling.
Purge the hose at the base of the bottle of any material followed by
removal of the WAF (aqueous phase) into a clean glass container
without disturbing the product on the surface. The WAF should be
remixed and used for the preparation of exposure solutions following
procedures outlined in section 4.4 of this Appendix.

4.4 Preparation of Exposure Concentrations

4.4.1 Concentration Selection. Preliminary rangefinder tests may
be necessary using a series of logarithmic concentrations (e.g. 0.1,
1, 10, 100 [micro]l test product/L) to determine the appropriate
exposure concentration range necessary to determine LC50
values and 95% confidence intervals. For definitive tests, conduct a
minimum of five test concentrations using a geometric ratio between
1.5 and 2.0 (e.g. 2, 4, 8, 16, and 32). Note that when testing the
product, the highest test concentration should not exceed the test
product's self-dispersibility limit.
4.4.2 Exposure Concentrations. Exposure solutions are prepared
by adding the appropriate amount of stock solution directly to
dilution water in each test chamber. Mix each exposure solution
using five rotations in one direction followed by five rotations in
the opposite direction using a solid glass stir rod.
4.4.3 Reference Toxicants. Separate toxicity tests must be
performed with a reference toxicant for each species tested. Conduct
additional reference toxicity tests any time a change in the culture
population or source of a test species occurs. Use reagent grade
quality sodium dodecyl sulfate (SDS), also known as dodecyl sodium
sulfate (DSS), and sodium lauryl sulfate (SLS) as the reference
toxicant. Information on procedures for conducting reference
toxicant tests with these species can be found in section 4 of EPA's
Methods for Measuring the Acute Toxicity of Effluents and Receiving
Waters to Freshwater and Marine Organisms (EPA-821-R-02-012) (3).

4.5 Saltwater Static Acute Tests With Menidia beryllina and
Americamysis bahia

4.5.1 General. Use EPA's Methods for Measuring the Acute
Toxicity of Effluents and Receiving Waters to Freshwater and Marine
Organisms (EPA-821-R-02-012) (1) for testing each species separately
with the test product.
4.5.2 Test Solutions. Modify procedures in EPA-821-R-02-012
specifically dealing with the handling and toxicity testing of
effluents or receiving water samples as follows: Prepare stock
solutions following the appropriate sections (4.3.1, 4.3.2, or
4.3.3) of this Appendix and exposure concentrations following
section 4.4 of this Appendix.
4.5.3 Number of Treatments, Replicates and Organisms. Conduct a
minimum of three replicates of at least five exposure treatments
plus a minimum of three replicate dilution water controls. Expose
ten organisms per replicate treatment.
4.5.4 Exposure Period. Test duration is 48-hr for A. bahia and
96-hr for M. beryllina. Mortality must be recorded at each 24 hour
period of each test.
4.5.5 Test Acceptability. For each test performed, survival of
control animals must be > 90% and test results must allow
determination of statistically valid LC50 and 95%
confidence interval values except in cases where the LC50
is >1000 [micro]l/L or is determined to be greater than the limits
of water solubility or dispersibility.
4.5.6 Static Acute Test Summary. A summary of required test
conditions is provided in Table 9 of this Appendix.

4.6 Freshwater Static Acute Tests With Pimephales promelas and
Ceriodaphnia dubia

4.6.1 General. Use EPA's Methods for Measuring the Acute
Toxicity of Effluents and Receiving Waters to Freshwater and Marine
Organisms (EPA-821-R-02-012) (1) for testing each species separately
with the test product.
4.6.2 Test Solutions. Modify procedures in EPA-821-R-02-012
specifically dealing with the handling and toxicity testing of
effluents or receiving water samples as follows: Prepare stock
solutions following the appropriate sections (4.3.1, 4.3.2, or
4.3.3) of this Appendix and exposure concentrations following
section 4.4 of this Appendix.
4.6.3 Number of Treatments, Replicates and Organisms. P.
promelas: Conduct a minimum of three replicates of at least five
exposure treatments plus a minimum of three replicate dilution water
controls. Expose ten organisms per replicate treatment. C. dubia:
Conduct a minimum of four replicates of at least five exposure
treatments plus a minimum of four replicate dilution water controls.
Expose five organisms per replicate treatment.
4.6.4 Exposure Period. Test duration is 48-hr for C. dubia and
96-hr for P. promelas. Mortality must be recorded at each 24 hour
period of each test.
4.6.5 Test Acceptability. For each test performed, survival of
control animals must be > 90% and test results must allow
determination of statistically valid LC50 and 95%
confidence interval values except in cases where the LC50
is >1000 [micro]l/L or is determined to be greater than the limits
of water solubility of dispersibility.
4.6.6 Static Acute Test Summary. A summary of required test
conditions is provided in Table 9 of this Appendix.

4.7 Laboratory Report

The laboratory must include, for each toxicity test report, all
applicable information, data and analyses as follows:
4.7.1 Test Objective: Protocol title and source, endpoint(s);
4.7.2 Product Information: Product name, manufacturer contact
information, lot number, production date, date received/chain of
custody;
4.7.3 Contract Facility: Contact information;
4.7.4 Dilution Water: Source, pretreatment, physical and
chemical characteristics (pH, salinity);
4.7.5 Test Conditions: Date and time of test (start and end),
test chambers type and volume, volume of solution per chamber,
number of organisms per chamber, number of replicate chambers per
treatment, feeding frequency, amount and type of food, test
concentrations, test temperature (mean and range), test salinity
(mean and range);
4.7.6 Test Organisms: Common and scientific name, source contact
information, age and date purchased, acclimation conditions (e.g.,
temperature, salinity, both mean and range), age at test start;
4.7.7 Reference toxicant: Date received, lot number, date of
most recent test, results

[[Page 3438]]

and current Cumulative Sum Chart, dilution water used, physical and
chemical methods used;
4.7.8 Quality Assurance: Verification of laboratory
accreditation, including subcontractor facilities;
4.7.9 Test Results: Raw data in tabular and graphical form,
daily records of affected organisms in each concentration replicate
and controls, table of required endpoints (i.e., LC50,
95% CI, inhibited concentration for 50% of the species
(IC50), lower observed effect concentration (LOEC) and no
observed effect concentration (NOEC)), statistical methods used to
calculate endpoints, summary tables of test conditions and QA data;
and
4.7.10 Conclusions: Relationship between test endpoints and
threshold limit.

Table 9--Summary of Test Conditions--Surface Washing Agents, Herding Agents, Bioremediation Agents and Solidifiers Toxicity
--------------------------------------------------------------------------------------------------------------------------------------------------------
Freshwater Acute P.
Saltwater Acute M. beryllina Saltwater Acute A. bahia promelas Freshwater Acute C. dubia
--------------------------------------------------------------------------------------------------------------------------------------------------------
Test type...................... Static non-renewal........... Static non-renewal.......... Static non-renewal.......... Static non-renewal.
Test duration.................. 96 hours..................... 48 hours.................... 96 hours.................... 48 hours.
Salinity....................... 20 2[permil].... 20 2[permil]... NA.......................... NA.
------------------------------------------------------------------------------------------------------------------------
Temperature.................... 25 1 [deg]C. Test temperatures must not deviate (maximum minus minimum temperature) by more than 3 [deg]C
during the test.
------------------------------------------------------------------------------------------------------------------------
Light quality.................. Ambient laboratory illumination
------------------------------------------------------------------------------------------------------------------------
Light intensity................ 10-20 [mu]E/m\2\/s
------------------------------------------------------------------------------------------------------------------------
Photoperiod.................... 16 h light, 8 h darkness, with phase in/out period recommended
------------------------------------------------------------------------------------------------------------------------
Test chamber size \1\.......... 250 mL....................... 250 mL...................... 250 mL...................... 30 mL.
Test solution volume \1\....... 200 mL....................... 200 mL...................... 200 mL...................... 15 mL.
Age of test organism \2\....... 9-14 days.................... 1-5 days.................... 1-14 days................... <24 hours.
No. organisms per test chamber. 10........................... 10.......................... 10.......................... 5.
No. of replicate chambers per 3............................ 3........................... 3........................... 4.
concentration (minimum).
------------------------------------------------------------------------------------------------------------------------
Feeding regime................. Refer to specific feeding procedures provided in each test method
------------------------------------------------------------------------------------------------------------------------
Aeration....................... None, unless DO falls below 4.0 mg/L, then aerate all chambers. Rate: <100 bubbles/minute
------------------------------------------------------------------------------------------------------------------------
Test concentrations............ 5 exposure concentrations and a control (minimum required)
------------------------------------------------------------------------------------------------------------------------
Test acceptability (required).. >=90% survival in controls
------------------------------------------------------------------------------------------------------------------------
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ Recommended minimum value.
\2\ Less than or equal to 24-hr range in age.

4.8 References for Section 4

5.0 Bioremediation Agent Efficacy Test Protocol

5.1 Summary. This protocol quantifies changes in weathered
Alaska North Slope (ANS) crude oil composition of alkanes and
aromatics resulting from the use of a bioremediation agent in either
artificial seawater or freshwater. The manufacturer may test either
one or both freshwater or saltwater, depending on the product's
intended use. Biodegradation of the alkanes and aromatics is
monitored for 28 days at 20-23 [deg]C. Product flasks at Day 28 are
compared to Day 0 flasks to determine reductions in alkanes and
aromatics. A positive control of a known oil-degrading bacterial
culture supplied by EPA is tested. A negative, sterile control is
also set up containing exposure water, weathered crude oil, product,
and a sterilant, sodium azide. The purpose of the negative, killed
control is to make sure the disappearance of the oil constituents at
day 28 is due to biodegradation and not some physical loss such as
volatilization. The day 28 GC/MS results from the killed control
must not be less than 90% of the day 0 results. The sample
preparation procedure extracts the oil phase into the solvent
dichloromethane (DCM) (also known as methylene chloride) with a
subsequent solvent exchange into hexane. The hexane extracts are
analyzed by a high resolution gas chromatograph/mass spectrometer
(GC/MS) operated in the selected ion monitoring mode (SIM) at a scan
rate of >5 scans per second. Note to 5.1: Artificially distilled at
521[emsp14][deg]F (272 [deg]C) to remove the low molecular weight
hydrocarbons to approximate natural weathering processes that occur
after a spill.

5.2 Apparatus. All equipment must be maintained and calibrated per
standard laboratory procedures.

5.2.1 Assorted flasks and other glassware;
5.2.2 Graduated cylinders (100 mL);
5.2.3 Deionized water; 250 mL borosilicate glass Erlenmeyer
flasks;
5.2.4 Pasteur pipettes;
5.2.5 Multichannel pipettor (5-50 mL and 50-200 mL);
5.2.6 Autoclave; environmental room or incubator;
5.2.7 Balance accurate to 0.1 mg;
5.2.8 Orbital shaker table with clamps sized to hold flasks
securely;
5.2.9 GC/MS instrument equipped with a DB-5 capillary column (30
m, 0.25 mm ID, and 0.25 mm film thickness) or equivalent, and a
split/splitless injection port operating in the splitless mode, such
as a Agilent 6890 GC/5973 MS (or equivalent) equipped with an auto-
sampler for testing multiple samples; and
5.2.10 Fixed Rotor Centrifuge.

5.3 Reagents and Culture Medium

5.3.1 Stock Seawater Preparation. Prepare the artificial
seawater GP2 (Spotte et al., 1984) following the procedures in
section 2.3 of this Appendix, to obtain the final concentration of
the salts listed in Table 1 of this Appendix, except for the sodium
bicarbonate (NaHCO3) which is prepared separately.
Autoclave the artificial seawater. Filter sterilize the concentrated
solution of sodium bicarbonate through a 0.45 [mu]m membrane filter
and add to the autoclaved and cooled artificial seawater GP2 to
obtain the final concentration listed in Table 1 of this Appendix.
5.3.2 Seawater for the positive control flasks. Prepare sodium
triphosphate (a.k.a.,

[[Page 3439]]

sodium tripolyphosphate)
(Na5P3O10), potassium nitrate
(KNO3), and ferric chloride hexahydrate (FeCl3
[middot] 6H2O) as a concentrated solution. Filter
sterilize through a 0.45 [mu]m membrane filter and add to autoclaved
artificial seawater to obtain the final nutrient concentrations
listed in Table 10 of this Appendix. Calibrate the pH meter at room
temperature (approximately 20-23 [deg]C) using commercial buffers of
pH 4.0, 7.0, and 10.0, as appropriate, prior to use. Adjust the pH
of the artificial seawater with concentrated hydrochloric acid (HCl)
or 10 normality sodium hydroxide (10 N NaOH), as appropriate.

Table 10--Artificial Seawater Nutrient Concentrations
------------------------------------------------------------------------
Final
Constituent concentration,
g/L
------------------------------------------------------------------------
* FeCl3 [middot] 6H2O................................... 0.050
KNO3.................................................... 2.890
* Na5P3O10.............................................. 0.297
------------------------------------------------------------------------
* Added aseptically after the GP2 has been autoclaved to limit
phosphorus and iron precipitation.

5.3.3 Seawater for bioremediation agents that do not include
nutrients. If a bioremediation agent contains living microorganisms
but not nutrients (or limiting concentrations of nutrients), then
nutrients may be added by the manufacturer. However, the total
concentration of the nutrients added to the bioremediation agent
must not exceed the final concentrations listed in Table 11 of this
Appendix.

Table 11--Artificial Seawater Nutrient Concentrations for Bioremediation
Agents Having No Nutrients Included
------------------------------------------------------------------------
Final
Constituent concentration,
g/L
------------------------------------------------------------------------
as Iron (Fe)............................................ 0.010
as Nitrogen (N)......................................... 0.400
as Phosphorus (P)....................................... 0.075
------------------------------------------------------------------------

If nutrients are supplied by the product manufacturer, the
specific composition and concentration used in the efficacy testing
must be submitted.
5.3.4 Freshwater Preparation. The artificial freshwater, which
is a modification of Bushnell-Haas medium (Haines et al., 2005), is
prepared following the concentrations listed in Table 12 of this
Appendix and then autoclaved. The pH is adjusted to 7.4 before
autoclaving. Constituents removed from the original formulation are
KNO3, K2HPO4 and KH2PO4.

Table 12--Constituent Concentrations for Artificial Freshwater
[Bushnell-Haas]
------------------------------------------------------------------------
Final
Constituent concentration
(mg/L)
------------------------------------------------------------------------
MgSO4 [middot] 7H2O..................................... 200
CaCl2 [middot] 2H2O..................................... 20
FeCl3 [middot] 6H2O..................................... 50
MnSO4 [middot] H2O...................................... 0.0302
H3BO3................................................... 0.0572
ZnSO4 [middot] 7H2O..................................... 0.0428
(NH4)6Mo7O2............................................. 0.0347
------------------------------------------------------------------------

5.3.5 Freshwater for the positive control. To prepare the
freshwater for the positive controls, prepare the nutrients
potassium phosphate monobasic (KH2PO4),
potassium phosphate dibasic (K2HPO4) and
potassium nitrate (KNO3) as a concentrated solution.
Filter sterilize and add to autoclaved artificial freshwater to
obtain the final concentrations given in Table 13 of this Appendix.
Calibrate the pH meter at room temperature (approximately 20-23
[deg]C) using commercial buffers of pH 4.0, 7.0, and 10.0, as
appropriate, prior to use. Adjust the pH of the artificial
freshwater to 7.4 with 1 N HCl or 1 N NaOH, as appropriate.

Table 13--Freshwater Nutrient Concentrations
------------------------------------------------------------------------
Final
Constituent concentration
(g/L) \1\
------------------------------------------------------------------------
KNO3.................................................... 2.89
KH2PO4.................................................. 1.00
K2HPO4.................................................. 1.00
------------------------------------------------------------------------
\1\ Adjust pH to 7.4 prior to autoclaving

5.3.6 Freshwater for bioremediation agents that contain living
microorganisms but not nutrients or limiting concentrations of
nutrients. If a bioremediation agent does not include nutrients,
then nutrients may be added. However, the total concentration of the
nutrients added to the bioremediation agent must not exceed the
final concentrations provided in Table 14 of this Appendix.

Table 14--Artificial Freshwater Nutrient Concentrations for
Bioremediation Agents Having No Nutrients Included
------------------------------------------------------------------------
Constituent Final concentration, g/L \1\
------------------------------------------------------------------------
as Iron (Fe)........................... not added since iron is already
in the freshwater solution.
as Nitrogen (N)........................ 0.400.
as Phosphorus (P)...................... 0.400.
------------------------------------------------------------------------
\1\ Adjust to pH 7.4 prior to autoclaving.

If nutrients are supplied by the product vendor, the specific
composition and concentration used in the efficacy testing must be
submitted.
5.3.7 Oil Preparation. The test oil, weathered ANS521 crude oil,
can be obtained from EPA at no charge (except for a minimal shipping
fee). See http://www.epa.gov/emergencies/content/ncp/index.htm for
more information.
5.3.8 Sodium azide sterilant. Prepare a stock solution of
NaN3 for addition to the negative killed control. The
final concentration in the killed controls will be 0.5 g/L.

5.4 Experimental Setup and Procedure

5.4.1 Autoclave clean borosilicate glass Erlenmeyer flasks (250
mL) for 20 minutes at 121 [deg]C at 15 psig.
5.4.2 Label flasks with the appropriate code (negative control,
positive control, or product; day to be sampled (0 or 28); letter
indicating replicate number) to reflect the following treatment
design in Table 15 of this Appendix:

Table 15--Bioremediation Efficacy Test--Summary of Experimental Setup
------------------------------------------------------------------------
Number of replicates at
sampling times
Treatment -------------------------- Analysis
Day 0 Day 28
------------------------------------------------------------------------
Negative (killed) Control (oil 0 3 GC/MS
+ exposure water + product +
EPA culture + NaN3 sterilant).
*Positive control (oil + 6 6 GC/MS
exposure water + nutrients +
EPA culture).
Test Type 1: Product 6 6 GC/MS
containing living
microorganisms (oil +
exposure water + living
product + supplemented
nutrients (if necessary)).
Test Type 2: Product 6 6 GC/MS
containing proprietary
nutrients but no live
microorganisms (oil +
exposure water + product +
EPA culture).
Test Type 3: Product (such as 6 6 GC/MS
an enzyme) containing no live
microorganisms and no
nutrients (oil + exposure
water + product).
------------------------------------------------------------------------
* The laboratory must report positive control test results conducted
within the year of any test results for bioremediation products, for
one or both types of water as applicable.

[[Page 3440]]

5.4.3 Aseptically dispense 100 mL of pre-sterilized artificial
exposure water (seawater or freshwater) into each flask. For the
positive control flasks, use exposure water containing nutrients.
Alternatively, the artificial exposure water can be dispensed into
clean flasks and then autoclaved.
5.4.4 Tare the labeled flasks containing exposure water and
other additions, as necessary, on the balance with a minimum
accuracy of 0.01 g. Add drop-wise 0.50 g oil (this results in a
final oil concentration of 5 g/L) using a sterile Pasteur pipette to
the center of the flask taking care to avoid splashing the oil onto
the sides of the flasks. Record the precise weight. ANS521 may be
previously warmed in a hot water bath to facilitate its flow. Take
precautions when handling and charging the flasks to minimize the
likelihood of contamination by exogenous microbes, including using a
new sterile pipette for each series of flasks.
5.4.5 Preparation of the EPA culture for both the positive
control flasks and the flasks containing non-living bio-stimulation
products. Use two vials containing approximately 5 mL of the known
EPA culture frozen in glycerol. Thaw both vials at room temperature,
transfer the contents of both thawed vials to a single sterile
centrifuge tube, rinse tubes with two volumes each of sterile
exposure water, centrifuge at between 6,000 and 7,000 xs gravity
(6,000-7,000 x g) for 15 minutes using a fixed rotor to fully pellet
the cells.
5.4.6 Positive control flasks contain exposure water, oil,
nutrients, and the EPA culture.
5.4.7 Negative killed control flasks for all products shall
contain exposure water, oil, product, the EPA culture for products
not containing a living culture, and the sodium azide sterilant at a
final concentration of 0.5 g/L. Add the sodium azide sterilant prior
to adding any product or EPA culture. For the negative killed
control flasks and product flasks, prepare and add the product to
the flasks in a concentration specified by the manufacturer or
vendor.
5.4.8 For non-living products that contain nutrient only, use
the EPA culture as the inoculum.
5.4.9 For other non-living products (e.g., enzymes), do not add
nutrients or the EPA culture as the inoculum as they are not needed.
5.4.10 For products containing microbial cultures, prepare 6
flasks the same way as in Steps a-d, but without the EPA culture. A
product that contains its own nutrients must not be amended with
nutrients, unless the product contains insufficient nutrients. Since
this is a closed flask test, nutrients could be limiting if they are
at the same concentration as used in the field. This could cause the
product to fail the test. Thus, the manufacturer has the option to
supplement its product with a higher concentration of nutrients than
that contained in the product. Any nutrient supplements to a product
must be reported and must not exceed the concentration limits in
Table 10 (for seawater) and 13 (for freshwater) of this Appendix, as
applicable.
5.4.11 Cap all flasks either with cotton stoppers or loosely
applied aluminum foil to allow gas exchange with the atmosphere. Set
aside the T=0 flasks for immediate extraction and analysis. Place
the rest of the flasks onto the orbital shaker table. Do not tip the
flasks excessively to avoid stranding oil above the mixing area of
the flask. Set the orbital shaker to 200 rpm and shake the flasks
for 28 days at 20-23 [deg]C.
5.4.12 Submit all information on added cultures and nutrients
for testing in the data report.

5.5 Sampling and Chemical Analysis

5.5.1 Summary. At each sampling event (Days 0 and 28), product
and control flasks are sacrificed for analysis of residual oil
concentrations (SOP 4 of this Appendix). Record all physical
observations for each flask (such as degree of emulsification,
whether the oil has congealed into tar balls, wall growth, color,
etc.) at each sampling. The analytical procedure is summarized in
Table 16 of this Appendix. Dichloromethane (DCM) is the solvent used
for the initial extraction. Solvent-exchange the extract into hexane
prior to injection into the gas chromatograph. The solvent exchange
is done to prevent asphaltenes from contaminating the column.

Table 16--Bioremediation Efficacy--Summary of Analytical Procedures
----------------------------------------------------------------------------------------------------------------
Sample
Sampling/ Analysis container/ Preservation/
Matrix Measurement measurement method quantity of storage Holding times
method sample
----------------------------------------------------------------------------------------------------------------
DCM........... N/A............. Solvent Exchange N/A.......... Capped Vial 4 [deg]C..... 6 months.
to Hexane. with Teflon
septa, 30 mL.
Hexane........ Hydrocarbon SOP 4........... GC/MS........ Capped Vial 4 [deg]C..... 6 months.
Concentration. with Teflon
septa, 10 mL.
----------------------------------------------------------------------------------------------------------------

5.5.2 Hydrocarbon Extraction. To measure extraction efficiency,
500 mL of the surrogate recovery standard (compounds and
concentrations described in SOP 1 in this Appendix) is added to each
flask. Add 50 mL DCM to each flask. Use magnetic stir bars to stir
the flasks for 20 minutes to transfer the oil into the DCM phase.
Allow the flasks to stand one hour for phase separation. If an
emulsion remains after one hour, centrifuge the emulsion in
Teflon[supreg] centrifuge tubes for at least ten minutes in a low
speed centrifuge at 3,000 x gravity (3,000 x g) to break the
emulsion and recover the DCM phase. Pass the DCM extract through a
funnel plugged with glass wool and containing approximately 20 g
anhydrous, granular sodium sulfate (Na2SO4) to
remove water. Collect the extract in 30 mL serum vials, capped with
Teflon lined septa and aluminum crimp seals, and store at 4 [deg]C
for up to 6 months.
5.5.3 Solvent Exchange. Perform a solvent exchange (DCM to
hexane) prior to GC/MS analysis to prevent injection of asphaltenes
into the GC/MS column. Using a Class A volumetric pipette,
transfer10 mL of DCM extract to 16 x 125 mm test tubes with Teflon
lined screw caps. Place the test tubes in a 37 [deg]C water bath
under a stream of dry nitrogen gas. Reduce the sample to 1 mL and
return to volume with hexane. Repeat the blow down and re-suspension
twice to exchange the hydrocarbons from DCM into the hexane.
5.5.4 Hydrocarbon Analysis. Quantify the concentrations of 25
alkanes (including hopane) and 31 aromatics (SOP 4, Table SOP 4.1 of
this Appendix) using an Agilent 6890 GC/5973 MS or equivalent
equipped with a 30-m x 0.25-mm ID x 0.25-[mu]m film thickness DB-5
or equivalent fused silica column. To prepare the samples, transfer
1.0 mL of the hexane extract into a 2 mL autosampler vial with
Teflon lined cap. Add 20 [mu]L of internal standard solution to each
vial with a syringe or positive displacement pipettor. SOP 2 of this
Appendix outlines the procedure for preparing the internal standard
solution. Load vials onto the autosampler tray and analyze in
selected ion monitoring mode (SIM). Sum the individual alkane
concentrations for the total alkane concentration and the individual
aromatic concentrations for total aromatic concentrations in each
flask.

5.6 Quality Assurance/Quality Control (QA/QC)

5.6.1 Objectives. The critical variables to be analyzed for each
set of experimental conditions are the individual petroleum
hydrocarbons, i.e., the alkanes ranging in carbon number from nC-14
to nC-35, plus pristane and phytane, and the 2- to 4-ring polycyclic
aromatic hydrocarbons (PAHs) and their alkylated homologs as listed
in SOP 4 of this Appendix. The quality assurance objectives for
precision, accuracy, and detection limits are 20%, 75-
125% recovery, and 22.5 [mu]g/L, respectively. For more details,
refer to the SOPs of this Appendix.
5.6.2 Precision Objectives. Precision is presented as relative
percent difference (RPD) for duplicate measurements and as relative
standard deviation (RSD, or coefficient of variance) for triplicate
measurements, applicable to replication of treatments as separate
samples.
5.6.3 Accuracy Objectives. These are based on the check
standards and standard oil samples run concurrently with the sample
analyses for GC/MS analysis of critical

[[Page 3441]]

compounds. Critical compounds in the check standards and in the oil
standards must fall within 75-125% of expected values for the
analysis to be valid. Six surrogate compounds (SOP 1 of this
Appendix) added to each sample before extraction can also serve as a
surrogate for determining accuracy. The measured surrogate
concentrations must fall within 75-125% of expected values.
5.6.4 Calibration Range. Conduct all measurements within the
linear calibration range of the instrument. The calibrated
concentration range for GC/MS analysis is 1 mg/L to 30 mg/L. If the
measured concentration of any critical compound is above the
calibration range, dilute the sample and re-analyze to quantify that
particular compound within the linear calibration range.
5.6.5 Quality Control. Table 17 of this Appendix summarizes the
QC checks for each measurement. See the corresponding SOP in this
Appendix for detailed descriptions of QC checks, frequency,
acceptance criteria, and corrective actions.

Table 17--QA/QC Checks
----------------------------------------------------------------------------------------------------------------
Acceptance
Sample matrix Measurement QA/QC check Frequency criteria Corrective action
----------------------------------------------------------------------------------------------------------------
DCM............. GC/MS hydrocarbon Blanks........... Once per Peak area of Flush with
analysis. calibrated run. interfering solvent, clean
peaks <10% of injection port,
lowest standard and/or bake
peak area. column.
DCM............. GC/MS hydrocarbon DFTPP Check Once per Must pass all If any criteria
analysis. Standard. calibrated run. DFTPP criteria. fail, retune and
rerun DFTPP
check standard.
DCM............. GC/MS hydrocarbon Initial Once per Response Factor If RSD for any
analysis. Calibration calibrated run. RSD <=25%. one compound
Samples. >25%,
recalibrate.
DCM............. GC/MS hydrocarbon Calibration Check Every 10-15 25% If >5 compounds
analysis. Standards. samples. of expected are out of
values. range,
recalibrate and
rerun samples.
Hexane.......... GC/MS hydrocarbon Surrogates....... Every Sample..... 30% Re-inject.
analysis. of expected
values.
Hexane.......... GC/MS hydrocarbon Biomarker Every Sample..... 25% Re-inject.
analysis. Concentration. of average
values.
----------------------------------------------------------------------------------------------------------------

5.7 Pass/Fail Criteria

5.7.1 Calculate the mean and standard deviation of the hopane-
normalized total aromatics (sum of all resolved aromatics) and
hopane-normalized total alkane concentrations (sum of all resolved
alkanes) from the 6 independent replicates at days 0 and 28. To
normalize, divide the sum of the alkane analytes and the sum of the
aromatic analytes in each replicate by the hopane concentration in
the corresponding replicate.
5.7.2 From those data, calculate the 95% Upper Confidence Level
(UCL95) at days 0 and 28 using the following formula
(Equation 11 of this Appendix):
[GRAPHIC] [TIFF OMITTED] TP22JA15.050

Where:

xt28 = total hopane-normalized alkane or total hopane-
normalized aromatic mean of 6 replicates at days 0 and 28,
t95, 5 df = the 95% one-tailed t-value with 5 degrees of
freedom (2.015),
[sigma] = the standard deviation of the 6 replicates at day 0 and
28, and
n = no. of replicates = 6.

5.7.3 Using Equation 12 of this Appendix, calculate the %
reduction of each oil fraction from day 0 to day 28, using the day 0
and 28 UCL95 hopane-normalized values for each fraction:
[GRAPHIC] [TIFF OMITTED] TP22JA15.051

Where:

t28(UCL95) = UCL95 of the hopane-normalized
total alkane or total aromatic mean of 6 replicates on day 28, and
t0(UCL95) = UCL95 of the hopane-normalized
total alkane or total aromatic mean of 6 replicates on day 0.

5.7.4 A product is successful in saltwater if the % reduction of
total alkanes (aliphatic fraction) from the GC/MS analysis is
greater than or equal to 95% and the % reduction of total aromatics
(aromatic fraction) is greater than or equal to 70% at day 28 based
on the UCL95 (Equation 12 of this Appendix). For
freshwater, a product is successful if the % reduction of total
alkanes and total aromatics is greater than or equal to 95% and 40%,
respectively. The benchmark reduction ranges in aliphatic and
aromatic fractions for the positive control are the same as for the
products specified above. The average concentration of the biomarker
hopane at day 28 must not differ from the average concentration at
day 0 by more than 12% in the positive control. If the conditions
for the positive control are not met, the entire procedure must be
repeated.
5.8 Data Verification and Reporting. GC/MS data files are
generated by MS ChemStation software (the Agilent standard software
for GC/MS) or equivalent for each injection. Data files contain
summed ion chromatograms and selected ion chromatograms. Calibration
curves are generated within MS ChemStation software, and all data
files are calculated against the calibration curve by MS
ChemStation. Data verification would be done by crosschecking
between analysts for 10% of the raw data and its reduction process.

[[Page 3442]]

5.9 Laboratory Report. The summary of findings from a product
test must include the data listings for each analyte that was
analyzed (i.e., all individual alkanes and aromatics in the list of
required analytes). Express all concentrations as mg analyte/L
exposure water.

5.10 Standard Operating Procedures (SOPs) 1-4

5.10.1 SOP 1. Preparation of Surrogate Recovery Standards
5.10.1.1 Preparation:
5.10.1.1.1 Solvents: Dichloromethane (DCM), Optima (Fisher)
grade or equivalent.
5.10.1.1.2 Reagents: D36-Heptadecane (C17), D50-Tetracosane
(C24), D66-Dotriacontane (C32), D10-1-Methylnaphthalene, D10-
Phenanthrene, D10-Pyrene, 5-beta-cholestane (coprostane).
Note: Deuterated reagents are available from Cambridge Isotope
Laboratories, Andover, MA.
5.10.1.1.3 Equipment: Micro-spatula, Small beakers, Glass
funnel, Analytical balance (0.0001g), Vials with Teflon-lined caps,
Teflon wash bottle with Optima grade DCM, Volumetric flask (250 mL),
class A, Pasteur pipettes.
5.10.1.2 Procedure:
5.10.1.2.1 Using a calibrated analytical balance, weigh 100 mg
(0.100 g) of each reagent into separate 10-25 mL beakers.
5.10.1.2.2 Dissolve the reagents in their beakers by adding 10
mL DCM. Use a Pasteur pipette to transfer the solutions to a single
250 mL volumetric flask.
5.10.1.2.3 Wash the beakers 3 or 4 times with DCM. Use a Pasteur
pipette to transfer each of the washings to the 250 mL volumetric
flask.
5.10.1.2.4 Dilute the solution to the 250 mL volume mark on the
volumetric flask with DCM.
5.10.1.2.5 Use a glass stopper to seal the flask and homogenize
the solution by inverting the flask 5 or more times. The final
concentration of this solution is 400 mg/L for each of the reagents.
5.10.1.2.6 Transfer the solution into 40 mL storage vials and
cap with Teflon-lined caps and label each with the date of
preparation, operator, sample names, and concentrations.
5.10.1.2.7 Weigh each vial and record its weight on the label.
This weight is used to monitor possible evaporation during storage.
5.10.1.2.8 Store these vials at 0 [deg]C or lower.
5.10.1.2.9 Before using, allow the solution to come to room
temperature, and then shake it well.
5.10.1.2.10 Weigh the vial before using it, and compare the
weight with the last weight recorded on the vial.
5.10.1.2.11 If the weights are consistent, the integrity of the
solution can be assumed. If not, investigate and resolve the cause.
Prepare a new solution if the integrity has been compromised.
5.10.1.3 Quality Control: Inject 20 [mu]L of the surrogate stock
solution into 1 mL DCM. Add 20 [mu]L of the internal standard
solution (SOP 2 of this Appendix). Analyze this solution by GC/MS
using a calibrated method (SOPs 3 and 4 of this Appendix). The
expected concentration of each of the corresponding surrogate
compounds is 8 2 mg/L. If the measured value does not
fall within this range, prepare and measure another independent
surrogate solution. If the measured concentration of the second
surrogate solution is within the allowable tolerance range, the
calibration and instrument conditions are acceptable; properly
discard the first surrogate solution. If the concentration of the
second surrogate solution is also out of range, then clean and
recalibrate the instrument until the problem is resolved.
5.10.2 SOP 2. Preparation of Internal Standard Solution

5.10.2.1 Preparation

5.10.2.1.1 Solvents: Dichloromethane (DCM), Optima (Fisher)
grade or equivalent.
5.10.2.1.2 Reagents: D34 n-Hexadecane (C16), D42 n-Eicosane
(C20), D62 n-Triacontane (C30), D8-Naphthalene, D10-Anthracene, D12-
Chrysene, 5-alpha-Androstane.
Note: Deuterated reagents are available from Cambridge Isotope
Laboratories, Andover, MA.
5.10.2.1.3 Equipment: Micro-spatula, Small beakers, Glass
funnel, Analytical balance (0.0001g), calibrated and checked for
accuracy, Amber vials with Teflon-lined caps, labeled, Teflon wash
bottle with DCM, Volumetric flask (200 mL), class A, Pasteur
pipettes.
5.10.2.2 Procedure:
5.10.2.2.1 Using a calibrated analytical balance, weigh 100 mg
(0.100 g) of each of the reagents into separate small beakers.
5.10.2.2.2 Dissolve the reagents in their beakers by adding 10
mL DCM; using a Pasteur pipette, transfer the solutions to a single
200 mL volumetric flask.
5.10.2.2.3 Wash the beakers 3 or 4 times with DCM; use a Pasteur
pipette to transfer each of the washings to the 200 mL volume mark
on the volumetric flask.
5.10.2.2.4 Dilute the solution with DCM to the 200 mL volume.
5.10.2.2.5 Seal the flask with a glass stopper and homogenize
the solution by inverting the flask a minimum of 5 times. The final
concentration of this solution is 500 mg/L of each reagent.
5.10.2.2.6 Transfer the solution into 40 mL storage vials and
cap with Teflon-lined caps. Label each vial with the date of
preparation, operator, sample names, and concentrations.
5.10.2.2.7 Weigh each vial, and record its weight on the label.
This weight is used to monitor possible evaporation during storage.
5.10.2.2.8 Store this solution at 0 [deg]C or lower.
5.10.2.2.9 Before using, allow the solution to come to room
temperature, and then shake it well.
5.10.2.2.10 Weigh the vial before using it, and compare the
weight with the last weight recorded on the vial.
5.10.2.2.11 If the weights are consistent, the integrity of the
solution can be assumed. If not, investigate and resolve the cause.
Prepare a new solution if the integrity has been compromised.
5.10.2.3 Quality Control: Inject 20 [mu]L of the internal
standard solution into 1 mL DCM. Analyze this solution by GC/MS. The
only peaks corresponding to the internal standards must appear. If
other peaks appear, particularly close to the internal standard
peaks, discard the internal standard solution and prepare a new
solution.
5.10.3 SOP 3. Preparation of Working Standards, Check Standards,
and Oil Standards for GC/MS Consistency.
5.10.3.1 Preparation:
5.10.3.1.1 Solvent: Dichloromethane (DCM), Optima (Fisher) grade
or equivalent.
5.10.3.1.2 Stock solutions:
5.10.3.1.2.1 Oil analysis standard: 44 compounds, 100 mg/L in
hexane/DCM (9:1), four, 1-mL vials required. Available from Absolute
Standards, Inc., Hamden, CT, Part # 90311.
5.10.3.1.2.2 Nine compound PAH standard: 1,000 mg/L in DCM, one
vial. Available from Absolute Standards, Inc., Hamden, CT, Part #
90822.
5.10.3.1.2.3 1,2-Benzodiphenylene sulfide, (synonym for
naphthobenzothiophene). Prepare a 2 mg/mL stock solution. Available
from Sigma-Aldrich Co., Part # 255122, purity 99%.
5.10.3.1.2.4 Hopane solution (17 [beta] (H), 21[beta] (H), 0.1
mg/mL in isooctane. Available from Sigma-Aldrich Co. Part # 07562.
5.10.3.1.2.5 Surrogate solution: 400 mg/L of each reagent in DCM
(see SOP 1 of this Appendix).
5.10.3.1.2.6 Internal standard solution, 500 mg/L in DCM (see
SOP 2 of this Appendix).
5.10.3.1.3 Alaska North Slope Crude Oil 521 (ANS521).
5.10.3.1.4 Equipment:
5.10.3.1.4.1 Glass storage vials with Teflon-lined caps (2 mL
and 40 mL capacity);
5.10.3.1.4.2 Volumetric flasks, Class A, 5 mL, 10 mL, and 100
mL.
5.10.3.1.4.3 Glass syringes capable of dispensing 25-500 mL with
an accuracy and precision of 1%, or equivalent.
5.10.3.1.4.4 Wheaton repetitive dispenser, Model 411 STEP-PETTE
or equivalent.
5.10.3.1.4.5 Teflon wash bottle filled with Optima grade DCM or
equivalent grade DCM.
5.10.3.1.4.6 Pasteur pipettes.
The volumes of stock solutions required to make the working
standards are listed in Table SOP 3.1 of this Appendix.

[[Page 3443]]

Table SOP 3.1--Amount of Stock Solutions Required To Make the Working Standards
--------------------------------------------------------------------------------------------------------------------------------------------------------
Stock standards A B C D E F
--------------------------------------------------------------------------------------------------------------------------------------------------------
Oil
Analysis Aromatics 1,2-Benzo- Surrogate Hopane
Mix (44 Mix (9 diphenylene solution solution ISTD (500
Working standards concentration, mg/L compounds, compounds, sulfide (100 mg/L) (100 mg/L) Volumetric Flask Volume mL mg/L)
100 mg/L) 1000 mg/L) (NBT) (2 mg/ [mu]L [mu]L [mu]L
[mu]L [mu]L mL) [mu]L
--------------------------------------------------------------------------------------------------------------------------------------------------------
STD 30 (no hopane)........................ 1500 150 75 375 0 5............................. 100
STD 20 (5 mg/L hopane).................... 1000 100 50 250 250 5............................. 100
STD 10 (2.5 mg/L hopane).................. 500 50 25 125 125 5............................. 100
STD 5 * (1 mg/L hopane)................... 500 50 25 125 100 10............................ 200
STD 5-Utility (1 mg/L hopane)............. 500 50 25 125 100 10 (used for preparation of 0
STD 2.5 & STD 1).
----------------------------------------------------------------- ------------
STD 2.5 (0.5 mg/L hopane)................. Use 5 mL of STD 5-Utility and dilute to 10 mL 200
STD 1 (0.2 mg/L hopane)................... Use 2 mL of STD 5-Utility and dilute to 10 mL 200
--------------------------------------------------------------------------------------------------------------------------------------------------------
* Make extra STD 5 for use as check standard.

5.10.3.2 Procedure for Working Standards and Check Standards:
5.10.3.2.1 Label three 5 mL volumetric flasks as STD30, STD20,
STD10, and two 10 mL volumetric flasks as STD5, and STD5-utility.
5.10.3.2.2 Add 1-2 mL of DCM to each volumetric flask.
5.10.3.2.3 Using glass syringes, add the appropriate volume of
stock solution A (as listed in Table SOP 3.1 of this Appendix) to
the flasks labeled STD30, STD20, STD10, STD5, and STD5-utility.
5.10.3.2.4 Wash the walls of the inner neck of the flasks with
several drops of DCM to rinse off the residue of the stock solution
into the flasks.
5.10.3.2.5 Repeat Step 3 and Step 4 to dispense stock solutions
B-E (do not add stock solution F, internal standard solution, at
this step).
5.10.3.2.6 Dilute to volume with DCM for all the above flasks,
seal with glass stoppers, and invert several times to homogenize the
solutions.
5.10.3.2.7 Label two additional 10 mL volumetric flasks as
STD2.5 and STD1. Wet with 1-2 mL DCM.
5.10.3.2.8 Dispense 5 mL of STD5-utility solution into flask
STD2.5, and 2 mL of STD5-utility solution into flask STD1.
5.10.3.2.9 Dilute to volume with DCM, seal with glass stoppers,
and invert several times to homogenize the solutions.
5.10.3.2.10 Using a 100 [mu]L glass syringe, dispense 100 [mu]L
of internal standard solution into flasks STD30, STD20, and STD10.
Dispense 200 [mu]L into flasks STD5, STD2.5, and STD1 to give a
final concentration of 10 mg/L internal standard.
5.10.3.2.11 Seal with glass stoppers, and invert the flasks
several times to homogenize the solutions.
5.10.3.2.12 Transfer the solutions into 2 mL storage vials, and
cap with Teflon-lined caps.
5.10.3.2.13 Label each vial with date of preparation, analyst,
sample names, and concentrations.
5.10.3.2.14 Weigh each storage vial and record its weight on the
label. This weight is used to monitor possible evaporation during
storage.
5.10.3.2.15 Store this solution at 0 [deg]C or below.
5.10.3.2.16 Before using, allow the solution to come to room
temperature, and shake it well.
5.10.3.2.17 Weigh the vial before opening, and compare the
weight with the last weight recorded on the vial. If the weights are
consistent, the integrity of the solution can be assumed. If not,
investigate and resolve the cause. Do not use the solution if the
integrity has been compromised.
5.10.3.3 Procedure for Oil Standard. In a 100 mL volumetric
flask, weigh 0.500 g of the standard ANS521 crude oil, add 2 mL of
surrogate solution (see SOP 1 of this Appendix), and bring to volume
with DCM. Add 2 mL of internal standard solution (see SOP 2 of this
Appendix). Follow steps 5.10.3.2.11 through 5.10.3.2.17 of this SOP,
substituting 40 mL storage vials for the 2 mL vials.
5.10.3.4 Quality Control/Quality Assurance:
5.10.3.4.1 Run the six standard solutions using the GC/MS method
(SOP 4) on a tuned GC/MS. Use the EnviroQuant software or equivalent
to calculate the average Relative Response Factor (RRF) and the
relative standard deviation (RSD) of the RRFs for each analyte over
the six concentrations. The RRF is defined as:
[GRAPHIC] [TIFF OMITTED] TP22JA15.052

5.10.3.4.2 The RSD of the RRFs for all analytes must be 25% or
less according to EPA Method 525.2.
5.10.4 SOP 4. GC/MS Method for the Analysis of Crude Oil
Samples.
5.10.4.1 Instrument Specifications:
5.10.4.1.1 Use an Agilent 6890 GC coupled with an Agilent 5973
mass selective detector (MSD) and an Agilent 6890 series auto
sampler or equivalent, equipped with a DB-5 capillary column (30 m,
0.25 mm I.D., and 0.25 [mu]m film thickness) or equivalent, and a
split/splitless injection port operating in the splitless mode. Data
acquisition occurs either in the SIM (selected ion monitoring) mode
for quantitative analysis or in SCAN mode for qualitative analysis.
In SIM mode, the dwell time of each ion is set to be 10 milliseconds
and the ions are split up into groups by retention time. One way to
divide the ions is by retention time grouping as shown in Table SOP
4-1 of this Appendix. The number of ions in each ion group must be
constant, yielding the same scan rate for each group.

Table SOP 4-1--Ions Associated With Retention Time Groups
------------------------------------------------------------------------
Group Ions
------------------------------------------------------------------------
1................................. 57, 66, 128, 136, 142, 152, 156,
166, 170, 184
2................................. 57, 66, 166, 170, 178, 180, 184,
188, 192, 194, 198, 208
3................................. 57, 66, 178, 184, 188, 192, 194,
198, 202, 206, 208, 212, 220, 226

[[Page 3444]]

4................................. 57, 66, 192, 198, 202, 206, 208,
212, 216, 220, 226, 230, 234, 245
5................................. 57, 66, 191, 217, 228, 240, 242,
248, 256, 262, 264, 270, 276, 284
------------------------------------------------------------------------

5.10.4.1.2 Table SOP 4.2 of this Appendix summarizes the
instrumental conditions for crude oil analysis. Use only ultra-high
purity helium (99.999% pure) as the carrier gas. In series, connect
a moisture trap, an oxygen trap, and an organic trap to the carrier
gas line before it enters the column.

Table SOP 4.2--Instrumental Conditions for Crude Oil Analysis
------------------------------------------------------------------------

------------------------------------------------------------------------
Instrument................................ Agilent 6890 Series II Gas
Chromatograph (GC) with an
Agilent 5973MSD and an
Agilent 6890 auto sampler,
or equivalent.
Column.................................... DB-5 capillary column (30 m,
0.25 mm I.D., and 0.25-
[mu]m film thickness) or
equivalent.
Carrier Gas............................... Helium, ultra-high purity
grade (99.999%).
Inlet Temperature......................... 300 [deg]C.
Transfer Line (detector) Temperature...... 310 [deg]C.
Oven Temperature Program.................. 50 [deg]C for 4 minutes,
then 7 [deg]C/min to 310
[deg]C, hold for 18
minutes.
Flow Rate................................. Constant flow at 1mL/min.
Linear velocity: 36.2 cm/
sec.
Injection Volume.......................... 1 [mu]L.
Split/Splitless Mode...................... Splitless.
Total Run Time............................ 59.18 minutes.
------------------------------------------------------------------------

5.10.4.2 Procedure for preparing the instrument:
5.10.4.2.1 Lower the injection port temperature and the oven
temperature to 50 [deg]C or less to avoid oxidation of the column.
5.10.4.2.2 Replace the liner with a clean, silanized liner. Do
not touch the liner with bare fingers. A small piece of muffled
glass wool may be inserted to protect the column.
5.10.4.2.3 Return the injection port and oven to the appropriate
temperatures.
5.10.4.2.4 Wait five minutes after the temperature equilibrates
before using the instrument.
5.10.4.3 Procedure for tuning the MSD:
5.10.4.3.1 Perform an air/water check. The value reported for
the relative abundance of water (m/z 18), nitrogen (m/z 28), oxygen
(m/z 32), or carbon dioxide (m/z 44) shall be less than 5% of the
base peak for the system to be considered leak free.
5.10.4.3.2 Tune the MSD using the Standard Autotune program and
the decafluorotriphenylphosphine (DFTPP) Tune program to reduce
instrument variability. The Autotune report file is referenced by
the instrument when performing an air/water check and thus must be
run at least once per month. Run standards and samples using DFTPP
Tune parameters, and retune the instrument using DFTPP Tune at least
once per week. The tune programs use three fragment ions of
perfluorotributylamine (PFTBA) as a standard for tuning: m/z 69,
219, and 502. Tune reports must meet the following criteria:
5.10.4.3.2.1 Symmetrical peaks;
5.10.4.3.2.2 Mass assignments within 0.2 amu's from
69, 219, and 502;
5.10.4.3.2.3 Peak widths within 0.5 0.1 amu's;
5.10.4.3.2.4 Relative abundance is 100% for ion 69, at least 35%
for ion 219, and at least 1% for ion 502;
5.10.4.3.2.5 Relative abundances for isotope masses 70, 220, and
503 0.2 amu's are 0.5-1.5%, 2-8%, and 5-15%,
respectively; and
5.10.4.3.2.6 Air and water peaks at m/z = 18, 28, 32, and 44
amu's must be very small and consistent with historical values.
5.10.4.4 Maintaining a log book. Maintain an instrument logbook,
and make entries for each use. Include the following information in
the logbook: operator name, helium cylinder tank pressure and outlet
pressure, vacuum gauge reading, any maintenance performed on the
instrument (such as changing the injection port liner, gold seal,
guard column, source cleaning), sequence name, data path, samples in
order of injection, method information, GC column number, and the
Standard Auto Tune report and DFTPP Tune report.
5.10.4.5 Running a Solvent Blank: Following a liner change or at
the start of a new run, run an injection of a pure solvent to
confirm that the system is free of excessive or interfering
contamination. Analyze the solvent in SCAN mode using the same
temperature program used for sample analysis. If contamination is
present, analyze additional samples of fresh solvent until the
interfering contamination is removed.
5.10.4.6 Checking the DFTPP Tune: Prior to running the first
calibration standard, verify the instrument tune conditions by
running a 10 ng/[mu]L DFTPP check standard to check the mass
measuring accuracy of the MS, the resolution sensitivity, the
baseline threshold, and the ion abundance ranges. Run the standard
using the DFTPP method provided with the instrument. Each of the
criteria identified in Table SOP 4.2 of this Appendix must be met
before using the instrument for analysis:

Table SOP 4.3--Ion Abundance Criteria for DFTPP
----------------------------------------------------------------------------------------------------------------
Relative to
Mass, M/z mass Relative abundance criteria Purpose of checkpoint
----------------------------------------------------------------------------------------------------------------
51....................................... 442 10-80% of the base peak.... Low mass sensitivity.
68....................................... 69 <2% of mass 69............. Low mass resolution.
70....................................... 69 <2% of mass 69............. Low mass resolution.
127...................................... 442 10-80% of the base peak.... Low-mid mass sensitivity.
197...................................... 198 <2% of mass 198............ Mid mass resolution.
198...................................... 442 Base peak or >50% of 442... Mid mass resolution and
sensitivity.
199...................................... 198 5-9% of mass 198........... Mid mass resolution and
isotope ratio.
275...................................... 442 10-60% of the base peak.... Mid-high mass sensitivity.
365...................................... 442 >1% of the base peak....... Baseline threshold.
441...................................... 443 Present and < mass 443..... High mass resolution.
442...................................... 442 Base peak or >50% of 198... High mass resolution and
sensitivity.
443...................................... 442 15-24% of mass 442......... High mass resolution and
isotopic ratio.
----------------------------------------------------------------------------------------------------------------

5.10.4.7 Calibrating with a Multiple-Point Calibration Curve. A
5- or 6-point calibration curve is obtained by running 5 or 6
working standards (see SOP 3) on the tuned GC/MS instrument.
Calculate the relative response factor (RRF) for each compound
relative to its corresponding deuterated internal standard as
indicated in Table SOP 4.3 of this Appendix. The relative standard
deviation (RSD) of the RRFs for each compound must be less than 25%.
Run an independently prepared check standard immediately after the
calibration standards to validate the accuracy of the calibration
curve.
5.10.4.8 Running Samples. Once the calibration curve has been
validated, samples can be analyzed. Dispense 1,000 [mu]L of sample
extract into labeled auto-sampler vials. Add

[[Page 3445]]

20 [mu]L of the internal standard solution (see SOP 2 of this
Appendix) to the extract using a syringe or a positive displacement
pipettor. Run a check standard every 10 samples to ensure the
consistency of the instrument. The RRF for each compound in the
check standard must be within 25% of the average RRF obtained in the
initial calibration.
5.10.4.9 Quantification: Once a calibration table has been
generated, quantify each data file using the ``Calculate and
Generate'' function in the MS ChemStation software, or equivalent
software. Review individual peak integration manually to ensure
proper baseline integration. The quantification of a compound is
based on the peak area of the primary ion (Q Ion) indicated in Table
SOP 4.4 of this Appendix.

Table SOP 4.4--Target Compound List
----------------------------------------------------------------------------------------------------------------
Quantitation Reference compound for Internal standard for
Compound name ion response factor quantitation
----------------------------------------------------------------------------------------------------------------
N D34 C16............................... 66 N D34 C16................. D34 n C16 Q Ion 66.
n-C14................................... 57 n C14.....................
n-C15................................... 57 n C15.....................
n-C16................................... 57 n C16.....................
N D34 C17............................... 66 N D34 C17.................
n-C17................................... 57 n C17.....................
Pristane................................ 57 Pristane..................
n-C18................................... 57 n C18.....................
Phytane................................. 57 Phytane...................
n C19................................... 57 n C19.....................
N D42 C20............................... 66 N D42 C20................. D42 n C20 Q Ion 66.
n C20................................... 57 n C20.....................
n C21................................... 57 n C21.....................
n C22................................... 57 n C22.....................
n C23................................... 57 n C23.....................
N D50 C 24.............................. 66 N D50 C 24................
n C24................................... 57 n C24.....................
n C25................................... 57 n C25.....................
n C26................................... 57 n C26.....................
n C27................................... 57 n C27.....................
n C28................................... 57 n C28.....................
n C29................................... 57 n C29.....................
N D62 C30............................... 66 N D62 C30................. D62 n C30Q Ion 66.
n C30................................... 57 n C30.....................
n C31................................... 57 n C31.....................
N D66 C32............................... 57 N D66 C32.................
n C32................................... 57 n C32.....................
n C33................................... 57 n C33.....................
n C34................................... 57 n C34.....................
n C35................................... 57 n C35.....................
D8 Naphthalene.......................... 136 D8 Naphthalene............ D8 Naphthalene Q Ion 136.
Naphthalene............................. 128 Naphthalene...............
D10 1-Methylnaphthalene................. 152 D10 1-Methylnaphthalene...
C1 Naphthalene *........................ 142 C1 Naphthalene............
C2 Naphthalene *........................ 156 C2 Naphthalene............
C3 Naphthalene *........................ 170 C3 Naphthalene............
C4 Naphthalene *........................ 184 C3 Naphthalene............
D10 Anthracene.......................... 188 D10 Anthracene............ D10 Anthracene Q Ion 188.
D10 Phenanthrene........................ 188 D10 Phenanthrene..........
Phenanthrene............................ 178 Phenanthrene..............
C1 Phenanthrene *....................... 192 C1 Phenanthrene...........
C2 Phenanthrene *....................... 206 C2 Phenanthrene...........
C3 Phenanthrene *....................... 220 C2 Phenanthrene...........
C4 Phenanthrene *....................... 234 C2 Phenanthrene...........
Fluorene................................ 166 Fluorene..................
C1 Fluorene *........................... 180 Fluorene..................
C2 Fluorene *........................... 194 Fluorene..................
C3 Fluorene *........................... 208 Fluorene..................
Dibenzothiophene........................ 184 Dibenzothiophene..........
C1 Dibenzothiophene *................... 198 Dibenzothiophene..........
C2 Dibenzothiophene *................... 212 Dibenzothiophene..........
C3 Dibenzothiophene *................... 226 Dibenzothiophene..........
Naphthobenzothiophene (NBT)............. 234 Naphthobenzothiophene.....
C1 NBT *................................ 248 Naphthobenzothiophene.....
C2 NBT *................................ 262 Naphthobenzothiophene.....
C3 NBT *................................ 276 Naphthobenzothiophene.....
Fluoranthene............................ 202 Fluoranthene..............
D10 Pyrene.............................. 212 D10 Pyrene................
Pyrene.................................. 202 Pyrene....................
C1 Pyrene *............................. 216 Pyrene....................
C2 Pyrene *............................. 230 Pyrene....................
D12 Chrysene............................ 240 D12 Chrysene.............. D12 Chrysene Q Ion 240.
Benzo(a)anthracene/Chrysene *........... 228 Chrysene..................
C1 Chrysene *........................... 242 Chrysene..................

[[Page 3446]]

C2 Chrysene *........................... 256 Chrysene..................
C3 Chrysene *........................... 270 Chrysene..................
C4 Chrysene *........................... 284 Chrysene..................
5[alpha]-androstane..................... 245 5[alpha]-androstane....... 5[alpha]-androstane Q Ion
245
Coprostane.............................. 219 Coprostane................
Hopane.................................. 191 Hopane....................
----------------------------------------------------------------------------------------------------------------
* Summed compounds; draw an integration line underneath all peaks with selected ion.

5.10.4.10 Equation 14 of this Appendix is used to calculate the
concentration of analytes in units of [mu]g/g oil added:
[GRAPHIC] [TIFF OMITTED] TP22JA15.054

where:

Aanalyte = the peak area of the analyte,
Cistd = the concentration of the internal standard,
Aistd = the area of the internal standard,
RRF = the relative response factor, and
100 is the conversion factor to convert mg/L DCM to [mu]g/g oil
added.

5.10.4.11 If some analytes are not commercially available, the
RRFs of other compounds (usually the parent compound) are used to
quantify those analytes. For example, the RRF of C3-naphthalene may
be used to calculate the concentrations of C3- and C4-naphthalenes.
See Table SOP 4.4 of this Appendix for details. The quantification
of these alkylated PAHs is relative because it is assumed that the
molecular ions of the alkylated PAHs have the same RRFs as the
parent compound ions. Nevertheless, these relative concentrations
are useful for monitoring the fate of these compounds during the
course of any analysis, as long as their concentrations are measured
in a consistent way throughout the analysis.
5.10.4.12 Concentration calculations for all target compounds
are performed using EnviroQuant software or equivalent. Data for
each sample can be printed directly using a customized report
template. Data can also be automatically entered into a spreadsheet
within the EnviroQuant software.
5.10.5 Quality Assurance/Quality Control. The following criteria
must be met before any samples are analyzed:
5.10.5.1 Air/water check to verify the system is leak free.
5.10.5.2 AutoTune and DFTPP Tune pass all criteria.
5.10.5.3 DFTPP check standard passes all criteria.
5.10.5.4 Solvent blank scan indicates the GC/MS system is free
of interfering contamination.
5.10.5.5 Prepare and monitor a control chart of a standard oil
analysis. Concentrations of the analytes in the control chart must
be no more than 25% different from their historical averages.
5.10.5.6 Relative response factors for analytes in the check
standards inserted between every 10 samples must be no more than 25
percent different from the average RRF of those same analytes in the
calibration curve. Peak shapes must be symmetrical.

5.11 References for Section 5

(1) Haines, J.R., E.J. Kleiner, K.A. McClellan, K.M. Koran, E.L.
Holder, D.W. King, and A.D. Venosa. 2005. ``Laboratory evaluation of
oil spill bioremediation products in salt and freshwater systems.''
J. Ind. Microbiol. Biotech 32: 171-185.
Appendix E to Part 300 [Removed]
0
17. Remove Appendix E to Part 300.

[FR Doc. 2015-00544 Filed 1-21-15; 8:45 am]
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