[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]



[[Page 3379]]

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  

[[Page 3380]]


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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 ([email protected]) or Vanessa Principe at 202-564-
7913 ([email protected]). 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
                                       ---------------------------------
                                         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.
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    \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.
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    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 
SuiteTM, 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.
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    \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.
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     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.
---------------------------------------------------------------------------

    \41\ http://www.epa.gov/oppefed1/ecorisk_ders/toera_analysis_eco.htm#Ecotox.
---------------------------------------------------------------------------

    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.
---------------------------------------------------------------------------

    \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.
---------------------------------------------------------------------------

    \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.
---------------------------------------------------------------------------

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.
---------------------------------------------------------------------------

    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.
---------------------------------------------------------------------------

    \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.
---------------------------------------------------------------------------

    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.
---------------------------------------------------------------------------

    \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.
---------------------------------------------------------------------------

    \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.
---------------------------------------------------------------------------

    \59\ USEPA 2010. http://www.epa.gov/oppefed1/ecorisk_ders/toera_analysiseco.htm#Ecotox.
---------------------------------------------------------------------------

    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 [email protected], 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
------------------------------------------------------------------------

                                                             [GRAPHIC] [TIFF OMITTED] TP22JA15.053
                                                             

[[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

    (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).

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.

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