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ENVIRONMENTAL PROTECTION information to support agent information whose disclosure is AGENCY preauthorization or authorization of use restricted by statute. Certain other decisions. material, such as copyrighted material, 40 CFR Parts 110 and 300 DATES: Comments must be received on will be publicly available only in hard copy. Publicly available docket [EPA–HQ–OPA–2006–0090; FRL–9689–9– or before April 22, 2015. OSWER] ADDRESSES: Submit your comments, materials are available either identified by Docket ID No. EPA–HQ– electronically in http:// RIN 2050–AE87 OPA–2006–0090, by one of the www.regulations.gov or in hard copy at the EPA Docket, EPA/DC, EPA West, National Oil and Hazardous following methods: • Federal Rulemaking Portal: http:// Room 3334, 1301 Constitution Avenue Substances Pollution Contingency NW., Washington, DC. The Public Plan www.regulations.gov. Follow the on-line instructions for submitting comments. Reading Room is open from 8:30 a.m. to AGENCY: U.S. Environmental Protection • Mail: The mailing address of the 4:30 p.m., Monday through Friday, Agency (EPA). docket for this rulemaking is EPA excluding legal holidays. The telephone number for the Public Reading Room is ACTION: Proposed rule. Docket Center (EPA/DC), Docket ID No. EPA–HQ–OPA–2006–0090, 1200 202–566–1744 to make an appointment SUMMARY: The Environmental Protection Pennsylvania Avenue NW., Washington, to view the docket. Agency (EPA or the Agency) proposes to DC 20460. FOR FURTHER INFORMATION CONTACT: For amend the requirements in Subpart J of • Hand Delivery: Such deliveries are general information, contact the the National Oil and Hazardous only accepted during the Docket’s Superfund, TRI, EPCRA, RMP, and Oil Substances Pollution Contingency Plan normal hours of operation, and special Information Center at 800–424–9346 or (NCP) that govern the use of dispersants, arrangements should be made for TDD at 800–553–7672 (hearing other chemical and biological agents, deliveries of boxed information. impaired). In the Washington, DC and other spill mitigating substances Instructions: Direct your comments to metropolitan area, contact the when responding to oil discharges into Docket ID No. EPA–HQ–OPA–2006– Superfund, TRI, EPCRA, RMP, and Oil waters of the United States (U.S.). The 0090. EPA’s policy is that all comments Information Center at 703–412–9810 or proposal addresses the efficacy, toxicity, received will be included in the public TDD 703–412–3323. For more detailed environmental monitoring of docket without change and may be information on this proposed rule dispersants, and other chemical and made available online at http:// contact Gregory Wilson at 202–564– biological agents, as well as public, www.regulations.gov, including any 7989 ([email protected]) or state, local, and federal officials’ personal information provided, unless Vanessa Principe at 202–564–7913 concerns regarding their use. the comment includes information ([email protected]). The Specifically, the proposal amends the claimed to be Confidential Business contacts address is: U.S. Environmental Subpart J regulatory requirements for Information (CBI) or other information Protection Agency, Office of Emergency the NCP Product Schedule (Schedule) whose disclosure is restricted by statute. Management, Regulations by adding new listing criteria, revising Do not submit information that you Implementation Division, 1200 the efficacy and toxicity testing consider to be CBI or otherwise Pennsylvania Avenue NW., Washington, protocols, and clarifying the evaluation protected through DC 20460–0002, Mail Code 5104A, or criteria for removing products from the http://www.regulations.gov. The http:// visit the Office of Emergency Schedule. The Agency also proposes www.regulations.gov Web site is an Management Web site at http:// amended requirements for the ‘‘anonymous access’’ system, which www.epa.gov/oem/. authorities, notifications, monitoring, means EPA will not know your identity SUPPLEMENTARY INFORMATION: The and data reporting when using chemical or contact information unless you contents of this preamble are: or biological agents in response to oil provide it in the body of your comment. I. General Information discharges to the navigable waters of the If you submit an electronic comment, II. Entities Potentially Affected by This United States and adjoining shorelines, EPA recommends that you include your Proposed Rule the waters of the contiguous zone, and name and other contact information in III. Statutory Authority and Delegation of the high seas beyond the contiguous the body of the comment and with any Authority zone in connection with activities under disk or CD–ROM you submit. If EPA IV. Background A. Historical Background the Outer Continental Shelf Lands Act, cannot read your comment due to B. Current Statute and Regulation activities under the Deepwater Port Act technical difficulties and cannot contact C. Advanced Response Planning of 1974, or activities that may affect you for clarification, EPA may not be V. This Action natural resources belonging to, able to consider your comment. A. Discharge of Oil appertaining to, or under the exclusive Electronic files should avoid the use of B. Subpart A—Introduction management authority of the United special characters, any form of 1. Definitions States, including resources under the encryption, and be free of any defects or C. Subpart J—Use of Dispersants, and Magnuson Fishery Conservation and Other Chemical and Biological Agents viruses. Comments and suggestions 1. General Management Act of 1976. These regarding the scope of any future 2. Authorization of Use requirements are anticipated to rulemaking should be clearly 3. Monitoring the Use of Dispersants encourage the development of safer and differentiated from comments specific to 4. Data and Information Requirements for more effective spill mitigating products, this proposal (e.g., label Suggestions for Product Schedule Listing and would better target the use of these Future Rulemaking and Comments on 5. Submission of Confidential Business products to reduce the risks to human Current Proposal). Information (CBI) health and the environment. Further, Docket: All documents in the docket 6. Addition of a Product to the Schedule 7. Mandatory Product Disclaimer the amendments are intended to ensure are listed in the http:// 8. Removal of a Product From the Schedule that On-Scene Coordinators (OSCs), www.regulations.gov index. Although 9. Appendix C to Part 300 Regional Response Teams (RRTs), and listed in the index, some information is 10. Appendix E to Part 300 Area Committees have sufficient not publicly available, e.g., CBI or other VI. Summary of Proposed Rule Provisions

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VII. Statutory and Executive Order Reviews EPA’s effort to inform the use of • Monitoring the Use of Dispersant. A. Executive Order 12866: Regulatory dispersants and other chemical or Establish monitoring requirements for Planning and Review and Executive biological agents when responding to oil dispersant use in response to major Order 13563: Improving Regulation and discharges. They incorporate lessons discharges and/or certain dispersant use Regulatory Review learned from the federal government’s situations. B. Paperwork Reduction Act • C. Regulatory Flexibility Act (RFA) experiences in the Gulf, and address General Product Information for D. Unfunded Mandates Reform Act recommendations specific to agent Schedule Listing. Revise and establish E. Executive Order 13132: Federalism testing and use in response to oil requirements, including designation of F. Executive Order 13175: Consultation discharges from the National and testing for all product categories and Coordination With Indian Tribal Commission on the BP Deepwater under which the listing is requested, Governments Horizon Oil Spill and Offshore Drilling Safety Data Sheets, sample product G. Executive Order 13045: Protection of Report to the President. labels, shelf life, collection and Children From Environmental Health The proposed amendments would recovery, persistence in the Risks and Safety Risks H. Executive Order 13211: Actions That help to ensure that only products that environment, storage and use Significantly Affect Energy Supply, perform effectively in laboratory testing conditions, physical and chemical Distribution or Use would be listed on the NCP Product properties, component identities, I. National Technology Transfer and Schedule (Schedule) for use in concentration limits on National Water Advancement Act mitigating the effects of oil discharges in Quality Criteria and Standards J. Executive Order 12898: Environmental the environment. Manufacturers would contaminants, laboratory accreditations, Justice be required to provide more detailed submission of all testing data and I. General Information product application materials, calculations, production capabilities, ecological toxicity data, and human and any other data or certification In April 2010, the Deepwater Horizon health and safety information, including informing the product’s performance underwater oil well blowout discharged more detailed instructions for product capabilities or environmental benefits. significant quantities of oil into the Gulf application in the field. Prohibitions on • Dispersant Testing and Listing of Mexico. The blowout discharged oil using products in certain areas under Requirements. Revise the efficacy from one mile below the sea surface. certain conditions determined by On- testing methodology using a baffled Approximately one million gallons of Scene Coordinators (OSCs), Regional flask test, establish new developmental dispersants over a three-month period Response Teams (RRTs), and EPA and sub-chronic toxicity testing were deployed on surface slicks over would help ensure that first responders requirements, revise the acute toxicity thousands of square miles of the Gulf, are better able to mitigate environmental testing methodologies, revise the listing and approximately three quarters of a effects when spills occur. The required criteria, and establish use limitations to million gallons of dispersants were, for submission of additional product saltwater environments. the first time, injected directly into the toxicity information would aid OSCs • Surface Washing Agent Testing and oil gushing from the well riser. This use and RRTs when evaluating specific Listing Requirements. Revise the acute of dispersants raised many questions product information and when deciding toxicity testing methodology and listing about efficacy, toxicity, environmental whether and which products to use to requirements, establish efficacy testing trade-offs, and monitoring challenges mitigate hazards to the environment and requirements and listing criteria, and that EPA seeks to address through the human health caused by discharges or establish use limitations based on proposed revisions to Subpart J. threatened discharges of oil. product testing for salt and/or The proposed revisions to Subpart J Specifically in this action, the Agency freshwater environments. address the use of dispersants and other proposes, for the following areas: • Bioremediation Agent Testing and chemical and biological agents to • Definitions. Amend definitions for Listing Requirements. Revise the respond to oil discharges into waters of Bioremediation agents, Burning agents, efficacy and acute toxicity testing the U.S. Over the past several years, Chemical agents, Dispersants, Sinking methodologies and listing criteria, EPA’s Office of Research and agents, Sorbents, and Surface washing establish exceptions for specified non- Development (ORD) has conducted agents; add new definitions for proprietary products, and establish use research on improved laboratory Bioaccumulation, Bioconcentration, limitations based on product testing for protocols for dispersant and Biodegradation, Biological agents, salt and/or freshwater environments. bioremediation efficacy, and revisions Bioremediation, Herding agents, • Solidifier and Herding Agent to Subpart J to address these new Products, and Solidifiers; and remove Testing and Listing Requirements. protocols were under consideration. As definitions for Miscellaneous Oil Spill Revise the acute toxicity testing a result of this research and the Control Agents (MOSCA) and Surface methodology and listing criteria, and Deepwater Horizon event, the new collecting agents. establish use limitations based on protocols in the proposed revisions, in • General Requirements. Revise to product testing for salt and/or addition to increasing the overall reflect new and amended regulatory freshwater environments. scientific soundness of the data, take definitions. • Sorbent Requirements. Establish a into consideration not only the efficacy • Authorization of Use. Revise to list of known, non-proprietary sorbents but also the toxicity, long-term clarify planning and preauthorization to be made publicly available in lieu of environmental impacts, endangered responsibilities, establish limitations listing sorbents on the Schedule, and species protection, and human health and prohibitions on the use of certain requirements for data and information concerns raised during responses to oil agents, establish requirements for for sorbent products with components discharges, including the Deepwater storage and use of agents, clarify other than those specifically identified Horizon blowout. Additionally, area authorities for requiring supplemental in the rule. planning requirements for dispersant testing, monitoring and information on • Submissions of Confidential use authorization, toxicity thresholds agents, establish requirements for agent Business Information. Revise the and advanced monitoring techniques recovery from the environment, and allowable confidential business are also proposed. The proposed establish reporting requirements for information claims and reporting amendments are a major component of agent use. procedures.

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• Addition of a Product to the provide a guide for readers to consider human life or limb, or substantial Schedule. Revise the submission regarding entities that potentially could hazard of fire to property, dispersants requirements including the package be affected by this action. However, this were restricted from use on or in any: contents, EPA’s review of submission action may affect other entities not Distillate fuel oil; spill of oil less than package, request for review of decision, listed in this table. If you have questions 200 barrels in quantity; shoreline; changes to a product listing, and regarding the applicability of this action waters less than 100 feet deep; waters transitioning of listed products from the to a particular entity, consult the containing major populations or current Schedule to the new Schedule. person(s) listed in the preceding section breeding or passage for species of fish or • Mandatory Product Disclaimer. entitled FOR FURTHER INFORMATION marine life which may be damaged or Revise the product disclaimer CONTACT. rendered commercially less marketable requirements. by exposure to the dispersant or • Removal of a Product from the III. Statutory Authority and Delegation dispersed oil; waters where the winds Schedule. Revise the basis for removal of Authority and/or currents are of such velocity and and appeals process. Under sections 311(d) and 311(j) of direction that the dispersed oil mixtures • Appendix C to part 300. Revise the the Clean Water Act (CWA), as amended would likely, in the judgment of the requirements for product testing by section 4201 of the Oil Pollution Act FWQA, be carried to shore areas within protocols and summary test data of 1990 (OPA), Public Law 101–380, the 24 hours; and waters where such use including new dispersant baffled flask President is directed to prepare and may affect surface water supplies. The efficacy and toxicity tests; new standard publish the National Oil and Hazardous CEQ revised the National Oil and acute toxicity tests for bioremediation Substances Pollution Contingency Plan Hazardous Materials Pollution agents, surface washing agents, herding (NCP) for removal of oil and hazardous Contingency Plan, renaming it the agents, and solidifiers; and revised substances. Specifically, section National Oil and Hazardous Substances bioremediation agent efficacy test. Pollution Contingency Plan (NCP) in • 311(d)(2)(G) requires the President to Appendix E to Part 300—Oil Spill include a schedule identifying 1971 (36 FR 16215). The NCP was Response. Remove this appendix from ‘‘dispersants, other chemicals, and other amended again in 1971 (36 FR 18411) the NCP. spill mitigating devices and substances, and 1972 (37 FR 28208), with no EPA estimates industry may incur if any, that may be used in carrying out’’ substantive changes to Annex X. total incremental costs of approximately the NCP. The authority of the President As a result of the Federal Water $668,000 to $694,000 annually. The to implement this portion of the CWA Pollution Control Act (Pub. L. 92–500) benefits of the Subpart J amendments is currently delegated to EPA in of 1972, CEQ again revised the NCP, are assessed qualitatively. Such benefits Executive Order 12777 (56 FR 54757, including revisions to Annex X (38 FR include, for example, greater clarity of October 22, 1991). Subpart J of the NCP 21887, August 13, 1973). The title of regulatory requirements, as well as less governs the use of dispersants, and any Annex X changed to the ‘‘Schedule of toxic products. This action does not other chemical or biological agent to Chemicals to Remove Oil & Hazardous pose significant impacts on a substantial respond to oil discharges (40 CFR part Substances Discharges.’’ While the number of small entities. The 300 series 900). Schedule still advocated mechanical Regulatory Impact analysis, which can and other control methods, and the be found in the docket, provides more IV. Background removal and proper disposal of oil from detail on the cost methodology and A. Historical Background the environment, it broadened its benefits of this action. applicability to chemical agents, The Council on Environmental including dispersants. It also recognized COST OF THE PROPOSED RULE Quality (CEQ) first published the separate authorizations of use for National Oil and Hazardous Materials chemical agents on minor, medium and Annualized costs, 20 years Pollution Contingency Plan in 1970 (35 major discharges. In addition, the FR 8508). Among its elements was revised schedule required an official Annualized at Annualized at Annex X—Schedule of Dispersants and 3% 7% report from a recognized laboratory with other Chemicals to Treat Oil Spills. a description of the analytical methods Costs ...... $667,610 $694,343 Annex X provided a basic regulatory employed and results obtained in framework that included authorization determining the chemical and biological II. Entities Potentially Affected by This of use, restrictions, and information characteristics of the chemical agent, Proposed Rule requirements to be submitted to the but no longer required the submission of Federal Water Quality Administration those analytical methods. Biological and Industrial category NAICS code (FWQA). This initial schedule burning agents were not part of the advocated mechanical and other control Schedule, which expressed caution on Chemical Manufacturing ...... 325 methods, and the removal and proper their use. Merchant Wholesalers, Non- disposal of oil from the environment. It In 1975 CEQ again revised the NCP, durable Goods ...... 424 also specified that dispersants might be Professional, Scientific, and including Annex X (40 FR 6282). Annex Technical Services ...... 541 used in accordance with the schedule if X was now the ‘‘Schedule of Chemicals Waste Management and Re- other control methods are judged to be and Other Additives to Remove Oil & mediation Services ...... 562 inadequate or infeasible, and if certain Hazardous Substances Discharges,’’ and Oil and Gas Extraction ...... 211 information requirements and usage it was ‘‘. . . revised and expanded to requirements were met. As a listing provide more precise and definitive The list of potentially affected entities requirement, manufacturers had to information, concerning substances in the above table includes provide the FWQA with methods for which may be employed to remove manufacturers and users of chemical analyzing the chemical components in discharges.’’ Additionally, Executive and biological agents, and other oil spill fresh and salt water, or reasons why Order 11735 (38 FR 21243, August 3, mitigating devices and substances used such analytical methods could not be 1973) made EPA responsible for Annex as countermeasures against oil provided. Except to prevent or X. Chemical agents or any other discharges. The Agency’s goal is to substantially reduce the hazard to substance not specifically defined in the

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Schedule were to be considered for use generated comparable data regarding the In 1994, EPA revised the NCP in on a case-by-case basis. The Schedule products’ effectiveness and toxicity. response to the passage of the Oil advocated the development and Appendix C detailed the methods and Pollution Act in 1990 (59 FR 47384). utilization of mechanical control types of apparatus to be used in carrying The final rule significantly revised methods to remove or mitigate oil, and out the revised standard dispersant Subpart J to its current regulatory to remove, mitigate, or neutralize effectiveness and toxicity tests, as well requirements with respect to hazardous substances discharges from as the format required for summary authorization of use, data requirements, the environment, with subsequent presentation of product test data. Listing dispersant effectiveness and toxicity proper disposal. The Schedule intended of a product on the Schedule was testing protocols, surface washing agent that no harmful quantities of any neither a recommendation nor toxicity testing protocol, bioremediation substance were to be applied to waters authorization for use on an oil agent effectiveness testing protocol, and to remove or mitigate the effects of oil discharge, but rather a confirmation that requirements for adding products to the or hazardous substances discharges. The data submission requirements had been Schedule. As a result, several Schedule also provided procedures for satisfied. EPA’s listing on the Schedule dispersants were re-classified as surface authorization of use for different agent did not confirm its safety or washing agents because they did not categories, and separate regulatory effectiveness or constitute an pass the dispersant efficacy test authorization of use for dispersants or endorsement; in fact, a new requirement threshold, but were effective in other chemical agents was established was established that either a written removing oil from solid surfaces. for minor, medium, and major disclaimer to this effect or EPA’s written B. Current Statute and Regulation discharges. Product shelf life, toxicity disclaimer be included in all product and effectiveness, and analytical technical literature or advertisements. Section 300.910 of Subpart J methods needed to obtain such data Products previously listed under Annex addresses the authorization of the use of were among the technical data X were included on the new Schedule products on the Schedule and specifies requirements. Similar provisions were as the previous data requirements were the conditions under which OSCs may tailored to surface collecting agents and sufficient to permit OSCs to make authorize the use of dispersants, other biological additives. informed decisions about product use. chemicals, and other spill mitigating In 1982, EPA amended the NCP; the substances. Sections 300.915 and The amendments also provided for revision included rewriting of Annex X 300.920 describe the data requirements OSC authorization for use of burning as Subpart H of 40 CFR part 300 of the and the process for adding products to revised Plan (47 FR 31180). The Agency agents on a case-by-case basis with the the Schedule. To list a product on the allowed OSCs to authorize the use of concurrence of the EPA RRT Schedule, Subpart J currently requires dispersants or other chemicals to treat representative and the States, and the submission of technical data on the discharges of oil, provided they were prohibited the use of sinking agents in product to EPA. Data on dispersants, listed in the previous Annex X, with the waters of the United States. They surface collecting agents, surface following limitations: encouraged advance planning by washing agents, and miscellaneous oil • Authorization applies only to allowing the OSC to act without the spill control agents must include the discharges of oil, not to releases of concurrence of the RRT and affected results of the toxicity test set for these hazardous substances. States if these parties have approved a products in Appendix C of the NCP. • OSCs may only authorize the use of plan identifying the products that may Data on dispersants must also include dispersant or other chemicals on EPA’s be used in specific contexts. The the results of the dispersant Acceptance list, which included the amendments also allowed the OSC to effectiveness test, while bioremediation twenty-eight products tested and found authorize the use of any product agents must include results of the acceptable for their intended purpose in (including products not on the bioremediation effectiveness test, also the previous Annex X. Schedule) without obtaining the set forth in Appendix C. These tests are • State consultation provisions concurrence of the EPA representative conducted at the expense of the product regarding the use of any dispersant or to the RRT or the affected States if the manufacturers and must be performed other chemicals in its waters required use of a dispersant, surface collecting by laboratories experienced with the OSC to obtain concurrence from the agent, or biological additive is necessary Appendix C protocols. EPA representative to the RRT. to prevent or substantially reduce The raw data and a summary of the The new Subpart H of 40 CFR part hazard to human life, and there is not results from these tests are then 300 also provided for a case-by-case sufficient time to obtain concurrence. submitted to EPA, where they are authorization by the EPA Administrator However, the OSC was to inform the reviewed to confirm that the data are (‘‘Administrator’’) or designee of the use EPA RRT representative and the affected complete and that the specified of dispersants or other chemicals not on States of the use of a product as soon as procedures were followed. The data EPA’s Acceptance list in treating oil possible, and obtain their concurrences requirements for placement of a product discharges or hazardous substances for the product’s continued use in the on the Schedule are designed to provide releases. However, EPA did not include situation once the threat to human life sufficient data for the OSCs to judge testing procedures or a process for had subsided. These provisions were whether and in what quantities a designation of dispersants or other designed to eliminate delays in life product may be used to control a chemicals as acceptable for use. threatening situations, such as spills of particular discharge. Inclusion of a In 1984, EPA published amendments highly flammable petroleum products in product on the Schedule means only to Subpart H, including adding harbors or near inhabited areas. Subpart that the data submission requirements Appendix C (49 FR 29192). The H was re-designated as Subpart J with have been satisfied. The listing of a amendments specified testing and data minor changes in 1990 (55 FR 8666), product on the Schedule does not mean requirements for listing of dispersants, with those definitions present in that the product is recommended or surface collecting agents, or biological Subpart H moved to Subpart A, and a authorized for use on any specific oil additives on the Schedule to ensure new definition and data requirements discharge nor does it imply that EPA sufficient data was available for the for miscellaneous spill control agents has in any other way endorsed the OSC. Standardized testing procedures added. product for the use listed or for other

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uses. The standardized testing AC responsibilities include enhancing Efficacy and Effects’’ (2005), procedures set forth in Appendix C contingency planning; ensuring recommends that steps be taken to provide OSCs comparable data preplanning of joint federal, state, and better support policymakers and spill regarding the toxicity, effectiveness, and local response efforts; and expediting responders faced with making choices other characteristics of different decisions on the use of dispersants and regarding the use of dispersants as part products. other spill mitigating devices and of spill contingency planning efforts or substances. The Area Contingency Plan during actual spills. The United States C. Advanced Response Planning (ACP) must list the equipment, Coast Guard has promulgated new Under the current 300.910(a) dispersants or other spill mitigating requirements for certain vessels to have regulation, RRTs and the Area substances, and personnel available to only Schedule listed dispersant Committees (ACs) are required to ensure effective and immediate removal response capabilities while operating in address, as part of their planning of a discharge. ACPs must also ensure designated dispersant preauthorization activities, the desirability of using the mitigation or prevention of a zones (74 FR 45004, August 31, 2009). appropriate dispersants, and other substantial threat of a discharge; provide The proposed amendments are aimed chemical or biological agents. The RRTs a description of the procedures to be at ensuring that chemical and biological and ACs generally develop followed for obtaining an expedited agents have met efficacy and toxicity ‘‘preauthorization plans’’ which address decision regarding the use of requirements, that product the specific context in which products dispersants (which may be addressed in manufacturers provide important use can be used under OSC direction. applicable preauthorization plans); and and safety information, and that the Preauthorization plans are approved identify the means to monitor use of planning and response community is with concurrences from EPA, chemical countermeasures. Many equipped with the proper information to Department of Interior (DOI) and coastal ACPs include some type of authorize and use the products in a Department of Commerce (DOC) natural preauthorization zones for dispersants, judicious and effective manner. resource trustees, and the state(s) with while most Regional Contingency Plans V. This Action jurisdiction over the water to the area, (RCPs) address other product categories, which they apply. When a such as bioremediation and surface This proposal addresses the efficacy, preauthorization plan approves in washing agents. RRTs, in cooperation toxicity, environmental monitoring of advance the use of certain products with the states and federal agencies, dispersants, other chemical and under specified circumstances, the OSC have addressed the requirements for the biological agents, and other spill may authorize the use of the products conduct of in-situ burns (ISB) of oil mitigating substances, as well as public, without obtaining the specific discharges in their RCPs. state, local, and federal officials concurrences described elsewhere in This planning has allowed concerns on their authorization and use. that section of the regulation. The use of consideration of chemical agent use on The sections below explain the chemical or biological agents is only one oil discharges as a viable response tool proposed requirements and revisions, approach of many available, such as in combination with other mitigation and EPA is requesting comments by mechanical collection or in-situ measures. These agents have section. Alternatives offered should burning, and decisions about their use increasingly been considered and used include rationale and supporting should be weighed to achieve greater in the field, as evidenced by research information in order for the Agency to overall environmental protection. and case studies presented at national include the alternative in any final rule. To facilitate the best possible and international oil spill conferences, A. Discharge of Oil response, it is important that the research and development funding from regional-level and area-level private and government stakeholders, The Agency is proposing revisions to contingency planning efforts of the RRT efforts to plan for their use, harmonize 40 CFR part 110.4 with the RRTs and ACs, respectively, are requests for EPA and other federal definitions for chemical and biological coordinated closely with each other and experts to advise field personnel on the agents proposed for Subpart J. The are consistent. Section 300.910(a) use of such products, and by the current language in § 110.4 is specific to authorizes the RRTs to review and response to the Deepwater Horizon oil dispersants and emulsifiers. The either approve, disapprove, or approve spill. While many research efforts have proposal replaces the terms ‘‘dispersants with modification the preauthorization helped to clarify issues and added and emulsifiers’’ with the broader terms plans developed by Area Committees information on the toxicity, efficacy, of ‘‘chemical agent’’ and ‘‘biological that addresses dispersants or other spill proper use, and human health impacts agent’’ as proposed to be amended in mitigating substances. This advanced of these response technologies, § 300.5. The proposed definition for planning has allowed the OSC to uncertainties still arise. The Agency has chemical agents includes elements, authorize the use of products without an interest in resolving the issues that compounds, or mixtures designed to obtaining the specific concurrences, if arise from the use of chemical and facilitate the removal of oil from a the RRT representatives from EPA and biological agents in spill responses, as contaminated environment and mitigate the states with jurisdiction over waters its representatives are asked to concur any deleterious effects. The proposed to which a preauthorization plan with chemical and biological agent use definition for biological agents includes applies, and DOC and DOI natural for marine and freshwater spills. microorganisms (typically bacteria, resource trustees approve their use in The use of non-mechanical oil spill fungi, or algae) or biological catalysts, advance. The OSC primarily uses the mitigating technologies, such as such as enzymes, able to enhance the Schedule to confirm if a product is dispersants, surface washing agents, biodegradation of a contaminated listed, analyze toxicity and efficacy sorbents, solidifiers, bioremediation environment. Chemical and biological data, note worker health and safety agents, and others are among the agents would include both the precautions, understand proper product available oil response options that dispersants and emulsifiers cited in application, and compare one product responders may consider in the United § 110.4. By revising 40 CFR part 110, the to another in order to make the most States and the world. The National Agency is clarifying that any chemical informed decision on how to mitigate an Academies’ National Research Council or biological agent added to a discharge oil discharge. report titled ‘‘Oil Spill Dispersants: of oil with the intent to circumvent any

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provision of 40 CFR part 110 is For example, the fuel used in helitorch (including biosurfactants), and prohibited. To further reflect the systems is a mixture of powdered additives. The proposed definition proposed revisions, the Agency is gelling agents with either gasoline, jet specifically addresses the process proposing to also amend the section title fuel, or a diesel/gas mixture, which are through which these agents assist in to ‘‘Chemical or biological agents.’’ EPA organic compounds.1 The Agency mitigating the consequences of a believes the proposed amendment is believes both the inorganic gelling agent discharge, clarifying for manufacturers consistent with U.S. Coast Guard and the organic fuel (e.g., gasoline) meet which testing requirements they will be (USCG) regulations, which prohibit the the burning agent definition by subject to when seeking to list a product discharge of chemicals or other improving the combustibility of the on the Schedule. substances into the sea that circumvent materials to which they are applied Sinking agents—The Agency is discharge conditions specified in their through physical or chemical means. proposing to revise the definition of regulation (33 CFR 151.10(g)). EPA The Agency considered including sinking agents to identify them as those requests comment on these revisions. ignition devices in the definition of substances deliberately introduced into burning agent because improving the an oil discharge to submerge the oil to B. Subpart A—Introduction combustibility of oil and igniting that the bottom of a water body. The current 1. Definitions oil could be considered one and the definition is ambiguous in regards to same. The intent would be to clarify the how much sinking below the water The Agency is proposing revisions to potential that not only substances, but surface would qualify as a sinking agent, § 300.5 that amend the definitions for also the devices holding those as some submersion below the surface Bioremediation agents, Burning agents, substances, be considered in the case- but generally not to the bottom of the Chemical agents, Dispersants, Sinking by-case authorization of use of such water body can also be associated with agents, and Sorbents. The Agency agents. The Agency rejected this other agents, such as dispersants. The proposes to revise the term Surface approach since many devices either proposed definition specifies these washing agent and amend its definition. deliver the agent to the oil to be burned agents purposely sink the oil to the Additionally, the proposal includes new and do not enter the water, or are bottom of a water body. The Agency is definitions for Bioaccumulation, consumed in the burn along with the prohibiting the use of sinking agents in Bioconcentration, Biodegradation, agent. The Agency requests comment on the remediation of oil discharges in Biological agents, Bioremediation, whether it should add ignition devices water because of their potential for Herding agents, Products, and to the definition of a burning agent. causing adverse effects on benthic Solidifiers. Finally, the Agency is Chemical agents—The Agency organisms vital to the food chain of the removing the definitions for proposes to revise the definition of aquatic environment. Miscellaneous Oil Spill Control Agent chemical agents to identify as such Sorbents—The Agency is proposing to (MOSCA) and Surface collecting agents. those elements, compounds, or mixtures revise the definition of sorbents to (a) Revised Definitions that are designed to facilitate the identify them as inert, insoluble removal of oil. These agents may be substances that readily absorb and/or Bioremediation agent—The Agency is used to mitigate deleterious effects of adsorb oil or hazardous substances. The proposing to revise the definition of the oil on a contaminated environment. proposed definition specifies that bioremediation agents to identify as The proposed definition would include sorbents are not combined with or act as such biological agents and/or nutrient under the chemical agent category any other chemical or biological agent. additives. These agents would be burning agents, dispersants, herding The proposed definition also specifies deliberately introduced into a agents, sinking agents, solidifiers, that sorbents are generally collected and contaminated environment to increase surface washing agents, and those recovered from the environment and the rate of biodegradation, which in turn bioremediation agents that consist of that they may be used in their natural would assist in mitigating deleterious nutrient additives. The proposed bulk form, or as manufactured products effects caused by contaminants. The language reflects the distinction the in particulate form, sheets, rolls, proposed definition identifies as Agency is now making between pillows, or booms. The proposed bioremediation agents microorganisms chemical and biological agents, allowing definition identifies sorbents as and enzymes. It also identifies nutrient product manufacturers to better target substances consisting of: (1) Natural additives such as fertilizers containing the testing requirements and OSCs to organic substances (e.g., feathers, cork, bio-available forms of nitrogen, better inform their authorization of peat moss, and cellulose fibers such as phosphorus, and potassium. The agent use in specific situations. The bagasse, corncobs, and straw); (2) proposed definition clarifies the current proposal also removes from the inorganic/mineral compounds (e.g., definition and adds specific examples of definition agent categories that are volcanic ash, perlite, vermiculite, bioremediation agents. This clarification either being eliminated, prohibited or zeolite, clay); and (3) synthetic will help manufacturers of products in amended to conform to the changes, as compounds (e.g., polypropylene, identifying the type of product, and discussed below. polyethylene, polyurethane, polyester). hence, what testing requirements they Dispersants—The Agency is The proposed changes simplify the will need to comply with to have a proposing to revise the definition of definition by removing the definitions product listed on the Schedule. dispersants to identify them as those of absorption and adsorption that are Burning agents—The Agency agents that promote the formation of embedded in the current definition of proposes to revise the definition of small droplets of oil in the water sorbents. The Agency believes this is burning agents to identify as such those column by reducing the oil-water appropriate given these are generally additives that improve the interfacial tension. Dispersants are recognized scientific terms and the combustibility of the materials to which proposed to be defined as typically proposal does not distinguish sorbents they are applied. This could be achieved mixtures of solvents, surfactants or in any way restrict their use based on through either physical or chemical whether they absorb or adsorb the oil. means. Burning agents include 1 Fingas, Mervin, (Ed) (2011), Oil Spill Science The definition also adds the ‘‘natural’’ inorganic compounds in the form of and Technology, Gulf Professional Publishing, pp. qualifier to organic substances, gelling agents, such as aluminum soap. 836, ISBN: 978–1–85617–943–0. indicating that organic substances that

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have been treated with other substances removal may cause more harm than the Finally, the Agency is proposing a would not necessarily fall under this oil itself due to trampling in the wetland new definition for the term product to category of agents and should not or salt marsh. Once the oil is brought to clarify the difference between a specific immediately be considered a sorbent. It the surface by the sorbent, product and an agent type or category. also expands on and simplifies the biodegradation of both the oil and the All of the proposed new definitions can examples by removing the references to sorbent can take place, especially if be found in the § 300.5 of this action. the type of birds that feathers could nutrients are added to enhance come from, by adding bagasse to the biodegradation. Another example would (c) Removed Definitions examples for natural organic substances, be the use of OMA technology to The Agency is proposing to remove and by adding clay to the examples for promote dispersion, which might not the definitions for surface collecting inorganic/mineral compounds. The lend itself to collect or remove the agent and for miscellaneous oil spill Agency requests comments on whether aggregates from the environment. Thus, control agent (MOSCA). The surface the definition is appropriate or if there the Agency is requesting comment on collecting agent definition is being are other materials that should also be whether testing and/or authorization of removed and replaced with a new included. use requirements should be considered herding agent definition to better reflect Additionally, the Agency requests for particulate materials in loose form or the common terminology used in comments on particulate materials (e.g., OMA technologies that may be used in industry for these agents. The MOSCA clay) as sorbents. There is concern that discharge situations where they would definition is being removed and particulate materials with densities not be collected and recovered from the replaced with a number of new and/or greater than the seawater (or freshwater environment. revised definitions for types of agents. depending on where they may be used) Surface washing agents—The Agency The original MOSCA category was used have the potential to become sinking is proposing to revise the term surface as a catchall for all types of products agents, settling to the seabed and posing washing agent and the definition for that did not meet other agent potential risks to benthic organisms. surface washing agents. The proposed definitions. As the Agency adds new, This question is also relevant when definition would identify surface more stringent testing requirements for considering emerging response washing agents as those substances that listing products on the Schedule, there technologies such as the use of separate oil from solid surfaces (e.g., is a need for more specific category particulate materials to form oil-mineral beaches, rocks, metals, or concrete) definitions to assist manufacturers in aggregates (OMAs) to promote through a detergency mechanism. This determining which of those testing dispersion. OMAs are stable detergency mechanism would lift and requirements apply to their products. microscopic entities formed when float the oil for collection and recovery The Agency believes it has identified particulate materials interact with the from the environment. The use of these categories that capture all products to be oil droplets resulting in distinct oil and agents results in minimal dissolution, listed on the Schedule; we request mineral phases. These fine mineral dispersion, or transfer of oil into the comment on whether the MOSCA particles could be intentionally water column. The proposed changes category should be retained, and introduced by themselves to promote revise the term from singular to plural whether the proposed categories are physical dispersion by preventing the to be consistent with the other agent appropriate, including sufficient oil to re-coalesce, or can also be used in definitions and clarifies that these information and rationale to support the conjunction with dispersants to enhance agents are to be recovered from the addition of any new categories. chemical dispersion. However, any environment along with the oil being particulate material that by itself, or treated. C. Subpart J—Use of Dispersants, and when combined with oil (e.g., OMA), Other Chemical and Biological Agents (b) New Definitions results in overall densities less than the 1. General waters where it may be used, would not The Agency is proposing to add be prohibited as a sinking agent. The several new definitions that serve as the EPA is proposing to amend § 300.900 Agency requests comment on whether foundation for the new proposed by revising paragraphs (a) and (c), and the use of sorbent materials in biological agent classification: by adding paragraph (d) to reserve for particulate form should be specified for Bioaccumulation, Bioconcentration, ‘‘Releases of Hazardous Substances’’. use only in booms or other contained Biodegradation, Biological agents, and The proposed revisions clarify that manufactured products, and whether Bioremediation. The proposed Subpart J addresses not only chemical there should be limitations on the definitions include basic terminology agents, but also those agents that now authorization of use on water for and are consistent with definitions of fall under the newly proposed biological sorbents in loose particulate form. these terms generally understood by the agent category. The revisions reaffirms Alternatively, the Agency also requests scientific community. the notion that Subpart J is not only comment and supporting rationale on The Agency is also proposing new comprised of a Schedule of chemical other approaches, including whether definitions for the terms herding agents and biological agents, but also includes particulate materials in loose form, or and solidifiers. The proposed testing requirements and authorization specifically OMA technologies, should definitions address types of agents of use procedures. Consistent with be excluded from the regulatory originally captured under the surface current Subpart J regulatory definition of sorbents. collecting agent or the miscellaneous oil requirements the Agency is proposing to Finally, EPA also requests comments spill control agent categories reserve a section for ‘‘Releases of on the qualifier phrase ‘‘that are respectively, and are terms that are more Hazardous Substances’’ to take place of generally collected and recovered from commonly used in industry. The the current placeholder in § 300.905, the environment.’’ For example, a definitions more specifically describe which is proposed to be removed. Based natural organic and biodegradable the specific process through which the on all relevant circumstances, testing sorbent (e.g., bagasse) may not product affects the oil for the categories data and information, and in accordance necessarily need to be removed after it and are consistent with definitions of with the authorization of use procedures has absorbed/adsorbed the oil when these terms generally understood by the (including the appropriate concurrences used in a wetland or salt marsh. Such scientific community. and consultations), the waters and

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quantities in which a dispersant, or charge of preparedness planning the (a) Use of Agents Identified on the other chemical or biological agents may opportunity to identify and resolve Schedule on Oil Discharges Addressed be safely used are to be determined in concerns in advance, leading to quick by a Preauthorization Plan each case by the OSC. When taken and effective operations during removal The Agency is proposing revisions to together, these testing requirements, actions. The Agency believes these § 300.910(a) of Subpart J to address the listing of agents and authorization of use proposed revisions to the authorization preauthorized use of chemical and procedures address the types of waters of use provisions will assist OSCs, biological agents identified on the and the quantities of listed agents that RRTs, and ACs in their advanced Schedule. The proposed revisions may be used in response to discharges planning activities as they consider clarify the process for preauthorization, of oil or hazardous substances. The response methods that result in the the responsibilities of all involved wide variability in waters, weather greatest environmental protection. The parties, and the factors to consider conditions, organisms living in the during the preauthorization process, waters, and types of oil that might be goal is to ensure that preauthorization or including the authorization for the use discharged requires this approach. expedited decision making plans are developed and maintained to effectively of agents by the OSC at the time of a 2. Authorization of Use support decisions by OSCs during discharge. EPA is also proposing to Section 300.910 sets forth the removal actions. In carrying out reorganize paragraph (a) to provide provisions for the authorization of use advanced planning activities, the greater clarity by making the regulatory of products on the Schedule in response Agency believes the NRT can assist text easier to read and follow. The to oil discharges. Subpart J does not RRTs by providing guidance on national Agency believes that the proposed state or imply that chemical or level issues that may arise during revisions do not change its fundamental policies regarding roles of Federal, state biological agents are preferred over planning activities. other response options such as and local representatives involved in EPA is amending § 300.910 by mechanical recovery devices. EPA planning for and responding to an oil believes that the circumstances revising paragraphs (a) through (f); and discharge, but rather clarify the current surrounding oil discharges and the by adding paragraphs (g), (h) and (i). requirements and further explain the factors influencing the choice of EPA is not proposing major changes to responsibilities for each party. The response methods are many. During the the current authorities granted to OSCs, Agency is also proposing added DWH response, a priority RRT representatives to the RRTs, States, procedures and review requirements countermeasures scheme was DOC, DOI, or other National Response intended to ensure preauthorization established to first use mechanical Team decision makers with regards to plans are up-to-date so they are most recovery via skimming/booming or in- the authorization and application of effective when implemented in case of situ burning followed by subsea chemical or biological agents. However, a discharge. dispersant and lastly surface dispersant EPA recognizes that the planning for EPA believes RRTs and ACs must use. Following DWH, EPA and the NRT and prolonged use and monitoring of work together in order to effectively and issued Interim Actions regarding the use chemical agents, especially dispersants, successfully manage contingency of dispersants on oil spills to NRT may require additional planning planning. Thus, the proposed revisions members and RRT co-chairs 2 and to activities and monitoring requirements. continue to require that, as part of their 3 planning activities, RRTs and ACs EPA Regional Administrators for Thus, the Agency is proposing to address in the preauthorization plan consideration during response planning. reorganize this section; to add titles to whether the use of chemical and While response actions are incident the paragraphs for ease of use; to add biological agents listed on the Schedule specific, the availability of response several requirements addressing the methods that address the specific on certain oil discharges is appropriate. storage and use of agents, notification of discharge situation depends largely on The Agency believes that the proposed agent use and recovery from the contingency planning activities and on revision clarifies the meaning of the how these requirements are environment; and to revise language to desirability of using appropriate implemented through the RCPs, ACPs clarify established EPA policy. The chemical or biological agents. The and vessel and facility response plans. proposed revisions and clarifications are Agency is removing ‘‘. . . the In order for a response to be effective, highlighted for each paragraph under desirability of using appropriate burning the NCP requires coordination between § 300.910. agents.’’ from paragraph (a) and the regulatory and planning entities EPA is also confirming, consistent addressing the use of burning agents responsible for all these response plans. with the intent of the NCP, that use of under paragraph (c) to provide greater The Agency believes that chemical or biological agents in flexibility to OSCs for authorization of preauthorization or expedited decision response to oil discharges to waters of use. making plans are critical elements of the U.S. or its adjoining shorelines must Under the current paragraph (a), ACs contingency planning activities. be authorized by an OSC in accordance are responsible for developing preauthorization plans. ACs are also Regularly reviewing or revising with Subpart J. The unauthorized use preauthorization or expedited decision responsible for developing ACPs, can result in violations of section 301 making plans provides those agencies in providing a forum to evaluate the and 311 of the CWA. Section 301(a) environments within a jurisdiction and makes unlawful ‘‘the discharge of any 2 Tulis, Dana S., EPA Chair and Caplis, Captain establishing protection priorities. The John, USCG Vice-Chair, National Response Team, pollutant by any person,’’ except in information gathered during the ACP ‘‘Use of Dispersants on Oil Spills—Interim compliance with certain provisions of development process should inform the Actions;’’ Memorandum to NRT Members and RRT the CWA. In addition, section 311(b) Co-Chairs; December 16, 2010. development of preauthorization plans. 3 Stanislaus, Mathy; Assistant Administrator, establishes penalties for persons who Identified representatives from the RRTs OSWER EPA; ‘‘Revision of Area Contingency Plans/ fail or refuse to comply with any are responsible for approving or Regional Contingency Plans Regarding Use of regulation issued under section 311(j) of requesting modifications of Dispersants on Oil Spills—Interim Actions;’’ Memorandum to EPA Regional Administrators, the CWA. preauthorization plans developed by the November 2, 2010. ACs. ACs can advocate for local

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

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

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and the factors to consider when must consider and document the mitigating devices is prohibited, authorizing the use of listed chemical or parameters for the use of agents situations where limits are placed on biological agents in these situations. The including, but not limited to, quantities the quantities of agents used, or Agency believes the proposed revisions to be used, the duration of use, the situations that require certain do not change its fundamental policies depth of water, the distance to shoreline monitoring requirements be in place. regarding the roles of Federal, state and and proximity to populated areas, and local representatives involved in an oil should address factors such as (c) Burning Agents discharge response. environmentally sensitive resources or The Agency is proposing to replace The proposed revisions maintain, restricted areas that might be impacted, the current authorization of use for with the appropriate concurrences and agent inventory and storage locations, burning agents in § 300.910(c) with a consultations, the OSC’s authority to agent manufacturing capability, provision that provides greater authorize the use of chemical or availability of equipment needed for flexibility to OSCs for authorizing the biological agents on the oil discharge, agent use, availability of adequately use of burning agents. Specifically, the provided that the agents are listed on trained operators and appropriate means Agency proposes that OSCs may the NCP Product Schedule. The to monitor agent use in the authorize the use of burning agents for concurrence of the EPA representative environment. These considerations are authorized in-situ burns. The proposed to the RRT and, as appropriate, the parallel to those proposed under amendments recognize that relatively concurrence of the RRT representatives paragraph (a) for preauthorization and small quantities of burning agents are from the states with jurisdiction over planning purposes. While the Agency is ignited prior to or immediately after the waters and adjoining shorelines not including other factors that may they are introduced to an oil discharge. threatened by the release or discharge is inform preauthorization planning Furthermore, they are composed of maintained. The requirement for development, such as various discharge substances that are expected to rapidly consultation with the DOC and DOI scenarios, this does not mean these burn off during use, which serves to natural resource trustees is also factors cannot or should not be remove them from the water. The maintained. However, the language is considered if RRTs and/or ACs choose Agency also recognizes that ISB has amended by removing ‘‘when to develop expedited decision making become an important response option practicable’’ with respect to plans. The Agency believes these are that is used more frequently and the consultation with the DOC and DOI fundamental elements that would proposed revisions would allow OSCs natural resource trustees. The Agency inform an assessment of the overall to authorize the use of burning agents believes that the case-by-case decision ecological risks for the OSC to consider for authorized burns. For example, a making should include consultations when authorizing the use of chemical or significant number of ISBs were with natural resource trustees since biological agents. conducted during the Deepwater these discharge situations may present Finally, while not required, EPA Horizon oil spill,5 and ISBs appear to be unique challenges when selecting a strongly recommends advanced gaining a more prominent role as a response option that involves chemical planning for expedited decision making response option in federal waters in or biological agents. While the Agency for cases where the discharge situation remote locations, such as the Arctic. recognizes the time-critical nature of is not addressed in the preauthorization Therefore the Agency believes the decision making during a response, plans. Some RRTs have developed proposed revisions better address OSC advances in communication technology expedited approval guidelines that are authorities for these situations, without (e.g., smart phones, email) provide OSCs not part of the preauthorization plans, compromising environmental concerns. with increased capabilities to but that offer an opportunity for Further, because of the nature of communicate quickly. Therefore, the advanced contingency planning by burning agents and the proposed Agency believes it is reasonable to gathering information on the key revisions to the authorization of use for expect an OSC to be able to notify and parameters discussed above. Because these products, the Agency continues to explain the circumstances requiring use discharge situations not covered by believe it is not necessary to require of the certain agents to natural resource preauthorization plans need incident product submissions for burning agents. trustees in a timely manner. Of note, specific (i.e., case-by-case) authorization Thus, the proposal removes the 4 while consultation with the trustees on concurrence, expedited approval provisions for burning agents under the removal actions as required by OPA guidelines can be used to support current data requirements. The Agency does not equate to a concurrence expedited incident specific requests comments on this approach. requirement, the Agency believes that authorizations. For chemical or such concurrence is highly desirable. biological agents listed on the Schedule (d) Exceptions The Agency is also proposing to revise that are not authorized for use under a The proposed rule maintains the the term ‘‘navigable waters threatened’’ preauthorization plan, the ACs and provision allowing OSCs to authorize to ‘‘waters and adjoining shorelines RRTs should work together to outline the use of any agent, including products threatened’’ to be consistent with the the process for expedited authorization not on the Schedule, when it is provisions in paragraph (a) of this decisions regarding their use. It is determined that the use of the agent is section. important to note that while the NCP necessary to prevent or substantially The preauthorization plan requires that the ACPs include reduce a threat to human life. The requirements in paragraph (a) proposes procedures for expedited decisions, proposed revisions do not change to remove the term ‘‘specific context’’ these procedures can include previous policy, but rather clarify the currently used and instead clearly disapproving the use of agents, or intent of the exception. The Agency establish what the term refers to. The approving the use of agents with certain believes that the protection of human proposal specifically identifies the operational conditions. For example, life is the primary consideration in parameters that must be considered by areas may be designated in which the responding to an oil discharge. Life- the OSC for authorizing agent use. use of certain agents or other discharge Similar requirements are proposed 5 http://www.restorethegulf.gov/release/2011/08/ under paragraph (b). Thus, in meeting 4 http://www.epaosc.org/sites/5083/files/rrt6_ 19/operations-and-ongoing-response-august-17- the provisions of § 300.910(b), the OSC nearshore_dispersant_eap_031605.pdf. 2011.

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threatening oil discharges (e.g., spills of (e) Prohibited Agents environmental samples taken from highly flammable petroleum products in The Agency is maintaining the freshwater, saltwater, groundwater, harbors or near inhabited areas) may current prohibition for the authorization sediment, soil and aquatic biota. NP has occur at locations where chemical of use of sinking agents, and is also been detected in human breast agents on the Schedule are not clarifying that this prohibition also milk, blood, and urine and is associated immediately available. The Agency applies to any other chemical agent, with reproductive and developmental believes that in such cases, an OSC must biological agent, or any substance that effects in rodents. EPA has encouraged have the ability to use agents that, in his acts as a sinking agent when mixed with the ongoing voluntary phase-out of professional judgment, would oil. While certain chemical and NPEs in industrial laundry detergents, effectively and expeditiously mitigate biological agents may submerge oil and intends to evaluate how releases the threat to human life. Allowing this below the water surface (e.g. dispersants and exposures are mitigated through the phase-out action prior to taking any authorization to occur without the are designed to break up oil into small, final regulatory action under the Toxic required concurrences for near neutrally buoyant particles that are Substances Control Act.6 The Agency preauthorization or authorization of use entrained in the water column between believes this prohibition would not for products on the Schedule under the surface and the bottom), they would not be considered ‘‘sinking agents’’ for adversely affect product manufacturers paragraphs (a) and (b) respectively, given there are viable alternatives to the eliminates delays in responding to purposes of the proposed definition and this prohibition, given that they do not use of NP and NPEs in product potentially life-threatening situations. formulations. However, we are The Agency is proposing to include completely submerge oil to the bottom of the water body when applied to an oil requesting comment on the potential ‘‘without obtaining the immediate impacts of modifying existing products discharge. Sinking agents, when applied concurrence’’ to clarify the scope of the to meet this new requirement, including to oil discharges, function by sinking exception. The proposed revisions are cost. consistent with the intent of the current floating oil to the bottom of any body of Alternatively, EPA considered a regulation which recognizes that once water where used, potentially causing broader prohibition from listing and adverse effects on benthic organisms the threat to human life has subsided, from authorizing the use of chemical or vital to the food chain of the aquatic the continued use of a product shall be biological agents formulated with any environment. Additionally, the oil and in accordance with authorization of use endocrine disrupting compounds (EDC). these agents are very difficult to remove. paragraphs (a) and (b) of the section. In EDCs impact exposed organisms by The Agency has similar concerns addition, this exception is intended for altering the hormonal and homeostatic regarding substances that could directly systems that allow them to interact with those extraordinary situations in which cause the oil to submerge to the bottom time is of the essence to mitigate the and respond to their environment. The of the water body when used in an oil group of molecules identified as threat to human life; revising the spill response, and thus it is specifically language to replace ‘‘hazard’’ with potential endocrine disruptors is highly proposing to exclude their use. varied and may be present in chemicals ‘‘threat’’ clearly establishes this. The The Agency is also proposing to add Agency emphasizes this authority is not used as industrial solvents or a prohibition from listing on the surfactants that can be found in intended to circumvent the Schedule and from authorizing use of dispersants and surface washing agents. authorization of use provisions in any chemical or biological agents that Because of the common properties of paragraphs (a) and (b) of this section, contain nonylphenol (NP) or these compounds and the similarities of which serve to address all other nonylphenol ethoxylates (NPEs) as the receptors and enzymes involved in situations. components. This prohibition reflects the synthesis, release, and degradation The proposed revisions also specify the Agency’s concern for these of hormones, no endocrine system is that the OSC immediately notify, and substances, as presented in the EPA immune to endocrine disrupting document the reasons for the use of an Nonylphenol and Nonylphenol compounds.7 agent to the EPA RRT representative and Ethoxylates Action Plan, released The 1996 Food Quality Protection Act the affected states as soon as possible, August 18, 2010. The Action Plan directed EPA to develop a screening specifically addresses nonylphenol (NP) and must obtain their concurrences program, using appropriate validated and nonylphenol ethoxylates (NPEs). where continued use of chemical or test systems and other scientifically NP and NPEs are produced in large biological agents extends beyond 48 relevant information, to determine volumes, with uses that currently lead hours. The Agency believes that whether certain substances may have to widespread release to the aquatic hormonal effects in humans; the 1996 advances in communication environment. NP is persistent in the technologies (e.g., smart phones, email) amendments to the Safe Drinking Water aquatic environment, moderately Act authorized EPA to screen provide OSCs the increased capabilities bioaccumulative, and extremely toxic to substances that may be found in sources to communicate quickly. Therefore, it is aquatic organisms. NP’s main use is in of drinking water for endocrine reasonable to expect that the OSC notify the manufacture of NPEs. NPEs are disruption potential. In response to and explain the circumstances requiring nonionic surfactants that are used in a these mandates, the Agency’s Endocrine use of the agent to the designated EPA wide variety of industrial applications Disruptor Screening Program is RRT representative and, as appropriate, and consumer products. Many of these, developing requirements for the the RRT representatives from the such as laundry detergents, are ‘‘down- screening and testing of pesticides, affected states and the DOC/DOI natural the-drain’’ applications. Some others, commercial chemicals, and resources trustees within 48 hours. The such as dust-control agents and deicers, Agency is requesting comments on these lead to direct release to the 6 For more information, refer to http:// revisions, and specifically on the 48 environment. NPEs, though less toxic www.epa.gov/oppt/existingchemicals/pubs/ hour timeframe within which the OSC and persistent than NP, are also highly actionplans/np-npe.html. 7 shall be operating in accordance with toxic to aquatic organisms, and, in the For more background information on endocrine disrupting compounds and their human health and authorization of use paragraphs (a) and environment, degrade into NP. Both NP environmental effects, please see http:// (b) of the section. and NPEs have been found in www.epa.gov/endo/pubs/edspoverview/index.htm.

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environmental contaminants for their organism’s endocrine system and is responsible party 10 provides the OSC potential to disrupt the endocrine requesting comment on this approach as documentation, developed in system.8 The science related to well. consultation with the submitter of the measuring and demonstrating endocrine The Agency believes the proposed product for listing, prior to product use, disruption is relatively new and prohibitions are appropriate in all cases, affirming the product has maintained its validated testing methods are still being notwithstanding the proposed integrity, including no changes in the developed. When complete, EPA will composition, storage conditions, provisions for case-by-case use use these validated methods or assays to efficacy, and toxicity of any product. In authorization of burning agents under identify and characterize the endocrine such cases where the product expiration § 300.910(c), or for authorization of use activity of pesticides, commercial date has passed but the owner or chemicals, and environmental of any chemical or biological agent operator of the facility/vessel storing the contaminants, specifically in relation to when it is necessary to prevent or product still wants to be able to use the estrogen, androgen, and thyroid substantially reduce an immediate product inventory, EPA proposes that hormones. EPA plans to use the assays threat to human life under § 300.910(d). samples of the expired product lot in a two-tiered screening and testing There are chemical and biological agent representative of all storage conditions process: Tier 1 will serve to identify alternatives to sinking agents and to at any end user location be tested chemicals that have the potential to agents containing NP or NPE, as well as following the applicable testing interact with the endocrine system; and mechanical methods for responding to protocols in Appendix C. The testing Tier 2 will determine the endocrine- oil discharges, including those documentation is to include laboratory related effects caused by each chemical situations that pose extreme threats or information (i.e., contacts, and obtain information about effects at are time critical. accreditations) and all test data and calculations (i.e., raw data and various doses. With this two-tiered (f) Storage and Use of Agents approach, the Agency will gather replicates, notes and observations, information needed to identify Section 300.915 currently requires calculated means and standard endocrine-active substances and take that information be provided on deviations, stock solution preparations, appropriate action, as mandated by recommended conditions of storage and source and preparations of test Congress. To date, EPA has developed use for each product at the time an organisms, test conditions, chain of and validated 11 assays that comprise application for listing a product under custody forms, and summary reports). the Tier 1 Screening Battery. EPA’s Subpart J is submitted to the Agency. Only if the owner or operator can validation effort continues with the This information is summarized in demonstrate that the product has current focus on Tier 2 tests and EPA’s NCP Product Schedule Technical maintained its integrity is the OSC 9 potential replacement assays for Tier 1. Notebook. Specifically, this information allowed to authorize the use of that product inventory. The owner or When all tests are finalized and includes: Special handling and worker operator of the facility/vessel, or their chemical information begins to be precautions for storage and field representative, must re-label the tested collected, EPA may further consider application; maximum and minimum how to incorporate that information into product lots and maintain storage temperatures (optimum ranges documentation of the test results until the Subpart J NCP requirements, and temperatures that will cause phase including additional testing and listing those lots are used or discarded, and separations, chemical changes, or other must retest the expired product lot requirements. Because validated testing alterations to product efficacy); shelf life methods are still being developed, the representative of the product at least of the product; recommended agency is not proposing any test once every 5 years to ensure efficacy application rates and procedures, requirements with respect to endocrine and to allow an OSC to authorize the concentrations and conditions disruption for products to be listed on product for use. The intent of these (considering water temperatures, the Schedule. proposed revisions is to ensure that However, because NP and the NPE are salinity, types and ages of the oil); and products being authorized and used extremely or highly toxic to aquatic any other application restrictions. have maintained their efficacy, even organisms, the Agency is proposing a The Agency proposes to add a new though storage beyond the products’ prohibition specific to Subpart J paragraph (f) to this section that original shelf life may have occurred. products containing NP and NPE as complements the existing information The Agency believes it is the owner or components. The Agency is not requirements for the person or entity operator’s responsibility to ensure that proposing to include a broad submitting a product for listing any product it stockpiles for future use prohibition on Subpart J products that (‘‘submitter’’). The proposed has maintained its efficacy and has not contain substances in which at least part requirements focus on the use of this changed from its listed composition, of the toxic mode of action may include information by the responder and the including the possibility of degrading disruption of the organism’s endocrine OSC. Specifically, the revised into more toxic byproducts, once the system, but is requesting comments on provisions require the OSC to only manufacturer’s expiration date has prohibiting similar substances that may authorize for use those products that are passed. This retesting provision is be found in products/agents that could stored under the conditions specified by supported by the proposed requirements be listed on the Schedule, or to what the the submitter of the product for listing, that the submitter of the product for listing provide not only the criteria should be in order to make that including the maximum, minimum and recommended storage conditions, but determination. As an alternative, the optimum temperatures, humidity and the anticipated shelf life of a product at Agency could require that all product any other relevant conditions. those conditions, and that the product components be tested for a toxic mode Additionally, the Agency proposes to label include both the manufacture and of action that includes disruption of the require that the OSC only authorize for expiration dates, and conditions for use those products whose date of use 8 storage. The flexibility in this proposed http://www.epa.gov/endo/pubs/edspoverview/ does not exceed the expiration date background.htm. listed on the container’s label at the 9 http://www.epa.gov/endo/pubs/assayvalidation/ 10 Responsible party is defined in the NCP under index.htm. time of an incident, unless the 40 CFR 300.5.

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

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for certain chemical and biological discharge.11 This type of application is discharges. The Agency chose 100,000 agents, procedures for authorizing the intended to minimize dispersant U.S. gallons as a threshold criterion for use of those agents, and monitoring dilution in the water before the a major oil discharge because the NCP requirements for certain discharge dispersant has had an opportunity to classifies a discharge of more than this situations. interact with the oil.12 This application quantity to coastal waters as major. In Each oil discharge represents a unique approach that is closer to the source is addition, EPA is proposing to this expected to reduce potential adverse quantity monitoring of dispersant use in situation with distinct conditions, environmental consequences from the response to major oil discharges which may require various response use of excessive quantities of occurring within 24 hours since a larger methods. When dispersants are applied dispersants.13 However, applying quantity of dispersant may be required to an oil discharge, field monitoring can dispersant to an oil discharge does not in a short time frame for an incident of be used to inform operational decisions result in the physical recovery of oil this scale. The Agency also believes by gathering site-specific information on from the environment. Instead, comprehensive monitoring should be the overall effectiveness, including the dispersing oil increases the potential required when surface dispersant is transport and environmental effects of exposure of aquatic organisms to the used for more than 96 hours because of the dispersant and the dispersed oil. dispersant-oil mixture, at least potentially longer exposures of The revisions to product test data and transiently, and subsurface application biological aquatic resources to information requirements are intended has the potential to more immediately dispersant and dispersed oil. Further, to provide OSCs, RRTs, and ACs with and effectively increase these exposures many acute toxicity studies use 96-hour the best information available when near the discharge. The Agency believes exposure durations, including the acute selecting products for use on an oil this new subsurface application toxicity tests using Menidia beryllina discharge. While laboratory test approach requires new environmental described in this proposal. While other protocols allow for comparison between monitoring capabilities to support toxicity tests have shorter exposure different products under standardized operational decision-making. These new durations (e.g., 24, 48, or 72 hours), the laboratory conditions and may be useful monitoring capabilities must be able to Agency believes 96 hours is a during the monitoring and assessment meet the operational conditions (e.g., reasonable threshold given its of a discharge event and/or for selection water depths, temperatures) and be commonality of use in the toxicology of the agents used in the response, they supported by knowledgeable personnel field. Therefore, the proposal requires a do not necessarily reflect field familiar with them. responsible party to implement conditions. Monitoring of agents in the The proposed rule adds § 300.913 monitoring for surface dispersant use in field informs the OSC and other establishing requirements for the response to an oil discharge under these agencies on the overall effectiveness of responsible party to monitor any discharge conditions and for the dispersant use, including the subsurface use of dispersant in response duration of dispersant use. The proposal environmental effects and transport of to an oil discharge, surface use of also requires the submission of a dispersed oil. dispersants in response to oil discharges Quality Assurance Project Plan for of more than 100,000 U.S. gallons approval to the OSC covering the The Agency believes that occurring within 24 hours, and surface collection of all environmental data to comprehensive monitoring in certain use of dispersants for more than 96 ensure and maximize its quality, discharge situations is necessary to hours in response to an oil discharge, as objectivity, utility, and integrity. The determine the overall effectiveness of directed by the OSC. The purpose of Agency welcomes comments on the dispersants and should transcend from monitoring subsurface application is to proposed monitoring requirements, the initial dispersant application to characterize the dispersed oil, follow including the thresholds. Specifically, include the transport and environmental the plume integrity and transport with the Agency requests comments on effects of the dispersant and dispersed the underwater current, and identify whether it should also consider a oil in the water column. Monitoring the and assess the potential adverse effects threshold for surface use of dispersants overall effectiveness of dispersant use in from the dispersed oil. The proposal that is based on the quantity of the field provides those Agencies with requires the responsible party to dispersant used within a given responsibility for authorizing the use of implement monitoring for any timeframe. Alternative thresholds must dispersant product information for subsurface dispersant use in response to include a rationale in order for the EPA decision-making during subsurface or an oil discharge upon initiation and for to consider them for final action. prolonged surface dispersant the duration of subsurface dispersant (a) Dispersant Application applications. Adverse effects on use. The Agency believes monitoring ecological receptors from exposures to subsurface use of dispersants is critical The proposal requires the responsible dispersed oil depend on the length of to inform response actions to minimize party to document the characteristics of time and concentration of the exposure, potential environmental effects. the source oil; best estimate of the oil which in turn is dependent on the While surface application of discharge flow rate, periodically transport of dispersed oil. Because these dispersants is not a new approach and reevaluated as conditions dictate, exposures may vary depending on the understood for small, short duration including a description of the method, discharge situation, the Agency believes discharges, the Agency believes it is associated uncertainties, and materials; comprehensive monitoring is important appropriate to require comprehensive dispersant(s) product used, rationale for for certain discharge situations. This monitoring for situations where dispersant choice(s), including the monitoring data will enhance the dispersants are used for an extended results of any efficacy and toxicity tests, information needed for an effective period of time or in cases of major oil recommended dispersant-to-oil ratio; response without delaying the use of and the application method and 11 http://marinewellcontainment.com/expanded_ agents under these conditions. procedures, including a description of system.php. the equipment to be used, hourly Equipment is being contemplated to 12 NRC, (2005), Oil Spill Dispersants: Efficacy and Effects, The National Academies Press, pp. 138, application rates, capacities, and total inject dispersants subsurface, directly http://www.nap.edu/catalog.php?record_id=11283. amount of dispersant needed. For into the oil near the source of the 13 Ibid. subsurface discharges, the proposal also

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

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In-Situ Scattering and Transmissometry analysis provides important data useful oil in the water column, as well as an (LISST) instrument or other similar in optimizing operational guidelines indicator of dispersion effectiveness as instruments. Small oil droplets (e.g., and decision making, modeling discussed in the following section. The diameters in the tens of mm range) have transport and fate, and potentially Agency request comments on alternative such low rise velocities that they tend evaluating biological effects of spectroscopy techniques such as to remain suspended in the water chemically dispersed oil. The proposal absorption measurements that may be column (neutrally buoyant), where they also includes larger oil droplet sizes of used to rapidly estimate oil can become widely dispersed by up to 2000 mm, intended to provide concentrations in the water during a advective forces, turbulent motion, and information that can inform the oil discharge event. to a lesser extent diffusion. These small distribution using trajectory modeling • Fluorescence signatures. In addition droplets are more readily amenable to analysis. to in-situ fluorometry, the proposal biodegradation due to their higher • In-situ fluorometry. When exposed requires the responsible party to surface area to volume ratio. In contrast, to ultraviolet (UV) light, certain conduct a fluorescence intensity large oil droplets (e.g., diameters >100 compounds absorb energy that can analyses on water samples collected to mm) will tend to recoalesce and rise elevate electrons into an excited higher determine fluorescence signatures of the faster to the surface.16 Effective energy level. The wavelength that dispersed oil. EPA proposes to use application of dispersants is expected to excites electrons into a higher energy fluorescence signatures as a relatively generate a larger number of small state is typically referred to as the simple and rapid means to assess droplets, reducing the average droplet excitation wavelength. Electrons dispersion effectiveness. This includes size.17 This will change the trajectory of unstable at the higher energy state but is not limited to, identifying the rising oil that is subjected to stratified return to a lower energy state, emitting peak wavelength position, magnitude horizontal subsurface currents. Near the energy at longer emission wavelengths and ratios of fluorescence intensity of water surface, hydrodynamic and other resulting in fluorescence.19 Many the dispersed oil. For example, environmental factors also influence the organic compounds fluoresce at specific measuring the reduction in an intensity oil droplet size distribution. Mixing excitation and emission wavelengths ratio after applying dispersant to the oil energy, especially from breaking waves, that allow for identifying many of the in seawater may provide an estimate of 23 24 dictates the breakup of large oil droplets components of dissolved organic matter the effect of chemical dispersion. into smaller droplets and the depth of and other compounds (e.g., crude oil) in Ratios of fluorescence intensity are submergence of the droplets. Plunging seawater.20 For crude petroleum oils, derived from the three dimensional breaking waves under experimental the aromatic fraction is responsible for excitation/emission matrix spectra conditions produced the smallest oil the fluorescence property of petroleum, (EEMS) acquired by combining multiple 13 14 droplets. Additionally, studies and these compounds are used to emission spectra obtained from oil indicate that the type of chemical determine the specific excitation and exposed to individual excitation dispersant used is an important factor in emission wavelengths for monitoring. wavelengths typically using a scanning controlling the dispersed oil droplet size When subject to excitation at certain spectrofluorometer. If the optimal distributions. Further, wave tank studies wavelengths in the near ultraviolet excitation and emission bands are have shown that the chemically spectrum, polycyclic aromatic known, then these ratios may be derived dispersed oil may result in a droplet hydrocarbons (PAH) fluoresce over a from measuring the fluorescence size distribution that has not been range of higher wavelengths, depending intensity at two different fixed emission wavelengths at a single fixed excitation observed without the use of dispersants on the number of aromatic rings in the wavelength. The ratios are calculated by (i.e., physically dispersed oil), both in structure.21 Fluorometers can be dividing the fluorescence intensity of terms of a smaller volumetric mean targeted to the type of oil discharged, the shorter emission band by the diameter and a bimodal distribution for and the excitation and emission 18 fluorescence intensity of the longer droplet size diameters below 100 mm. wavelengths chosen should match the band. Studies have shown that adding EPA recognizes that the aforementioned aromatic properties of the oil dispersants to crude petroleum oil studies were conducted under discharged. Although this measure does increases the fluorescence intensity of conditions characteristic of surface not include all oil constituents, the longer emission band, driving down waters. However, the effect of the high fluorescence is a valuable screening tool velocities of oil that may occur from a 22 the value of the ratio. Although deployed during a response, providing individual petroleum oils may have discharge from a subsurface oil well on a rapid indication of potential dispersed the oil droplet size distribution requires common spectral characteristics, the ideal three-dimensional EEMS for the further scientific investigation to 19 Henry, C.B., Roberts, P.O., Overton, E.B., A understand the contribution of Primer on In Situ Fluorometry to Monitor Dispersed discharged oil should be obtained from physically dispersed oil relative to Oil, IOSC 1999;246. scanning the source oil. Therefore, the chemically dispersed oil. In either 20 Coble, P.G., (2007) Marine Optical monitoring should include procedures event, it is clear droplet size distribution Biogeochemistry: The Chemistry of Ocean Color, to obtain the EEMS using the source oil Chem. Rev., Vol. 107, pp. 402–418. to determine the optimal excitation- 21 Bugden, J.B.C., Yeung, C.W., Kepkay, P.E., Lee, 16 Li, M. and Garrett, C., (1998) The Relationship K. (2008) Application of Ultraviolet Fluorometry emission wavelengths. The Agency Between Oil Droplet Size and Upper Ocean and Excitation-Emission Matrix Spectroscopy Turbulence, Mar. Poll. Bull., Vol. 36, pp. 961–970. (EEMS) to Fingerprint Oil and Chemically 23 Bugden, J.B.C., Yeung, C.W., Kepkay, P.E., Lee, 17 Li, Z., Lee, K., King, T., Boufadel, M.C., Venosa, Dispersed Oil in Seawater, Mar Pollut Bull, Vol. 56, K. (2008) Application of Ultraviolet Fluorometry A.D., (2008) Assessment of Chemical Dispersant pp. 677–685. and Excitation-Emission Matrix Spectroscopy Effectiveness in a Wave Tank under Regular Non- 22 Conmy, R.N., Coble, P.G., Farr, J., Wood, A.M., (EEMS) to Fingerprint Oil and Chemically Breaking and Breaking Wave Conditions, Mar Pollut Lee, K., Pegau, W.S, Walsh, I.D., Koch, C.R., Dispersed Oil in Seawater, Mar Pollut Bull, Vol. 56, Bull, Vol. 56, pp. 903–912. Abercrombie, M.I., Miles, M.S, Lewis, M.R., Ryan, pp. 677–685. 18 Li, Z., Lee, K., King, T., Boufadel, M.C., Venosa, S.A., Robinson, B.J., King, T.L., Kelble, C.R., and 24 Kepkay, P.E., Yeung, C.W., Bugden, J.C.B., Li, A.D., (2009) Evaluating Chemical Dispersant Lacoste, J. (2014) Submersible Optical Sensors Z., and Lee, K. (2008) Ultraviolet Fluorescence Efficacy in an Experimental Wave Tank: 2— Exposed to Chemically Dispersed Crude Oil: Wave Spectroscopy (UVFS): A New Means of Determining Significant Factors Determining In Situ Oil Droplet Tank Simulations for Improved Oil Spill the Effect of Chemical Dispersants on Oil Spills, Size Distribution, Env Eng Scien, Vol. 26, pp 1407– Monitoring, Environ Sci Technol, Vol. 48, pp. IOSC, pp. 639–644. http://ioscproceedings.org/doi/ 1418. 1803–1810. abs/10.7901/2169-3358-2008-1-639.

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

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

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

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

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

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persistent organic pollutants, having working towards standardization of evaluated every ingredient in the toxic effects such as endocrine laboratory accreditations throughout the product to ensure it meets DfE’s disruption. PAHs are potent industry; ILAC is the international stringent criteria. Products that meet the atmospheric pollutants, of concern counterpart collaboration of laboratory DfE criteria are safer chemical choices. because some compounds have been and inspection accreditation bodies. In an effort to encourage the identified as carcinogenic, mutagenic, Established to ensure that laboratories development and use of safer and teratogenic. The proposed threshold are subject to oversight by an technologies, the Agency is proposing a requirements for all of these authoritative body, accreditation requirement for the submitter to identify contaminants is intended to provide organizations have been evaluated by products that have met and can be information for listing decisions that peers as competent and have signed labeled DfE certified as part of the ensure the use of any product will not arrangements to enhance the acceptance general information, and would include result in exceeding established water of products and services. Because this information in the NCP Product safety levels. The Agency requests interested parties can have confidence Schedule Technical Notebook.34 This comments on whether it should in the test results and certifications Technical Notebook presents establish a listing threshold for products provided by accredited laboratories, the manufacturer’s summary information on based on these criteria, and whether the Agency is proposing to amend the the conditions under which each levels selected for certification are the laboratory requirement and believes that product is recommended to be used, appropriate levels for this application. having no prior experience with a and is a source of information for the The Agency also requests comments on specific methodology should not OSC in the event of a response. whether there are any other disqualify a laboratory that has been (14) International product contaminants that should be included accredited by an appropriate certifications, testing or use data for evaluation of a product prior to authoritative body. However, the informing the performance capabilities listing. Agency reserves the right to not accept or environmental benefits of the product. The Agency believes that any (11) Removal of the requirement for particular lab data should EPA find additional data available from other laboratories performing the efficacy and cause to doubt the quality and integrity of the work. EPA also reserves the right countries may help identify the benefits toxicity testing for products to have to conduct its own testing of any or concerns for the listing and/or the prior experience specific to the required product. authorization of use of a product. The methodology in lieu of recognized (12) Estimated annual product Agency, however, is not proposing any national or international accreditations. production volume, average and specific listing criterion or threshold Currently, laboratories performing maximum amounts that could be associated with this broad information testing for products to be submitted for produced per day, and time frame request, as some products (particularly listing consideration are required to needed to reach maximum production new formulations) may not have any of document previous experience with the rate (days). While there is currently no this additional data available. specific testing methodologies in requirement for production capability Appendix C to part 300. The Agency information, the Agency believes it is (b) Dispersant Testing and Listing believes it is more appropriate to require important for the OSCs and responders Requirements that laboratories be nationally or to have this information. The The Agency is proposing revisions to internationally accredited. Accredited availability of a product may impact the efficacy and toxicity testing laboratories are expected to be capable decisions of authorization of use, protocols, as well as establishing new of following a prescribed testing depending on inventory or production thresholds for listing dispersants on the protocol and good general practices, capabilities. This would prove to be of Schedule in § 300.915(b). The Agency providing assurance that the test results key importance, for example, in the proposes to define dispersants as will be reliable. Therefore, the Agency event of a major environmental disaster typically mixtures of solvents, is proposing to remove the requirement (e.g., a SONS event). surfactants, and additives that promote for laboratories to have previous (13) Recognition received from EPA’s the formation of small droplets of oil in experience specific to the Design for the Environment (DfE). EPA’s the water column by reducing the oil- methodologies in Appendix C, and Design for the Environment (DfE) 33 water interfacial tension. These droplets instead require that the laboratories works in partnership with industry, are driven into the water column by hold accreditations from recognized environmental groups, and academia to wave action. Emergency response national or international organizations. reduce risk to people and the personnel need to know whether a National and international accreditation environment by finding ways to prevent dispersant or any other type of chemical organizations include, for example, the pollution. DfE evaluates human health or biological agent on the Schedule International Organization for and environmental concerns associated could have negative environmental Standardization (ISO), and the with traditional and alternative impacts relative to the oil before Laboratory Accreditation Bureau chemicals and processes in a range of decisions are made about its use in a (recognized in the US through the industries in order to select safer particular oil discharge situation. National Cooperation for Laboratory chemicals and technologies. DfE focuses Consequently, it is essential to consider Accreditation (NACLA) and the its review of formulation ingredients on comparative information about the International Laboratory Accreditation key environmental and human health efficacy and the toxicity of these Cooperation (ILAC)). The ISO 17025, characteristics of concern within products. The proposed revisions are in Laboratory Competence standard, functional classes. This allows response to concerns not only for an identifies high technical competence formulators to use those ingredients increase in the frequency of planning for and management system requirements with the lowest hazard in their the use of these agents, but also for their to guarantee laboratory test results and functional class, while still formulating potential use in large quantities, such as calibrations are consistently accurate. high-performing products. The DfE label when responding to oil discharges from NACLA is a national voluntary means that EPA scientists have organization of regulators, accreditation 34 http://www.epa.gov/oem/docs/oil/ncp/ bodies and laboratories cooperatively 33 http://www.epa.gov/dfe/. notebook.pdf.

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oil tanker accidents and offshore well Intermediate Fuel Oil (IFO–120) were Additionally, the Agency is proposing blowouts, as evidenced during the tested for this proposal. Both oils are to that efficacy testing be conducted at two Deepwater Horizon incident in 2010. be tested at two temperatures: 5 °C and different temperatures, 5 °C and 25 °C, 25 °C. Finally, based on the ANS and rather than at an ambient temperature (1) Dispersant Efficacy IFO–120 testing, the Agency proposes range of 20–23 °C as currently required. Current Requirements: The current that dispersants considered for listing The Agency recognizes the current and NCP Subpart J requires dispersants to be must demonstrate that they attain all of future interest in arctic and deepwater tested for saltwater efficacy in order to the following dispersant effectiveness drilling, and the continued oil determine listing eligibility on the (DE) values: production in the southern, more Schedule. Dispersant efficacy is tested • ° ≥ tropical areas of the country. Given the following the Swirling Flask Test (SFT) ANS at 5 C: DELCL95 70%. • ° ≥ potential range of locations where listed in Appendix C to part 300 of the ANS at 25 C: DELCL95 75%. dispersants may be used, the Agency • ° ≥ NCP. This protocol was developed by IFO–120 at 5 C: DELCL95 55%. believes it is appropriate to have Environment Canada to provide a • IFO–120 at 25 °C: DELCL95 ≥65%. products tested at temperatures that relatively rapid and simple testing The Agency tested eight of the would reflect that range. These procedure for evaluating dispersant dispersants currently listed on the temperatures are intended to capture efficacy (i.e., the percentage of oil that Schedule. Three of the eight dispersants dispersant use scenarios in a wide range is dispersed). The procedure places clearly differentiated themselves from of geographic locations and under seawater, oil, and a dispersant into an different temperatures that may occur in Erlenmeyer flask, which is then placed the other five dispersants for having the best DE efficacy results; they would the same geographical location (such as, on a shaker table for a specified period LCL95 for example, the deep sea and surface of time. The flask is modified by the meet all the proposed thresholds. For the next best dispersant tested, the water in the Gulf of Mexico, where the addition of a side spout attached to the temperatures are typically 5 and 25 °C, bottom of the flask, which allows the results were substantially lower than those in the top group and would not respectively). analyst to pour off dispersed oil from The Agency is also proposing to meet all the thresholds proposed today. the bottom into a collection vessel for replace the current SFT with the BFT, This natural break in the results extraction and measurement. After 20 which is designed to be more provided the Agency with the basis for minutes, a sample of water is poured off representative of moderately turbulent and chemically analyzed for dispersed the proposed threshold criteria. The sea conditions where dispersants are oil. For products to be listed, they must Agency is also proposing to replace the more likely to be successful when used. attain an efficacy value of 45 percent or SLC and PBC test oils currently used for The revised testing protocol improves greater average dispersion efficacy of efficacy testing with two other oils that test repeatability and reproducibility two different crude oils (South represent a wider range of within and between laboratories, as well Louisiana Crude (SLC) and Prudhoe Bay characteristics. The proposal is based on as greatly reduces both the inherent Crude (PBC)) at room temperature (20– the results of tests using ANS and IFO– error of the method and the human error 23 degrees Celsius (°C)). 120 oils with the new protocol. In associated with the current SFT, as Proposed Revisions: The Agency proposing two new oils for efficacy discussed below. In addition, reporting proposes to change the testing protocol testing, the Agency is seeking to ensure the test results in terms of the product’s that the efficacy testing uses oils that for measuring efficacy and adopt the LCL95 accounts for between- and within- Baffled Flask Test (BFT) as the testing represent a wider range of oil gravities laboratory error variability and the protocol for dispersant efficacy. The throughout the different geographic inherent error of the method. Only one new BFT procedure incorporates a locations in the country where number is reported compared to a mean redesign of the testing flask by dispersants might be used. The oils and standard deviation, as the variation eliminating the side arm, incorporating selected should exhibit sufficiently has already been subtracted in the baffles in the wall of the flask, and different characteristics to produce reported number. Specifically: adding a stopcock at the bottom, which results that have statistically significant • The new baffled trypsinizing flask improves reproducibility in the hands of variation between them. The proposal is design, fitted with a glass stopcock different operators. This protocol has to replace the SLC and PBC oils, both positioned at the bottom side, promotes undergone extensive peer review 35 and of which were light oils, with a range of less manipulation that could result in has been tested in several laboratories, light-to-medium, and heavier oils. The erroneous re-suspension of non- providing reproducible and repeatable light-to-medium gravity ANS pipeline dispersed oil, as in the SFT. The re- results. The Agency also proposes blend and the heavier refined product, suspension of oil when using the SFT revisions to the efficacy listing criteria IFO–120 were selected for testing the test protocol was a major source of error. for dispersants to be listed. Specifically, protocol in this proposal. The current In the SFT, the flask has a side arm the dispersant must demonstrate that protocol, testing 4 replicates of both the spout, requiring the analyst to pick up the lower 95% confidence level (LCL95) SLC and the PBC oils and combining the flask and pour the contents out of six replicate flasks meets the new their results, provided one threshold manually. Through that action, re- proposed efficacy listing criteria at two criterion after determining that each of suspension of the dispersed oil can test temperatures. New test oils the oils produced statistically similar easily take place, leading to potentially representing a wider range of results. In contrast, the efficacy test erroneous results. In contrast, in the characteristics are also proposed for this results between the ANS and the IFO– BFT, the flask contains a stopcock at the protocol: Alaska North Slope (ANS) and 120 showed statistically significant bottom, so the analyst need only open differences at each temperature. The the stopcock to drain the contents from 35 Venosa, Albert D., National Risk Management Agency believes the use of ANS and the flask without the potential of Research Laboratory, US EPA; Sorial, George A., IFO–120, or similar oils that represent a remixing or re-suspending the dispersed Department of Civil & Environmental Engineering, wider range of oil gravities, will provide oil. University of Cincinnati; King, Dennis W., Statking • Consulting; Round-Robin Testing of a New EPA better information on the efficacy of the The BFT provides more turbulent Dispersant Effectiveness Protocol, International Oil products when used on different types mixing and better enables more Spill Conference, 2001. of oils. reproducible and repeatable dispersant

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action than the SFT. The mixing energy authorization for use, as the alone, and the dispersant mixed with within the flask is higher and, as a result temperatures may change drastically in both oils used for efficacy testing; the of this increased mixing energy, better some geographical regions affected by proposal is based on the ANS and IFO– dispersion is possible. Turbulence is the same oil discharge. Even within 120 oils. While the Agency currently needed for the proper mixing of more stable geographical regions, there provides the toxicity testing results to dispersant and oil and for producing the may be variations at the time of an oil the OSC to assist in authorization of use sheer forces needed to create the small discharge that could affect the decision determinations, it is proposing to use droplet sizes with high surface area-to- to use a dispersant stockpiled for a these testing results to determine volume ratio that promote the effective different temperature range. While these eligibility for listing on the Schedule. dispersion of the oil into the water more specific listing approaches would Specifically, the Agency is proposing column. The BFT provides such mixing provide more information on effective to require evaluations of dispersant and better enables more repeatable and product choices, the Agency is toxicity using acute toxicity tests reproducible dispersant effectiveness concerned about how such specific following existing USEPA effluent than the SFT. The BFT was tested listing approaches may contribute to testing guidelines,39 40 modified for use extensively in a nine-participant round- OSC confusion in an emergency, the with dispersant product or dispersant robin inter-laboratory calibration test on cost of stockpiling multiple types of product/oil mixtures, as detailed in six commercial dispersant products.36 dispersants, or the immediate Appendix C to part 300. Measured In addition, based on the mixing energy availability of the appropriate toxicity values for dispersant product that can be achieved using the new dispersant in an emergency. and dispersant product/oil mixtures are baffled flask, the Agency believes a Furthermore, the Agency is proposing proposed to include static acute toxicity higher efficacy threshold is warranted. revisions to Subpart J to authorize RRTs tests using A. bahia and M. beryllina. As a result of this increased mixing to request supplementary testing and Developmental toxicity using a sea energy, better dispersion is realized information to provide greater flexibility urchin assay, and sub-chronic effects under conditions more realistic of wave in tailoring testing conditions to address using A. bahia and M. beryllina are also action in the sea. area- and site-specific concerns. Given proposed to be conducted, but with • The variability both between these factors, the Agency believes that it dispersant product only. The Agency is analysts and within analysts is is appropriate that only those proposing the following toxicity substantially lower for the BFT dispersants that achieve efficacy for thresholds for listing dispersants on the both types of oils and at both Schedule: compared to the SFT, as measured by • the coefficient of variation (CV). The CV temperatures be listed. Listing only the Lethal concentration for 50% of the is defined as the standard deviation products that achieve efficacy for both test species (LC50) at the lower 95% divided by the mean and is expressed in types of oils at both temperatures would confidence interval for all acute toxicity terms of percent; the higher the CV, the demonstrate a wide range of efficacy for tests greater than 10 ppm; • Inhibition concentration for 50% of greater the variability.37 38 the product, and a single listing would The Agency considered establishing facilitate authorizing their use during a the test species (IC50) at the lower 95% listing thresholds for efficacy based on response action. The Agency requests confidence interval greater than 10 ppm; • No Observed Effect Concentration the types of oil. The Schedule could list comments on this approach. (NOEC) equal to or greater than 1 ppm sub-categories of dispersants based on (2) Dispersant Toxicity for sub-chronic toxicity. gravities of the oil (i.e., light-medium or Test Oils and Oil Acute Toxicity heavy), so that a dispersant would only Current Requirements: The current NCP Subpart J requires dispersants to be Values. The Agency proposes to replace be authorized for use on oils that fall the No. 2 fuel oil currently used for within the range for which it tested tested for toxicity to saltwater species. This information is available to the OSC toxicity testing with two test oils that effective. Similarly, the Schedule could better represent a wider range of list dispersants based on temperature, for their consideration in authorizing dispersant use. Dispersant toxicity is characteristics and that may be allowing a dispersant to be authorized tested following the protocols in encountered during an incident. The for use only at the temperature for Appendix C to part 300 of the NCP. The proposal is based on ANS and IFO–120, which it tested effective. However, standard toxicity test for dispersants as previously discussed. In addition to determining ranges or definitions for involves exposing two saltwater species, making the test oils consistent with the when oil changes from light to medium the inland silverside fish (Menidia dispersant efficacy tests, testing oils of or heavy, is challenging because they beryllina or M. beryllina) and the mysid different gravities also provides a better may be affected by a number of external shrimp (Americamysis bahia or A. estimation of dispersant/oil toxicity factors, including temperature. bahia), to five concentrations of the test associated with differing oil Likewise, listing dispersants based on product and No. 2 fuel oil, alone and in constituencies, and ultimately a better temperature would require an a 1:10 mixture of product to oil. representation of the potential overall additional degree of complexity to the Reference toxicity tests are conducted toxicity of a product. using dodecyl sodium sulfate (DSS) as The Agency proposes to conduct the 36 Venosa, A. D., D. W. King, and G. A. Sorial. oil-only acute toxicity tests for the two 2002. The Baffled Flask Test for Dispersant a reference toxicant. The test length is Effectiveness: A Round Robin Evaluation of 96 hours for M. beryllina and 48 hours reference oils, with both A. bahia and Reproducibility and Repeatability. Spill Sci. & for A. bahia. The concentration of test Technol. Bulletin 7(5–6):299–308. product causing 50% lethality to the test 39 USEPA 2002a Methods for Measuring the 37 Sorial, G. A., A. D. Venosa, K. M. Miller, E. organisms (LC ) is calculated at the end Acute Toxicity of Effluents and Receiving Waters to Holder, and D. W. King. 2004a. Oil Spill Dispersant 50 Freshwater and Marine Organisms, Fifth edition. Effectiveness Protocol—Part I Impact of Operational of the exposure period. (Acute Methods Manual), Office of Water, Variables. ASCE. J. Env. Eng. Div., 130(10):1073– Proposed Revisions: The Agency Cincinnati, OH. EPA–821–R–02–012. 1084. proposes to revise the toxicity testing 40 USEPA 2002b. Short-term Methods for 38 Sorial, G. A., A. D. Venosa, K. M. Miller, E. requirements for dispersants, including Estimating the Chronic toxicity of Effluents and Holder, and D. W. King. 2004b. Oil Spill Dispersant Receiving Waters to Marine and Estuarine Effectiveness Protocol—Part II Performance of the the testing protocol and the use of the Organisms, Third Edition. (Saltwater Chronic Revised Protocol. ASCE ASCE. J. Env. Eng. Div., test results. The proposal would require Methods manual). Office of Water, Cincinnati, OH. 130(10):1085–1093. acute toxicity testing for the dispersant EPA–821–R–02–014.

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

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

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evaluation prior to listing on the surface to which the oil can adhere. The proposes to require surface washing Schedule. Changes over established Environment Canada method uses a agents be tested for acute toxicity using protocols the Agency considered stainless-steel ‘trough’ which is placed fresh water species Ceriodaphnia dubia include: Using natural substrates to at a specified angle. The target oil is and Pimephales promelas, or saltwater reflect the most commonly impacted placed on an area on the trough. The species Americamysis bahia and shoreline material; establishing treating agent is then applied in droplets Menidia beryllina, or both, depending sufficient weathering time to permit to the surface of the oil and after 10 on the intended product use. The strong attachment of the oil to the minutes at 5-minute intervals, rinses of concentration of test product causing substrate surface; fully quantifiable water are applied to the trough. After 50% lethality to the test organisms approaches with known volumes and drying, the trough is weighed and the (LC50) and lower and upper 95% precise measurements to allow mass removal calculated from the weight loss. confidence intervals (LCI95 and ULCI95) balance; and a standardized and Repeatability is within 5%. The Agency are calculated at the end of the exposure reproducible methodology to minimize is requesting comment on available period. To be listed on the Schedule, operator error. PBC oil was used as the methodologies and its published surface washing agents must representative standard reference oil in protocol to incorporate as the testing demonstrate an acute lethal developing the protocol since it had protocol for these agents. The Agency concentration for 50% of the test species previously been selected as one of two also requests comment on whether the (LC50) at the lower 95% confidence standard oils for the Agency’s published rule should identify the specific interval greater than 10 ppm in either protocols for dispersant and methodologies to be used until EPA fresh or salt water, consistent with the bioremediation agent testing. However, develops and adopts a new testing acute toxicity thresholds proposed for the Agency is proposing revisions to the protocol for SWA efficacy testing. dispersants. EPA’s toxicity classification 55 dispersant and bioremediation testing The Agency is also proposing an scheme classifies LC50 values ranging protocols, including replacing the PBC efficacy threshold of 30% in either fresh from 10 ppm to 100 ppm as slightly reference oil. The protocol being or salt water or both depending on the toxic and values above 100 ppm developed has not been tested: With the intended product use. This is based on substances are considered practically IFO–120 or the ANS oils that are the efficacy data published in ‘‘Surface- nontoxic to aquatic organisms. By proposed to be used in the revised washing Agents or Beach Cleaners.’’ 48 proposing this threshold level, the dispersant efficacy testing protocol; at Numerous surface washing agent Agency is establishing an adequate multiple temperatures; or to include products, including several from the safety margin without being overly freshwater systems. The Agency expects Schedule were tested using the restrictive. The Agency requests to develop final recommendations for Environment Canada methodology. The comments on the proposed acute the testing protocol following round average efficacy of the surface washing toxicity methods (or any others robin testing after adjusting for the new agents tested is approximately 30%. The available) and thresholds for surface variables. The Agency would propose Agency requests comments on this washing agents. this protocol in the Federal Register approach and other efficacy test data The Agency is proposing provisions through notice and comment before available. for conducting acute toxicity tests with adopting it as part of Subpart J dispersant-oil mixtures, but not for any requirements. (2) Surface Washing Agent Toxicity other agent, including SWAs. EPA Consequently, because of the Current Requirements: The current believes that non-dispersant products additional work needed to finalize its NCP Subpart J requires surface washing are not likely to be used in the same protocol, the Agency is proposing to agents to be tested for saltwater species quantities or durations as dispersants allow the use of standard recognized toxicity. Surface washing agent toxicity and some may be recovered making a efficacy testing methodologies for is tested following the dispersant requirement to conduct toxicity tests of surface washing agents. An example of toxicity testing protocols in Appendix C product/oil mixtures unnecessary. such a standard recognized to part 300 of the NCP. There may be concerns, however, for methodology is the American Society Proposed Revisions: The Agency is increased product toxicity because of for Testing and Materials (ASTM) proposing revisions to the toxicity their interaction with the oil. Thus, the Standard Test Method for Evaluating the testing requirements for surface washing Agency is requesting comment on the Effectiveness of Cleaning Agents.52 agents, including the testing protocol. need for acute toxicity tests conducted Another methodology is Environment While the Agency currently provides with surface washing agents-reference Canada’s Test Method.53 The capability the toxicity testing results to the OSC to oil mixtures. A protocol for preparation of a particular surface washing agent assist in authorization of use of product/oil mixtures for toxicity depends upon the application determinations, it is proposing to use testing is available for review in the procedures and the characteristics of the these toxicity testing results to docket. surface being cleaned, such as size, determine listing eligibility on the (3) Limitations shape, and material. The ASTM test Schedule. method in particular covers a procedure The proposed revisions to the testing The Agency is proposing a for evaluating the capability of the protocols for surface washing agents are conditional use listing for SWAs. The agents, providing a relatively rough detailed in Appendix C to part 300. The proposal specifies that these products proposed acute toxicity test protocol for may only be used in those water 52 ASTM Standard Test Method for Evaluating the surface washing agents is based on environments for which the product Effectiveness of Cleaning Agents. Designation: was tested and for which it met the G122—96 (Reapproved 2008). ASTM International, EPA’s protocol, Methods for Measuring 100 Barr Harbour Dr., P.O. Box C–700 West the Acute Toxicity of Effluents and listing threshold criteria. The Agency Conshohocken, Pennsylvania 19428–2959, United Receiving Waters for Freshwater and recognizes that products may yield States Marine Organisms.54 The Agency effective results in certain environments 53 Fingas, Merv and Fieldhouse, Ben; ‘‘Surface- and not in others. Products that may be washing Agents or Beach Cleaners’’ (2010). Chapter 21 Surface-Washing Agents or Beach Cleaners. In 54 http://water.epa.gov/scitech/methods/cwa/wet/ Oil Spill Science and Technology (p716). London: upload/2007_07_10_methods_wet_disk2_atx1- 55 USEPA 2010. http://www.epa.gov/oppefed1/ Gulf Professional Publishing. 6.pdf. ecorisk_ders/toera_analysiseco.htm#Ecotox.

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effective in freshwater environments with the chemical analysis, a resolved aromatics was achieved in that may not necessarily be so in saltwater microbiological analysis is also time period. Product flasks contain environments, and vice versa. The performed to determine and monitor the exposure water, weathered oil, and Agency is proposing this limitation to viability and growth of the microbial product in concentrations specified by allow product manufacturers the cultures being studied. For commercial the manufacturer. Positive control flasks flexibility to select which environment products that are strictly microbial must contain exposure water, oil, the product is to be tested and agents not containing their own nutrients, and the standard culture authorized for use, either saltwater, nutrients, a mineral nutrient solution is supplied by the Agency. A negative fresh water, or both environments. provided if requested by the submitter; control, consisting of artificial exposure Therefore, the product would be listed no further nutrients are added to water, product, weathered crude oil, and could only be authorized for use in commercial products containing their nutrients, and a sterilant is also used to those water environments for which it own nutrients. To be listed on the ensure that the observed degradation of was tested and for which it met both the Schedule, bioremediation agents must hydrocarbons was not caused by abiotic efficacy and toxicity listing criteria. demonstrate a statistically significant losses or interaction with the product. difference between the average The Agency is requesting comment on (d) Bioremediation Testing and Listing degradation of both total alkanes and whether an additional protocol specific Requirements total aromatics in the oil achieved by to products containing enzymes only The Agency is proposing to define the product after 28 days and the would be appropriate; this would bioremediation agents as biological average degradation for the same consist only of exposure water, agents and/or nutrient additives compounds achieved by the non- weathered oil and the enzymatic deliberately introduced into a nutrient control in the same time product in the concentrations specified contaminated environment to increase period. by the manufacturer. The proposed the rate of biodegradation and mitigate Proposed Revisions: The proposal protocol quantifies the degradation (or any deleterious effects caused by the reflects a series of changes to the current disappearance) of alkane hydrocarbons contaminant constituents. efficacy testing protocol for and aromatic hydrocarbons. The sample Bioremediation agents include bioremediation agents. The protocol preparation procedure extracts the oil microorganisms, enzymes, and nutrient includes freshwater testing in addition phase into the solvent dichloromethane additives such as fertilizers containing to the current saltwater-based test, and (DCM; also known as methylene bioavailable forms of nitrogen, uses artificial water for both fresh and chloride) with a subsequent solvent phosphorus and potassium. For this saltwater testing, replacing the natural exchange into hexane. The test method agent category, the Agency is proposing seawater currently used. The proposed targets the relatively easy to degrade to revise the efficacy testing protocols, protocol also eliminates several normal alkanes and the more resistant to establish toxicity testing protocols, gravimetric and microbiological and toxic aromatics. The analytical and to establish both efficacy and analyses and testing endpoints not used technique uses a high resolution GC/MS toxicity listing thresholds in in the proposed listing determinations. because of its high degree of chemical § 300.915(d). Additionally, the proposed protocol separation and spectral resolution. GC/ limits the levels at which external (1) Bioremediation Agent Efficacy MS has long been used to study the nutrients may be added, which allows weathering and fate of oil spilled into Current Requirements: the addition for product formulations the environment. It gives unambiguous without nutrients, or for product Bioremediation agent efficacy is results for determining biodegradation formulations that have nutrient currently tested following the protocols efficacy. For quantitative analyses, the concentrations at insufficient levels for in Appendix C to part 300 of the NCP. instrument is operated in the selected the experimental setup. Finally, the The current bioremediation agent ion monitoring mode (SIM) of detection methodology streamlines the statistical efficacy testing protocol is designed to at a scan rate of > 5 scans per second analysis. The proposed revisions determine a product’s ability to to maximize the linear quantitative address concerns with the existing biodegrade oil by quantifying changes in range and precision of the instrument. methodology as discussed below, the oil composition resulting from Fresh and Saltwater Environments. biodegradation using natural seawater expanding its application to include freshwater environments, improving the The existing bioremediation test is as the test water. The protocol tests the exclusively for saline environments bioremediation agent for microbial consistency and comparability of the test results, and generally streamlining with no equivalent test for freshwater activity and quantifies the environments. Further, the existing test disappearance of saturated the protocol. Protocol. The proposed efficacy uses natural seawater and has been hydrocarbons and PAHs in weathered testing protocol is designed to found to give variable results due to the oil; for purposes of the proposal the determine a bioremediation agent’s compositional variability of seawater Agency tested the protocol using ANS ability to biodegrade weathered crude both chemically and microbiologically. 521.56 The sample preparation oil in the exposure water (saltwater or The Agency proposes to replace the procedure extracts the oil phase into freshwater) by quantifying changes in natural seawater with a standardized dichloromethane (DCM), with a the oil composition resulting from artificial saltwater formula called GP2, subsequent solvent exchange into biodegradation. It consists of a series of whose components and concentrations hexane. The analytical technique uses a six product and control flasks are generally recognized, and which is high-resolution gas chromatograph/mass containing artificial seawater or easily made. The use of artificial spectrometer (GC/MS); GC/MS provides artificial freshwater and weathered saltwater allows for better test for a high degree of chemical separation crude oil in which biodegradation of the reproducibility. Additionally, the and spectral resolution. Concurrently crude oil hydrocarbons is monitored for Agency proposes to expand the 28 days. Product flasks at day 28 are requirement for efficacy testing to 56 Artificially distilled Alaska North Slope crude oil at 521 °F (272°C) to remove the low molecular compared to product flasks at day 0 to include freshwater, which allows for a weight hydrocarbons to approximate natural determine if a specified reduction both better evaluation of the use of these weathering processes that occur after a spill. in total resolved alkanes and total agents in this environment. Similarly to

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

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the Schedule, the Agency proposes the aliphatics (including all resolvable and an acute lethal concentration for 50% of percent reduction of the total alkane non-resolvable but GC-detectable the test species (LC50) at the lower 95% fraction (sum of all alkane aliphatics) is approximately equivalent confidence interval greater than 10 ppm concentrations determined by GC/MS) to an 80% reduction in total GC/MS- in either fresh or salt water, consistent to be greater than 95% at day 28, and resolvable target n-alkanes, based on with the acute toxicity thresholds that the percent reduction of the total Canadian data. The 10% reduction in proposed for dispersants. EPA’s toxicity 59 aromatic fraction (sum of all aromatic total aromatics is approximately classification scheme classifies LC50 concentrations determined by GC/MS) equivalent to a 50% reduction of the 5- values ranging from 10 ppm to 100 ppm must be greater than 70% at day 28, aromatic homologue group consisting of as slightly toxic, and values above 100 both based on the one-tailed Upper 95% naphthalene, fluorene, ppm substances are considered Confidence Limit (UCL95) for salt water. dibenzothiophene, phenanthrene, and practically nontoxic to aquatic For freshwater, the Agency proposes the chrysene and their alkylated homologs. organisms. By proposing this threshold percent reduction of the total alkane The U.S. aromatic series includes 2 level the Agency is establishing an fraction (sum of all alkane other 4-ring aromatics in addition to adequate safety margin without being concentrations determined by GC/MS) those 5 aromatic series considered by overly restrictive. The Agency requests to be greater than 95% at day 28, and Blenkinsopp et al.58 Thus, the U.S. and comments on the proposed acute that the percent reduction of the total Canadian protocols are similar in terms toxicity methods (or any others aromatic fraction (sum of all aromatic of decision criteria. The Agency available) and thresholds for concentrations determined by GC/MS) requests comments on all the proposed bioremediation agents. must be greater than 40% at day 28, changes and listing thresholds. Similarly to surface washing agents, both based on the one-tailed Upper 95% the Agency is not proposing provisions (2) Bioremediation Agent Toxicity Confidence Limit (UCL95). for conducting acute toxicity tests with Basis of Efficacy Thresholds. Current Requirements: The Agency bioremediation agent-oil mixtures. The According to Haines et al. (2005),57 the currently has no bioremediation agent Agency is requesting comment on the positive control culture was able to toxicity testing requirements for need for acute toxicity tests conducted biodegrade total alkanes in saltwater by purposes of listing these agents on the with bioremediation agents-reference oil 98.9% and total aromatics by 79.8% in Schedule. Section 5 of Appendix C is mixtures. A protocol for preparation of 28 days, based on the UCL90. In reserved for this purpose. The Agency product/oil mixtures for toxicity testing freshwater, the percent reduction values has, however, on a case-by-case basis, is available for review in the docket. were 97.9% and 37.8%, respectively, requested manufacturers to test (3) Listing of Non-Proprietary Nutrients again based on the UCL90. Thus, the bioremediation agents for toxicity if the proposed listing thresholds for the product contains surfactants or other The Agency recognizes there may be percent reduction of total alkanes and ingredients that may be harmful to the oil discharge situations where it is total aromatics from the GC/MS analysis environment. determined that the addition of are based on the findings of Haines et Proposed Revisions: The Agency is nutrients in the form of salts of nitrogen, al. (95% for alkanes vs. 98.9% in proposing an acute toxicity testing phosphorus and potassium (i.e., saltwater and 97.9% in freshwater, and protocol for bioremediation agents to fertilizers) to stimulate or enhance 70% for aromatics in saltwater and 40% include both fresh and saltwater. The bioremediation may be the most in freshwater vs. 79.8% in saltwater and Agency will use these testing results to effective and environmentally favorable 37.8% in freshwater). As for the positive determine listing eligibility on the mitigation method. However, non- control, the Agency believes a Schedule. The proposed testing proprietary commercially available reasonable target in saltwater would be protocols for bioremediation agents are formulations of nutrients are not 95% for total alkanes in both types of detailed in Appendix C. The proposed specifically listed on the Schedule, even exposure waters. For aromatics acute toxicity test protocol for though as nutrient additives they are reduction, 70% is considered reasonable bioremediation agents is based on EPA’s subject to Subpart J requirements. in saltwater and 40% in freshwater, protocol, Methods for Measuring the Currently, an OSC may only authorize based on Haines et al. EPA is using Acute Toxicity of Effluents and the use of an agent not listed on the UCL95 values rather than the UCL90 Receiving Waters for Freshwater and Schedule when its use is necessary to values from Haines because EPA’s latest Marine Organisms. The Agency prevent or substantially reduce a hazard research uses 6 replicates for the test proposes to require bioremediation to human life. Further, RRTs are not protocol which increases precision. The agents be tested for acute toxicity for the currently able to preauthorize the use of proposed criteria demonstrate that the product alone using fresh water species nutrients unless they are listed on the product can cause a substantial Ceriodaphnia dubia and Pimephales Schedule. To address these concerns, degradation of the alkane and aromatic promelas, and saltwater species the Agency proposes to include on the fractions of weathered crude oil Americamysis bahia and Menidia Schedule a specific list of the following compared to a control, as determined beryllina. The concentration of test generic non-proprietary nutrients: solely by GC/MS analysis. product causing 50% lethality to the test Ammonium nitrate, ammonium Of note, these proposed thresholds for organisms (LC50) lower and upper 95% phosphate, sodium nitrate, potassium listing bioremediation products on the confidence intervals (LCI95 and ULCI95) nitrate, urea, sodium triphosphate (or Schedule are similar to those are calculated at the end of the exposure tripolyphosphate), sodium phosphate, established for Canadian efficacy period. To be listed on the Schedule, potassium phosphate (mono- or testing, which are reductions of 30% for bioremediation agents must demonstrate dibasic), triple super phosphate, or any total aliphatics and 10% for total combination thereof. For these non- aromatics. The 30% reduction in total 58 Blenkinsopp, S, G Sergy, Z Wang, MF Fingas, proprietary commercial nutrients, the J Foght and DWS Westlake. 1995. Oil spill Agency believes there is no need for 57 Haines, J.R., E.J. Kleiner, K.A. McClellan, K.M. bioremediation agents-Canadian efficacy test submission of readily available Koran, E.L. Holder, D.W. King, and A.D. Venosa. protocols. Proceedings of the 1995 International Oil 2005. ‘‘Laboratory evaluation of oil spill Spill Conference, Feb 27–March 2, Long Beach, CA. bioremediation products in salt and freshwater American Petroleum Institute, Washington, DC. pp. 59 USEPA 2010. http://www.epa.gov/oppefed1/ systems.’’ J. Ind. Micorbiol. Biotechnol. 32:171–185. 91–96. ecorisk_ders/toera_analysiseco.htm#Ecotox.

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information. Thus, the proposal requires existing protocols to determine the establishing an adequate safety margin no technical product data or further effectiveness of solidifiers, its focus has without being overly restrictive. The action on the part of a manufacturer been on reviewing the protocols for Agency requests comments on the prior to authorizing their use in dispersants and bioremediation agents, proposed acute toxicity methods (or any response to a discharge event. However, given that their specific process for others available) and thresholds for this listing will be limited to products affecting the oil allows them to be left solidifiers. commonly formulated entirely of those in the environment, whereas solidifiers Similarly to surface washing agents, mineral nutrients and synthetically- are intended for removal from the the Agency is not proposing provisions derived urea listed. For products that environment. Therefore, the Agency is for conducting acute toxicity tests with may contain additional proprietary not proposing an efficacy testing solidifiers-oil mixtures. The Agency is components or have unique proprietary methodology for solidifiers, but is requesting comment on the need for formulations, the requirement for the requesting comment on available acute toxicity tests conducted with submitter to provide the toxicity and methodologies and/or performance solidifiers-reference oil mixtures. A efficacy data under the bioremediation criteria (e.g., buoyancy) it can consider. protocol for preparation of product/oil agent category will apply. mixtures for toxicity testing is available The Agency considered proposing a (2) Solidifier Toxicity for review in the docket. definition of ‘‘fertilizer’’ to specifically Current Requirements: The current (3) Limitations capture the listed bioremediation agents NCP Subpart J requires solidifiers to be proposed to be exempted. However, tested for saltwater species toxicity. The Agency is proposing a fertilizer is a term commonly used to Solidifier toxicity is tested following the conditional use listing for solidifiers. describe organic nutrients, which may dispersant toxicity testing protocols in The proposal specifies that the listing of contain substances that do not play a Appendix C to part 300 of the NCP. these products is limited to use only in role in mitigating oil discharges, and Proposed Revisions: The proposal those water environments for which the that may have deleterious effects on the revises the toxicity testing requirements product was tested and for which it met environment. Some non-proprietary for solidifiers, including the testing the listing threshold criteria. The fertilizers, for example, comprised of protocol. While the Agency currently Agency recognizes that products may activated sewage sludge or manure, provides the toxicity testing results to yield effective results in certain could contain unwanted pathogens and the OSC to assist in authorization of use environments and not in others. trace metals that could further stress the determinations, it is proposing to use Products that may be effective in environment if used in response to an these results to determine listing freshwater may not necessarily be so in oil discharge. Thus, instead of an eligibility on the Schedule. saltwater, and vice versa. The Agency is exemption based on a fertilizer The proposed revisions to the testing proposing this limitation to allow definition, EPA proposes to restrict the protocols for solidifiers are detailed in product manufacturers the flexibility to exemption under the bioremediation Appendix C to part 300. The proposed select which environment the product is category only to those nutrients listed acute toxicity test protocol for solidifiers to be tested and could be authorized for above in order to avoid any confusion. is based on EPA’s protocol, Methods for use, either saltwater, fresh water, or The Agency requests comments on this Measuring the Acute Toxicity of both. Therefore, the product would be approach. Effluents and Receiving Waters for listed and may only be authorized for Freshwater and Marine Organisms. The use in those water environments for (e) Solidifier Testing and Listing Agency proposes to require solidifiers which it was tested and for which it met Requirements be tested for acute toxicity for the the listing criteria. The proposal defines solidifiers as product alone using fresh water species (f) Herding Agent Testing and Listing substances that cause oil to become a Ceriodaphnia dubia and Pimephales Requirements coherent mass, preventing oil from promelas, or saltwater species dissolving or dispersing into the water Americamysis bahia and Menidia The proposal defines herding agents column, and which are collected and beryllina, or both, depending on the as substances that are used to control recovered from the environment. For intended product use. The the spreading of oil across the water this agent category, the Agency proposes concentration of test product causing surface. For this agent category, the to revise the toxicity testing protocol 50% lethality to the test organisms Agency proposes to revise the toxicity and to establish a listing threshold for (LC50) and lower and upper 95% testing protocol and to establish a listing toxicity in § 300.915(e). Although confidence intervals (LCI95 and ULCI95) threshold for toxicity in § 300.915(f). solidifiers are intended to be removed are calculated at the end of the exposure While these agents are intended to be from the environment, the proposed period. To be listed on the Schedule, removed from the environment, the revisions and new toxicity listing solidifiers must demonstrate an acute proposed revisions and new toxicity threshold respond to concerns regarding lethal concentration for 50% of the test listing threshold respond to concerns the general increase in the use of species (LC50) at the lower 95% regarding the general increase in the use chemical and biological agents as tools confidence interval greater than 10 ppm of chemical and biological agents as available for oil discharge responses. in either fresh or salt water, consistent tools available for oil discharge responses. (1) Solidifier Efficacy with the acute toxicity thresholds proposed for dispersants. EPA’s toxicity Currently, there is a test requirement 60 There are currently no efficacy testing classification scheme considers LC50 for distinguishing surface collecting requirements in the NCP Subpart J for values ranging from 10 ppm to 100 ppm agents from other chemical agents solidifiers to determine listing eligibility as slightly toxic and values above 100 (§ 300.915(c)(9), Test to Distinguish on the Schedule. These agents would ppm substances practically nontoxic to Between Surface Collecting Agents and have been captured by the current aquatic organisms. By proposing this Other Chemical Agents). Because the MOSCA agent category, which currently threshold level, the Agency is proposal eliminates surface collecting has no efficacy testing requirements, agents as a category and redefines and which the Agency is proposing to 60 USEPA 2010. http://www.epa.gov/oppefed1/ herding agents to better reflect its eliminate. While the Agency is aware of ecorisk_ders/toera_analysis_eco.htm#Ecotox. specific process for affecting the oil, and

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given that the agents will need to be dispersants. EPA’s toxicity classification to be tested and could be authorized for 61 identified in order for the required scheme considers LC50 values ranging use, either saltwater, fresh water, or testing to be submitted, the Agency is from 10 ppm to 100 ppm as slightly both. Therefore, the product would be eliminating this requirement. toxic and values above 100 ppm listed and may only be authorized for substances practically nontoxic to use in those water environments for (1) Herding Agent Efficacy aquatic organisms. By proposing this which it was tested and for which it met There are currently no efficacy testing threshold level, the Agency is the listing criteria. requirements in the NCP Subpart J for establishing an adequate safety margin (g) Sorbent Requirements herding agents to determine listing without being overly restrictive. The eligibility on the Schedule. These agents Agency requests comments on the The proposal defines sorbents as would have been captured by the proposed acute toxicity methods (or any inert, insoluble substances that readily current surface collecting agent others available) and thresholds for absorb and/or adsorb oil or hazardous category, which currently has no herding agents. substances. Sorbents would exclude efficacy testing requirements, and which Herding agents form a monolayer of those contaminated with substances that the proposal eliminates. The Agency is surfactants on the water surface that would interact with the environment not proposing an efficacy testing result in the contraction of the oil beyond their absorption/adsorption methodology for herding agents, but is slick.62 63 Herding agent composition capabilities (e.g., an invasive species). requesting comment on available may include hydrocarbons, The proposed definition states that methodologies and/or performance fluorosurfactants and/or silicone-based sorbents are generally collected and criteria it can consider. surfactants, which suggests that a stock removed from the environment and may be used in their natural bulk form, or as (2) Herding Agent Toxicity solution prepared using a WAF procedure similar to solidifiers may be manufactured products in particulate Current Requirements: The current appropriate. The Agency is requesting form, sheets, rolls, pillows, or booms. NCP Subpart J requires herding agents comment on the procedure for preparing The list of sorbent materials in the to be tested for saltwater species the stock solution for herding agents for proposed definition includes: Natural toxicity. Herding agent toxicity is tested the acute toxicity tests proposed in organic substances (e.g., feathers, cork, following the dispersant toxicity testing Appendix C. Any alternative procedure peat moss, and cellulose fibers such as protocols in Appendix C to part 300 of for preparing the stock solution must bagasse, corncobs, and straw); (2) the NCP. include an appropriate rationale in inorganic/mineral compounds (e.g., Proposed Revisions: The proposal order for the Agency to be able to volcanic ash, perlite, vermiculite, revises the toxicity testing requirements consider it for final action. zeolite, clay); and (3) synthetic for herding agents, including the testing Similarly to surface washing agents, compounds (e.g., polypropylene, protocol. While the Agency currently the Agency is not proposing provisions polyethylene, polyurethane, polyester). provides the toxicity testing results to for conducting acute toxicity tests with The Agency proposes to identify a list the OSC to assist in authorization of use herding agents-oil mixtures. The Agency of known sorbent materials, and make it determinations, we are proposing to use is requesting comment on the need for publicly available so that emergency these results to determine listing acute toxicity tests conducted with responders can be aware and make use eligibility on the Schedule. herding agents-reference oil mixtures. A of such sorbents on oil discharges. The The proposed revisions to the testing protocol for preparation of product/oil Agency is also proposing a process for protocols for herding agents follow the mixtures for toxicity testing is available submitters to request to include other same procedures as described for for review in the docket. products as sorbents if they can certify surface washing agents and are detailed they meet the inert, insoluble criteria. in Appendix C to part 300. The acute (3) Limitations Current Requirements: Sorbents are toxicity test protocol for herding agents The Agency is proposing a currently not listed on the Schedule, but is based on EPA’s protocol, Methods for conditional use listing for herding rather a list characterizing these Measuring the Acute Toxicity of agents. The proposal specifies that these materials is included in section Effluents and Receiving Waters for products may only be used in those 300.915(g). The current rule allows the Freshwater and Marine Organisms. The water environments for which the OSC to request written certification Agency proposes to require herding product was tested and for which it met from the manufacturers that their agents to be tested for acute toxicity for the listing threshold criteria. The particular sorbent product is comprised the product alone using fresh water Agency recognizes that products may solely of those materials identified in species Ceriodaphnia dubia and yield effective results in certain the rule. When a sorbent consists of Pimephales promelas, or saltwater environments and not in others. materials that are not specifically listed species Americamysis bahia and Products that may be effective in in the current rule, the Agency issues Menidia beryllina, or both, depending freshwater may not necessarily be so in written certifications, and sometimes on the intended product use. The saltwater, and vice versa. The Agency is requires testing and evaluation for concentration of test product causing proposing this limitation to allow possible listing on the Schedule. 50% lethality to the test organisms product manufacturers the flexibility to Proposed Revisions: The Agency (LC50) and lower and upper 95% select which environment the product is proposes to provide a Sorbent Product confidence intervals (LCI95 and List that includes certain publicly ULCI95) are calculated at the end of the 61 USEPA 2010. http://www.epa.gov/oppefed1/ available non-proprietary sorbent _ _ _ exposure period. To be listed on the ecorisk ders/toera analysis eco.htm#Ecotox. materials. The Agency also proposes to 62 Buist, I., Potter, S., Nedwed, T., (2011) Herding Schedule, herding agents must Agents to Thicken Oil Spills in Drift Ice for In Situ allow submitters to request that other demonstrate an acute lethal Burning: New Developments, IOSC, http:// products be included in this list as concentration for 50% of the test species ioscproceedings.org/doi/abs/10.7901/2169-3358- sorbents if they provide the technical 2011-1-230. (LC50) at the lower 95% confidence information required, including data to 63 Buist, I., Nedwed, T., (2011) Using Herders for interval greater than 10 ppm in either Rapid In Situ Burning Of Oil Spills on Open Water, support the claim that their product fresh or salt water, consistent with the IOSC, http://ioscproceedings.org/doi/abs/10.7901/ meets the sorbent definition. The acute toxicity thresholds proposed for 2169-3358-2011-1-231. Agency recognizes that a sorbent

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

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

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

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currently in § 300.920(a)(2) or (b)(2), or may result in their improper or incorrect Appendix C—Requirements for Product include the disclaimer currently set use. Falsification of federal documents, Testing Protocols and Summary Test forth in § 300.920(e). It remains the unsupported toxicity or efficacy claims, Data: Dispersant Baffled Flask Efficacy Agency’s position that listing a product submission of incorrect product and Toxicity Tests; Standard Acute on the Schedule does not constitute composition or use information, or Toxicity Test for Bioremediation Agents, approval or endorsement of that withholding technical product data are Surface Washing Agents, Herding product, nor a recommendation of its some examples of these acts. To Agents, and Solidifiers; and use. The Agency continues to believe minimize potential misuse of listed Bioremediation Agent Efficacy Test. The that it is important to avoid any possible products, the Agency believes it is proposed revisions reflect the proposed misinterpretation or misrepresentation appropriate to further clarify the criteria new and revised testing protocols for of this policy. Thus, the requirement for for the removal of a product from the listing agents on the Schedule. The a disclaimer to be included on any label, Schedule. In § 300.970 the proposal details of the technical changes and advertisement, or technical literature for specifically includes, but does not limit, rationale are discussed for each agent in the product is maintained. However, the as causes for removal from the section V.C.4 of this preamble—Data proposal removes the alternative to Schedule: Any misleading, inaccurate, and Information Requirements for reproduce in its entirety EPA’s written or incorrect statements within the Product Schedule Listing. The appendix notification that it will add the product product submission to EPA or to any reflects the proposed technical to the Schedule currently in person or private or public entity considerations and listing requirements. § 300.920(a)(2) or (b)(2). The Agency regarding the composition or use of the The Agency is requesting comment on believes it will be able to update the product to remove or control oil the protocols and their technical Schedule list within a reasonable discharges, including on labels, rationale. The Agency is also requesting timeframe given the advances in advertisements, or technical literature; comment on its organization and ease of information technology, and thus the any alterations to the chemical use. components, concentrations, or use option of producing the EPA letter of 10. Appendix E to Part 300 notification for a product listing should conditions of the product without no longer be necessary. The Agency is proper notification to EPA as required The 1994 revisions to the NCP proposing to modify the disclaimer by § 300.955(e); the failure to print the established Appendix E, Oil Spill language as follows: disclaimer provided in § 300.965 on all Response, which separates the oil spill labels, advertisements, or technical response requirements of the NCP from [PRODUCT NAME] is listed on the the hazardous substance release National Contingency Plan (NCP) Product literature; or any new or previously Schedule. This listing does NOT mean that unknown relevant information requirements (59 FR 47414). The EPA approves, recommends, licenses, or concerning the impacts or potential purpose of creating this appendix was to certifies the use of [PRODUCT NAME] on an impacts of the product to human health compile general oil discharge response oil discharge. This listing means only that or the environment. It also establishes a requirements into one document to aid data have been submitted to EPA as required process for removal if the Agency responsible parties and responders with by Subpart J of the NCP. Only a Federal On- obtains evidence of cause for removal. their duties under the national response Scene Coordinator (OSC) may authorize use EPA would notify the submitter in system. The Agency’s intent was to of this product according to the NCP. writing, at the address of record, of its provide guidance, and not to alter in The proposed revisions set forth in reasons for removal of the product from any way the meaning or policy stated in § 300.965 are intended to clarify that the the Schedule. The proposal would allow other sections or subparts of the NCP. use of these products is conditional to for an appeals process similar to the one However, some minor variations OSC authorization following the set forth for listing determinations. between the Appendix E provisions and requirements set forth under the NCP Appeals must be received within 30 the analogous provisions of the NCP regulations. The disclaimer language days of receipt of EPA’s removal rule language were necessary to ensure must continue to be conspicuously notification and must contain a clear that the appendix addressed only oil displayed in its entirety, and must be and concise statement with supporting discharges; hazardous substance fully reproduced on all product facts and technical analysis releases continue to be addressed in the literatures, labels, and electronic media, demonstrating why the submitter NCP rule but are not addressed in including Web site pages. As discussed believes EPA’s decision was incorrect. Appendix E. in the next section, a product can be Written notification from the The Agency proposes to remove removed from the Schedule if the Administrator will be sent to the Appendix E. While having all of the submitter does not comply with the submitter within 60 days of any appeal, information pertaining to oil discharges disclaimer requirements, or makes any or within 60 days of receipt of any compiled in one location may offer improper attempt to demonstrate the requested additional information. useful guidance, it is not necessary that approval or endorsement of a product. However, if no appeal is received within this guidance be codified as a regulatory The Agency requests comments on the the 30 days of receipt of EPA’s removal appendix to the NCP. The provisions in proposed revisions. notification, the product would be the appendix do not alter any NCP delisted without further notice. The requirement; however, they do contain 8. Removal of a Product From the Agency requests comments on the variations from the main NCP Schedule proposed clarification of criteria for requirements in order to have the Products that are not properly used in removal of products from the Schedule, appendix be relevant solely to oil the field may cause harm to human and on the associated appeals process. discharges. While EPA carefully health and the environment, and may reviewed the appendix and the relevant constitute violations of the CWA, and 9. Appendix C to Part 300 sections of the NCP at the time it was other federal, state, or local laws. The Agency is proposing to revise the established to ensure consistency in Misleading, inaccurate, or incorrect current Appendix C—Swirling Flask policy, instructions, guidance and statements within a product submittal Dispersant Efficacy Test, Revised requirements, there were intentional package or within language that refers to Standard Dispersant Toxicity Test, and minor variations. These may result in the listing of a product on the Schedule Bioremediation Agent Efficacy Test as having responses to oil discharges

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subject to two sets of what appear to be preauthorization plan and add new • Paragraph (b), Surface Washing potentially conflicting requirements, parameters for use considerations. Agents, would be moved to new causing unnecessary confusion. • Paragraph (c) would be revised to paragraph (c), Surface Washing Agent Because all requirements in Appendix clarify the requirements for authorizing Testing and Listing Requirements. The E are part of the NCP, any revisions to the use of burning agents by an OSC for paragraph would be revised to add new the NCP necessitate revisions to this authorized in-situ burns. toxicity and efficacy testing appendix. This adds burden not only for • Paragraph (d) would be revised to requirements, limitations for use, and the Agency in revising and ensuring clarify the exception requirements and new criteria for listing a surface washing consistency, but also for the regulated add specific time frames for notification agent to the Schedule. Existing community in reviewing redundant and of continued agent use. paragraph (c), Surface Collecting • duplicative requirements. While it may Paragraph (e) would be revised to Agents, would be deleted. be a useful tool to have all of the oil expand the prohibition to include • Paragraph (d), Bioremediation discharge specific requirements in one nonylphenol (NP) or nonylphenol Agents, would be revised to add new location, the Agency has reconsidered ethoxylates (NPEs) as components of toxicity and efficacy testing chemical or biological agents. requirements, limitations for use, and its position and believes that this is • more appropriately achieved through a Paragraph (f) would be revised to new criteria for listing a bioremediation separate guidance document, one that add new regulatory requirements for agent to the Schedule. Existing does not codify duplicative regulatory agent storage and use. Existing paragraphs (d)(9) and (10) were moved requirements. The Agency requests paragraph (f) requirements would be to new paragraph (a), General Product comments on the proposal to remove moved to new paragraph (g), Information. Appendix E from the NCP regulation, Supplemental Testing, Monitoring, and • Paragraph (e) would be revised to Information. add new regulatory requirements for and whether it should continue to offer • similar guidance through other formats. New paragraph (g), Supplemental submission and listing of a solidifier. Testing, Monitoring, and Information, Existing paragraph (e), Burning Agents, VI. Summary of Proposed Rule would revise the regulatory text to would be deleted. Provisions clarify the requirements for • Paragraph (f) would be revised to This section summarizes the proposed supplemental testing, monitoring and add new toxicity testing requirements, changes to 40 CFR parts 110 and 300. information. limitations of use, and criteria for listing • New paragraph (h), Recovery of Oil Subpart J has been renumbered to a herding agent on the Schedule. and Agents from the Environment, include new, consolidated, and revised Existing paragraph (f), Miscellaneous would add regulatory requirements for sections. Some of the rule sections have Oil Spill Control Agents, would be recovery of oil and agents from the been retained, removed, or moved in deleted. environment. • their entirety. The Table below provides Paragraph (g), Sorbents, would be • New paragraph (i), Reporting of an overview of the existing rule and revised to add new exceptions for listing Agent Use, would add regulatory proposed rule citations for a quick a sorbent to the Schedule. requirements for notification of agent reference of the proposed changes. Section 300.920, Addition of Products use on an oil discharge. Section 110.4, Dispersants, would be to Schedule, would be moved to new New section 300.913, Monitoring the section 300.955, Addition of a Product revised to link the rule with the new Use of Dispersants, would add and amended regulatory definitions for to the Schedule. regulatory requirements for monitoring • Paragraph (a) would be revised to Subpart J product categories. certain prolonged surface and include submission instructions for all Section 300.5, Definitions, would be subsurface use of dispersants. product categories. Existing paragraphs revised to include new, amended, and Section 300.915, Data Requirements, (a)(1) through (3) regulatory text specific deleted definitions. would be revised to consolidate general to dispersant applications would be Subpart J—Use of Dispersants, submission requirements applicable to moved to new §§ 300.915(b) and Chemicals, and Bioremediations Agents, all product categories. The section 300.955(c) and (d). heading would be revised to reflect new would be restructured to include new • Paragraph (b) would be revised to and amended regulatory definitions for testing and listing requirements for add new regulatory text for preparation product categories. specific product categories. of complete submission packages. • Section 300.900, General, paragraphs Paragraph (a), Dispersants, would Existing paragraph (b) regulatory text (a) and (c) would be revised to reflect be revised to consolidate general testing would be moved to new § 300.955(c) new and amended regulatory definitions and listing requirements from existing and (d). for product categories. paragraphs (a), (b), (d), and (f). The • Paragraph (c) would be revised to Section 300.905, NCP Product paragraph would include revisions and add regulatory text for EPA’s review of Schedule, would be removed. new requirements for the identification submission packages and decision Section 300.910, Authorization of of and testing for all product categories criteria for listing. Existing paragraph (c) Use, would be revised and new designated for listing. Existing would be moved to new § 300.950, paragraphs added to clarify planning paragraph (a) requirements specific to Submission of Confidential Business and preauthorization responsibilities. dispersants would be moved to new Information (CBI). • Paragraph (a) would be revised to section 300.915(b), Dispersant Testing • Paragraph (d) would be revised to clarify the requirements, including and Listing Requirements. The add regulatory text for requesting a process, responsibilities, and factors to paragraph would also be revised to add listing decision review. Existing consider for preauthorization; and add new toxicity and efficacy testing paragraph (d) would be moved to new new requirements for preauthorization requirements, limitations for use, and § 300.955(e), Changes to a Listed plan review, concurrence, and new criteria for listing a dispersant to Product. withdrawal procedures. the Schedule. Existing paragraph (b) • Paragraph (e) would be revised to • Paragraph (b) would be revised to would be moved to new paragraph (c), add new regulatory text for notification clarify the requirements for using a Surface Washing Agent Testing and of changes to a listed product. Existing listed product not addressed by a Listing Requirements. paragraph (e) would be moved to new

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

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

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

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40 CFR PART 300—NATIONAL OIL AND HAZARDOUS SUBSTANCES POLLUTION CONTINGENCY PLAN—DISTRIBUTION TABLE—Continued

Current citations Proposed rule citations

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

VII. Statutory and Executive Order (OMB) under the Paperwork Reduction numbers for EPA’s regulations in 40 Reviews Act, 44 U.S.C. 3501 et seq. The CFR are listed in 40 CFR part 9. Information Collection Request (ICR) Submit your comments on the A. Executive Order 12866: Regulatory document prepared by EPA has been Agency’s need for this information, the Planning and Review and Executive assigned EPA ICR number 1664.10. You accuracy of the provided burden Order 13563: Improving Regulation and can find a copy of the ICR in the docket estimates, and any suggested methods Regulatory Review for this rule, and it is briefly for minimizing respondent burden to Under Executive Order 12866 (58 FR summarized here. The ICR supporting the EPA using the docket identified at 51735, October 4, 1993), this action is a this proposed rule is largely self- the beginning of this rule. You may also ‘‘significant regulatory action.’’ This implementing. The information send your ICR-related comments to action raises novel legal or policy issues collection is to ensure that: (1) The OMB’s Office of Information and arising out of legal mandates, the Agency has the necessary information to Regulatory Affairs via email to oria_ President’s priorities, or the principles make Schedule listing determinations [email protected], Attention: set forth in the Executive Order. specific to the different product Desk Officer for EPA. Since OMB is Accordingly, EPA submitted this action categories; (2) product use by owners or required to make a decision concerning to the Office of Management and Budget operators of facilities or vessels, or the ICR between 30 and 60 days after (OMB) for review under Executive response personnel, in response to oil receipt, OMB must receive comments no Orders 12866 and 13563 (76 FR 3821, discharges is performed in accordance later than February 23, 2015. The EPA January 21, 2011) and any changes made with all applicable requirements; and will respond to any ICR-related in response to OMB recommendations (3) the Agency can verify compliance as comments in the final rule. have been documented in the docket for needed. Section 300.950 of the NCP C. Regulatory Flexibility Act (RFA) this action. contains provisions for confidentiality. In addition, EPA prepared an analysis EPA has carefully considered the The Regulatory Flexibility Act (RFA) of the potential costs and benefits burden imposed upon the regulated generally requires an agency to prepare associated with this action. This community by the proposed regulations. a regulatory flexibility analysis of any analysis is contained in the Regulatory EPA believes that the activities required rule subject to notice and comment Impact Analysis for Proposed Revisions are necessary and, to the extent rulemaking requirements under the to the National Oil and Hazardous possible, has attempted to minimize the Administrative Procedure Act or any Substances Pollution Contingency Plan burden imposed. The minimum other statute unless the agency certifies Regulations. A copy of the analysis is requirements specified in the proposed that the rule will not have a significant available in the docket for this action rule are intended to ensure that, when economic impact on a substantial and the analysis is briefly summarized needed, products are used properly in number of small entities. Small entities here. the field to respond to an oil discharge include small businesses, small The Agency expects the proposed rule in a manner protective of human health organizations, and small governmental would not cause a significant economic and the environment. jurisdictions. For purposes of assessing the impacts impact on a substantial number of small Respondents/affected entities: of the proposed rule on small entities, businesses. The total incremental costs Manufacturers of oil spill mitigating small entity is defined as: (1) As defined are estimated as $667,610 to $694,343 agents (products)/Oil spill responsible by the Small Business Administration’s annually at 3% and 7% ($2011) parties. annualization rates, respectively. The (SBA) regulations at 13 CFR 121.201; (2) Respondent’s obligation to respond: benefits of this action are assessed a small governmental jurisdiction that is Mandatory (40 CFR Part 300, Subpart J). qualitatively and include, for example, a government of a city, county, town, Estimated number of respondents: 65. greater clarity of regulatory school district or special district with a requirements, as well as less toxic Frequency of response: Initially. population of less than 50,000; or (3) a products. The resulting ratio of Total estimated burden: 721 hours small organization that is any not-for- compliance cost to annual sales revenue (per year). Burden is defined at 5 CFR profit enterprise that is independently for the proposed rule for existing and 1320.3(b). owned and operated and is not new product manufacturers would be Total estimated cost: $584,504 (per dominant in its field. less than one percent in most instances. year), includes $575,400 operation & After considering the economic maintenance costs. impacts of this proposed rule on small B. Paperwork Reduction Act An agency may not conduct or entities, I certify that this action will not The information collection sponsor, and a person is not required to have a significant economic impact on requirements in this proposed rule have respond to, a collection of information a substantial number of small entities. been submitted for approval to the unless it displays a currently valid OMB The small entities directly regulated by Office of Management and Budget control number. The OMB control this proposed rule are product

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manufacturers and laboratories and state because it contains no regulatory G. Executive Order 13045: Protection of and local governments that are involved requirements that might significantly or Children From Environmental Health in product development, testing and use uniquely affect small governments. Risks and Safety Risks for oil discharge response. EPA EPA interprets EO 13045 (62 FR conducted a small business analysis E. Executive Order 13132: Federalism 19885, April 23, 1997) as applying only consistent with the Agency’s 2006 small This action does not have federalism to those regulatory actions that concern business guidance. The Agency’s implications. It will not have substantial health or safety risks, such that the analysis indicates that about 95 percent direct effects on the States, on the analysis required under section 5–501 of of manufacturers are small businesses. the EO has the potential to influence the In conducting the small business relationship between the national regulation. This action is not subject to analysis, the agency compared the government and the States, or on the EO 13045 because it does not establish incremental annualized compliance distribution of power and environmental standards, such as limits costs to the annual sales revenue for the responsibilities among the various smallest entities. The results indicate levels of government, as specified in on levels of pollutants in the water, that that 90 percent of the smallest Executive Order 13132. This proposal are intended to directly mitigate health manufacturers have annualized does not alter the general procedures or safety risks. compliance costs that are less than 1 already defined in the NCP of how state, H. Executive Order 13211: Actions That percent of their annual sales revenue, local, and federal agencies cooperate in Significantly Affect Energy Supply, and that no manufacturers are expected responding to oil spills and how to Distribution or Use to have incremental costs that exceed 3 consult with the OSC and RRT when This proposed rule is not a percent of annual sales. The small considering the use of products on the ‘‘significant energy action’’ as defined in business analysis is available for review Schedule. Thus, Executive Order 13132 Executive Order 13211, ‘‘Actions in the Regulatory Impact Analysis (RIA). does not apply to this action. In the Therefore, we have determined that this Concerning Regulations that spirit of Executive Order 13132, and Significantly Affect Energy Supply, proposed rule does not have a consistent with EPA policy to promote significant impact on a substantial Distribution, or Use’’ (66 FR 28355, May communications between EPA and State 22, 2001) because it is not likely to have number of small entities. and local governments, EPA specifically Nonetheless, EPA has tried to reduce a significant adverse effect on the the impact of this rule on small entities solicits comment on this proposed supply, distribution, or use of energy. in developing the regulatory action from State and local officials. The proposal focuses on maintaining the availability of certain response tools requirements that balance the costs and F. Executive Order 13175: Consultation burden, while addressing the that can be considered when responding and Coordination With Indian Tribal to oil discharges, minimizing any environmental protection concerns. We Governments continue to be interested in the potential adverse impacts from their potential impacts of this proposed rule Subject to Executive Order 13175 (65 use, and resulting in greater overall on small business entities and welcome FR 67249, November 9, 2000), EPA may environmental protection. Thus, the comments on the issues related to such not issue a regulation that has tribal proposed rule would not cause reductions in the supply or production impacts. implications, that imposes substantial of oil, fuel, coal, or electricity; nor direct compliance costs, and that is not D. Unfunded Mandates Reform Act would it result in increased energy required by statute, unless the Federal This action contains no Federal prices, increased cost of energy government provides the funds mandates under the provisions of Title distribution, or an increased II of the Unfunded Mandates Reform necessary to pay the direct compliance dependence on foreign supplies of Act of 1995 (UMRA), 2 U.S.C. 1531– costs incurred by tribal governments, or energy. 1538 for State, local, or tribal EPA consults with tribal officials early I. National Technology Transfer and governments or the private sector. This in the process of developing the Advancement Act proposed rule imposes no new proposed regulation and develops a enforceable duty on any state, local or tribal summary impact statement. Section 12(d) of the National tribal governments or the private sector. EPA has concluded that this action Technology Transfer and Advancement UMRA excludes from the definition of may have tribal implications. However, Act of 1995 (‘‘NTTAA’’), Public Law ‘‘Federal intergovernmental mandate’’ it will neither impose substantial direct 104–113, 12(d) (15 U.S.C. 272 note) and ‘‘Federal private sector mandate’’ compliance costs on tribal governments, directs EPA to use voluntary consensus duties that arise from conditions of nor preempt Tribal law, similarly to the standards in its regulatory activities Federal assistance. UMRA generally effect on states. EPA will be consulting unless to do so would be inconsistent excludes from the definition of ‘‘Federal with applicable law or otherwise with tribal officials as it develops this intergovernmental mandate’’ duties that impractical. Voluntary consensus regulation to permit them to have arise from participation in a voluntary standards are technical standards (e.g., Federal program. UMRA also excludes meaningful and timely input into its materials specifications, test methods, from the definition of ‘‘Federal private development. Consultation will include sampling procedures, and business sector mandate’’ duties that arise from conference calls, webinars, and practices) that are developed or adopted participation in a voluntary Federal meetings with interested tribal by voluntary consensus standards program. Since the decision on whether representatives to ensure that their bodies. NTTAA directs EPA to provide to request that a product be included on concerns are addressed before the rule Congress, through OMB, explanations the Schedule is voluntary, the Agency is finalized. In the spirit of Executive when the Agency decides not to use has determined that this proposed rule Order 13175 and consistent with EPA available and applicable voluntary is not subject to the requirements of policy to promote communications consensus standards. sections 202 or 205 of UMRA. This between EPA and tribal governments, This rulemaking involves technical action is also not subject to the EPA specifically solicits comment on standards. The Agency conducted a requirements of section 203 of UMRA this proposed rule from tribal officials. search to identify potentially applicable

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voluntary consensus standards for planning activities, the desirability of devices, Regional response teams, efficacy testing. However, we identified using appropriate chemical or biological Sorbents, and Surface washing agents. no such standards. Therefore, EPA agents, or other spill mitigating devices. Dated: January 9, 2015. developed the Baffled Flask Efficacy In addition, the OSC, under authority Gina McCarthy, Test and the Bioremediation Efficacy granted by the NCP, must respond to an Administrator. Test required in Appendix C of this oil spill in a diligent and effective proposed rule. Voluntary consensus manner to protect human health and the For the reasons set out in the standards developed by ASTM are environment. If chemical or biological preamble, the Environmental Protection recommended for several product agents are needed, the OSC must Agency proposes to amend 40 CFR parts property data points, such as pH, flash coordinate with the RRT and ACs before 110 and 300 to read as follows: point and pour point. The product their use is authorized. In all cases, the PART 110—DISCHARGE OF OIL toxicity testing relies on existing RRT, ACs and OSC will address a broad protocols that are universally accepted. array of oil spill response and mitigation ■ 1. The authority citation for part 110 EPA welcomes comments on this aspect issues, including the potential for continues to read as follows: of the proposed rulemaking and, environmental justice concerns. specifically, invites the public to Historically, EPA has not found any Authority: 33 U.S.C. 1321(b)(3) and (b)(4) identify potentially-applicable and 1361(a); E.O. 11735, 38 FR 21243, 3 CFR evidence that the use of chemical or parts 1971–1975 Comp., p. 793. voluntary consensus standards for biological agents on the Schedule on oil ■ product efficacy and to explain why spills in the U.S. has had any 2. Revise § 110.4 and its section such standards should be used in this disproportionate effect on any heading to read as follows: regulation. environmental justice communities. § 110.4 Chemical or biological agents. J. Executive Order 12898: However, EPA will continue to monitor Addition of any chemical or Environmental Justice the implementation of the rule to ensure biological agent, as defined in § 300.5, to the planned or actual use of chemical or oil to be discharged that would Executive Order 12898, ‘‘Federal biological agents has no Actions to Address Environmental circumvent the provisions of this part is disproportionate effect on any EJ prohibited. Justice in Minority Populations and communities. Low-Income Populations’’ (59 FR 7629 EPA has determined that this PART 300—NATIONAL OIL AND (February 11, 1994)) establishes federal proposed rule will not have executive policy on environmental HAZARDOUS SUBSTANCES disproportionately high and adverse POLLUTION CONTINGENCY PLAN justice. Its main provision directs human health or environmental effects federal agencies, to the greatest extent on minority or low-income populations ■ 3. The authority citation for part 300 practicable and permitted by law, to because it increases the level of continues to read as follows: make environmental justice part of their environmental protection for all affected mission by identifying and addressing, Authority: 33 U.S.C. 1321(c)(2); 42 U.S.C. populations without having any 9601–9657; E.O. 13626, 77 FR 56749, 3 CFR, as appropriate, disproportionately high disproportionately high and adverse 2013 Comp., p. 306; E.O. 12777, 56 FR 54757, and adverse human health or human health or environmental effects 3 CFR, 1991 Comp., p. 351; E.O. 12580, 52 environmental effects of their programs, on any population, including any FR 2923, 3 CFR, 1987 Comp., p. 193. policies, and activities on minority minority or low-income population. populations and low-income Subpart A—Introduction Specifically, the proposed rule provides populations in the United States. EPA is committed to addressing additional safeguards before any ■ 4. Amend § 300.5 by: environmental justice concerns and has product can be listed on the Schedule, ■ a. Adding in alphabetical order the assumed a leadership role in as well as allows OSCs and RRTs to definitions of ‘‘Bioaccumulation’’, environmental justice initiatives to request additional information to ensure ‘‘Bioconcentration’’, ‘‘Biodegradation’’, enhance environmental quality for all that the use of any chemical or ‘‘Biological agents’’, and citizens of the United States. The biological agent, or any other spill ‘‘Bioremediation’’; Agency’s goals are to ensure that no mitigating substance, in responding to ■ b. Revising the definitions of segment of the population, regardless of oil discharges is protective of human ‘‘Bioremediation agents’’, ‘‘Burning race, color, national origin, income, or health and the environment. This agents’’, ‘‘Chemical agents’’, and net worth bears disproportionately high proposed rule is consistent with EPA’s ‘‘Dispersants’’; and adverse human health and Environmental Justice Strategy and the ■ c. Adding in alphabetical order the environmental impacts as a result of OSWER Environmental Justice Action definition of ‘‘Herding agents’’; EPA’s policies, programs, and activities. Agenda. ■ d. Removing the definitions for In response to Executive Order 12898, List of Subjects ‘‘Miscellaneous oil spill control agent’’; EPA’s Office of Solid Waste and ■ e. Adding in alphabetical order the Emergency Response (OSWER) formed 40 CFR Part 110 definition of ‘‘Products’’; an Environmental Justice Task Force to Environmental protection, Oil ■ f. Revising the definition of ‘‘Sinking analyze the array of environmental pollution, and Reporting and agents’’; justice issues specific to waste programs recordkeeping requirements. ■ g. Adding in alphabetical order the and to develop an overall strategy to definition of ‘‘Solidifiers’’; and 40 CFR Part 300 identify and address these issues ■ h. Revising the definition of (OSWER Directive No. 9200.3–17). To Air pollution control, Area ‘‘Sorbents’’ address this goal, EPA conducted a contingency planning, Bioremediation, ■ i. Removing the definition for qualitative analysis of the Chemicals, Dispersants, Environmental ‘‘Surface collecting agents’’. environmental justice issues under this protection, Hazardous materials, ■ j. Revising the definition title ‘‘Surface proposed rule. Hazardous substances, washing agent’’ and its definition; Under the NCP, RRTs and ACs are Intergovernmental relations, Natural The revisions and additions read as required to address, as part of their resources, Oil spills, Oil spill mitigating follows:

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§ 300.5 Definitions. Products are chemical or biological together, identify the waters and * * * * * agents manufactured using a unique quantities in which such dispersants, Bioaccumulation is the process of composition or formulation. other chemicals, or other spill accumulation of chemicals in the tissue * * * * * mitigating devices and substances may of organisms through any route, Sinking agents are substances be used. including respiration, ingestion, or deliberately introduced into an oil * * * * * direct contact with the ambient or discharge for the purpose of submerging (c) This subpart applies to the use of contaminated medium. the oil to the bottom of a water body. chemical and biological agents as Bioconcentration is the accumulation * * * * * defined in Subpart A of this part, or of chemicals in the tissues of organisms Solidifiers are substances that through other substances that may be used to from water alone. a chemical reaction cause oil to become remove, control, or otherwise mitigate Biodegradation is a process by which a cohesive mass, preventing oil from oil discharges. microorganisms metabolically dissolving or dispersing into the water (d) [Reserved] decompose contaminants into biomass column, and which are collected and § 300.905 [Removed] and simpler compounds such as carbon recovered from the environment. ■ 7. Remove § 300.905. dioxide, water, and innocuous end Sorbents are inert, insoluble ■ 8. Revise § 300.910 and the section products. substances that readily absorb and/or heading to read as follows: Biological agents are microorganisms adsorb oil or hazardous substances, and (typically bacteria, fungi, or algae) or that are not combined with or act as a § 300.910 Authorization for agent use. biological catalysts, such as enzymes, chemical or biological agent. Sorbents Use of chemical or biological agents able to enhance the biodegradation of a are generally collected and recovered in response to oil discharges to waters contaminated environment. from the environment. Sorbents may be of the U.S. or adjoining shorelines must Bioremediation is the process of used in their natural bulk form, or as be authorized by the OSC in accordance enhancing the ability of microorganisms manufactured products in particulate with the provisions of this section: to convert contaminants into biomass form, sheets, rolls, pillows, or booms. (a) Use of Agents Identified on the and innocuous end products by the Sorbents consist of: Schedule on Oil Discharges Addressed addition of materials into a (1) Natural organic substances (e.g., by a Preauthorization Plan. RRTs and contaminated environment to accelerate feathers, cork, peat moss, and cellulose Area Committees shall address in a the natural biodegradation process. fibers such as bagasse, corncobs, and preauthorization plan, as part of their Bioremediation agents are biological straw); planning activities, whether the use of agents and/or nutrient additives (2) Inorganic/mineral compounds chemical and biological agents listed on deliberately introduced into a (e.g., volcanic ash, perlite, vermiculite, the Schedule on certain oil discharges is contaminated environment to increase zeolite, clay); and appropriate. RRTs and Area Committees the rate of biodegradation and mitigate (3) Synthetic compounds (e.g., shall, as appropriate, include applicable any deleterious effects caused by the polypropylene, polyethylene, approved preauthorization plans in contaminant constituents. polyurethane, polyester). RCPs and ACPs. When a Bioremediation agents include * * * * * preauthorization plan is approved in microorganisms, enzymes, and nutrient Surface washing agents are substances advance for the use of certain agents additives such as fertilizers containing that separate oil from solid surfaces, under specified discharge situations, bioavailable forms of nitrogen, such as beaches, rocks, metals, or then the OSC may authorize the use of phosphorus and potassium. concrete, through a detergency agents on the Schedule for their Burning agents are additives that mechanism that lifts and floats oil for intended purpose without obtaining the improve the combustibility of the collection and recovery from the incident specific concurrences materials to which they are applied environment with minimal dissolution, described in paragraph (b) of this through physical or chemical means. dispersion, or transfer of oil into the section. water column. * * * * * (1) Preauthorization Plan Chemical agents are elements, * * * * * Development. For discharge situations compounds, or mixtures designed to identified where such agents may be Subpart J—Use of Dispersants, and used, the preauthorization plan must facilitate the removal of oil from a Other Chemical and Biological Agents contaminated environment and mitigate specify limits for the quantities and the any deleterious effects. Chemical agent ■ 5. Revise the heading of Subpart J as duration of use, and use parameters for categories include burning agents, set out above. water depth, distance to shoreline, and dispersants, herding agents, sinking ■ 6. Amend § 300.900 by revising proximity to populated areas. In agents, solidifiers, surface washing paragraphs (a) and (c), and by adding meeting the provisions of this agents, and bioremediation agents that paragraph (d) to read as follows: paragraph, preauthorization plans consist of nutrient additives. should document how regional factors § 300.900 General. are addressed including likely sources * * * * * (a) Section 311(d)(2)(G) of the Clean and types of oil that might be Dispersants are typically mixtures of Water Act (CWA) requires EPA to discharged, various discharge scenarios, solvents, surfactants, and additives that prepare a schedule identifying the existence and location of promote the formation of small droplets dispersants, other chemicals, other spill environmentally sensitive resources or of oil in the water column by reducing mitigating devices and substances if restricted areas that might be impacted the oil-water interfacial tension. any, that may be used in carrying out by discharged oil, and logistical factors * * * * * the NCP; and the waters and quantities including inventory, storage locations Herding agents are substances that are in which they may be used. This and manufacturing capability of used to control the spreading of the oil subpart establishes a schedule available agents, availability of across the water surface. identifying chemical and biological equipment needed for agent use, * * * * * agents, and procedures that, when taken availability of adequately trained

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

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§ 300.913 Monitoring the use of (4) Total petroleum hydrocarbons, within 24 hours of collection), including dispersants. individual resolvable constituents documented observations, photographs, As directed by the OSC, the including volatile organic compounds, video, and any other information related responsible party must monitor any aliphatic hydrocarbons, monocyclic, to dispersant use, unless an alternate subsurface use of dispersant in response polycyclic, and other aromatic timeframe is authorized by the OSC; to an oil discharge, surface use of hydrocarbons including alkylated (3) For analyses that take more than dispersant in response to oil discharges homologs, and hopane and sterane 24 hours due to analytical methods, of more than 100,000 U.S. gallons biomarker compounds; provide such data and results within 5 occurring within 24 hours, and surface (5) Carbon dioxide (CO2) (subsurface days, unless an alternate timeframe is use of dispersant for more than 96 hours only); authorized by the OSC; and in response to an oil discharge, and (6) Methane, if present (subsurface (4) Estimates of the daily transport of submit a Quality Assurance Project Plan only); dispersed and non-dispersed oil and for approval to the OSC covering the (7) Heavy metals, including nickel associated volatile petroleum collection of all environmental data. and vanadium; hydrocarbons, and dispersants, using When these dispersant use conditions (8) Turbidity; the best available trajectory modeling. are met, and for the duration of (9) Water temperature; ■ 10. Revise § 300.915 and the section dispersant operations, the responsible (10) pH; and heading to read as follows: party shall: (11) Conductivity. (c) In consultation with the OSC, and § 300.915 Data and information (a) Document the characteristics of the using best available technologies, requirements for Product Schedule listing. source oil; best estimate of the oil characterize the dispersant effectiveness If you are submitting an application discharge flow rate, periodically and oil distribution, considering the for listing a product to the Schedule, reevaluated as conditions dictate, condition of oil, dispersant, and you must provide EPA the information including a description of the method, dispersed oil components from the required under § 300.955. Your associated uncertainties, and materials; discharge location; submission must contain: dispersant(s) product used, rationale for (d) In consultation with the OSC, (a) General Information for any dispersant product choice(s) including characterize the ecological receptors Product Category. (1) Your name, the results of any efficacy and toxicity (e.g. aquatic species, wildlife, and/or physical address, email, and telephone tests specific to area or site conditions, other biological resources) and their number; recommended dispersant-to-oil ratio habitats that may be present in the (2) Your identity as the manufacturer (DOR); and the application method and discharge area and their exposure of the product, a vendor, importer, or procedures, including a description of pathways. Include those species that distributor of the product, and/or a the equipment to be used, hourly may be in sensitive life stages, transient designated agent acting on behalf of the application rates, capacities, and total or migratory species, breeding or manufacturer. Provide documentation of amount of dispersant needed. For breeding-related activities (e.g., embryo such identity; subsurface discharges also document and larvae development), and (3) All name(s), brand(s), and/or the best estimate of the discharge flow threatened and/or endangered species trademark(s) under which the product is rate of any associated volatile petroleum that may be exposed to the oil that is not to be sold; hydrocarbons, periodically reevaluated dispersed, the dispersed oil, and the (4) Names, physical addresses, emails as conditions dictate, including a dispersant alone. Estimate an acute and telephone numbers of the primary description of the method, associated toxicity level of concern for the distributors, vendors, importers, and/or uncertainties, and materials. dispersed oil using available dose/ designated agent acting on behalf of the (b) In areas not affected by the response information relevant to manufacturer; discharge of oil, collect a representative potentially exposed species. (5) A Safety Data Sheet (SDS) for the set of background water column (e) Immediately report to the OSC product; samples following standard operating any: (6) The maximum, minimum and and quality assurance procedures, at the (1) Deviation of more than 10 percent optimum temperature, humidity and closest safe distance from the discharge from the mean hourly dispersant use other relevant conditions for product as determined by the OSC and in any rate for subsurface application, based on storage and a brief description of the direction of likely transport considering the dispersant volume authorized for 24 consequences to performance if the surface and subsurface currents and oil hours use, and the reason for the product is not stored within these properties for the variables listed below. deviation; and limits; In the dispersed oil plume, collect daily (2) Ecological receptors, including any (7) The anticipated shelf life of the water column samples following threatened or endangered species that product at the storage conditions noted standard operating and quality may be exposed based on dispersed in paragraph (a)(6) of this section and assurance procedures, at such depths plume trajectory modeling and level of documentation for this determination; and locations where dispersed oil is concern information. (8) A sample product label for all likely to be present and analyze for: (f) Report daily to the OSC water name(s), brand(s), and/or trademark(s) (1) In-situ oil droplet size distribution, sampling and data analyses collected in under which the product is to be sold including mass or volume mean § 300.913(b) and include: that includes manufacture and diameter for droplet sizes ranging from (1) Specific hourly dispersant expiration dates, and conditions for 2.5 to 2,000 mm, with the majority of application rate and the total amount of storage. You may use an existing label data collected between the 2.5 and 100 dispersant used for the previous provided it already contains the mm size; reporting period established by the OSC required dates and storage information; (2) In-situ fluorometry and with concurrence from the EPA (9) The chemical or biological agent fluorescence signatures targeted to the representative to the RRT; category under which you want the type of oil discharged and referenced (2) All collected data and analyses of product to be considered for listing on against the source oil; those data within a timeframe necessary the Schedule, including detailed (3) Dissolved oxygen (DO); to make operational decisions (e.g., information on the specific process(es)

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

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(2) Surface Washing Agent Toxicity sodium phosphate, potassium it as a sorbent on the Sorbent Product test and listing criteria. Using the phosphate (mono- or dibasic), triple List: toxicity test methodology in Appendix super phosphate, potassium sulphate, or (i) The information required under C to part 300, test the surface washing any combination thereof, no technical paragraphs (a)(1) through (8), and agent for acute toxicity against fresh product data are required, are paragraph (a)(13) of this section; water species Ceriodaphnia dubia and generically listed as non-proprietary (ii) The certifications required under Pimephales promelas, or saltwater nutrients on the Schedule, and no paragraphs (a)(14)(iv), (a)(15), and species Americamysis bahia and further action is necessary. (a)(16) of this section; and Menidia beryllina, or both, depending (e) Solidifier Testing and Listing (iii) Information, including data, to on the intended product use. To be Requirements. (1) Solidifiers must be support the claim your product meets listed on the Schedule, the surface tested for acute toxicity in saltwater, the sorbent definition under § 300.5. washing agent must demonstrate an freshwater or both, depending on the § 300.920 [Removed] LC50 at the lower 95% confidence intended product use, following the interval of greater than 10 ppm in either method specified in Appendix C to part ■ 11. Remove § 300.920. fresh or saltwater for all tested species. 300. To be listed on the Schedule, the ■ 12. Add § 300.950 to subpart J to read (3) Limitations. Based on testing, solidifier must demonstrate an LC50 at as follows: product listing would be for use only in the lower 95% confidence interval of the fresh and/or saltwater environments § 300.950 Submission of Confidential greater than 10 ppm in either fresh or Business Information (CBI). for which it was tested and for which it saltwater for all tested species. (a) Except as provided in paragraph met the efficacy and toxicity listing (2) Limitations. Based on testing, (b) of this section, all product criteria. product listing would be for use only in information submitted to EPA as (d) Bioremediation Agent Testing and the fresh and/or saltwater environments required under § 300.915 will be Listing Requirements—(1) for which it was tested and for which it disclosed to the public. Bioremediation Agent Efficacy test and met the toxicity listing criteria. listing criteria. To be listed on the (b) You may only claim the (f) Herding Agent Testing and Listing concentration and the maximum, Schedule, a bioremediation agent must Requirements. (1) Herding agents must successfully degrade both alkanes and minimum, and average weight percent be tested for acute toxicity in saltwater, aromatics as determined by gas of each chemical component or freshwater, or both, depending on the chromatography/mass spectrometry microorganism in your product, as intended product use, following the (GC/MS) in salt or fresh water or both, identified in § 300.915(a)(13) or (14), to method specified in Appendix C to part depending on the intended product use, be CBI. EPA will handle such claims in 300. The herding agent must following the test method specified in accordance with 40 CFR part 2, subpart demonstrate an LC at the lower 95% Appendix C to part 300. The percentage 50 B. confidence interval of greater than 10 reduction of total alkanes (aliphatic (1) You must make your CBI claim at ppm in either fresh or saltwater for all fraction) from the GC/MS analysis must the time you submit your information to be greater than or equal to 95% at day tested species. EPA to be listed on the Schedule. 28, based on the ninety-fifth percentile (2) Limitations. Based on testing, (2) You must redact the CBI from all product listing would be for use only in Upper Confidence Limit (UCL95) for submitted information but include the both salt and freshwater. The percentage fresh and/or saltwater environments for CBI separately with your submission reduction of total aromatics (aromatic which it was tested and for which it met package. Clearly identify and mark the fraction) must be greater than or equal the toxicity listing criteria. information as ‘‘Confidential Business to 70% at day 28 for saltwater and (g) Sorbent Requirements. Known Information’’ and place it in a separate greater than or equal to 40% for sorbent materials and products will be inner envelope in your submission identified on a publicly available freshwater based on the UCL95. package labeled with ‘‘CONFIDENTIAL (2) Bioremediation Agent Toxicity test Sorbent Product List for the use of such BUSINESS INFORMATION—TO BE and listing criteria. The bioremediation products when responding to an oil OPENED BY THE PRODUCT agent must be tested for acute toxicity discharge as follows: SCHEDULE MANAGER ONLY.’’ in saltwater, freshwater or both, (1) For sorbent products that consist ■ 13. Add § 300.955 to subpart J to read depending on the intended product use, solely of the following materials, or any as follows: following the method specified in combination thereof, no technical data Appendix C to part 300. To be listed on are required and no further action is § 300.955 Addition of a product to the the Schedule, the bioremediation agent necessary for use as a sorbent: Schedule. must demonstrate an LC50 at the lower (i) Feathers, cork, peat moss, and (a) Submission. Submit your complete 95% confidence interval of greater than cellulose fibers such as bagasse, package to: U.S. Environmental 10 ppm in either fresh or saltwater for corncobs, and straw; Protection Agency, 1200 Pennsylvania all tested species. (ii) Volcanic ash, perlite, vermiculite, Ave. NW., Mail Code: 5104A, Room (3) Limitations. Based on testing, zeolite, and clay; and 1448, William J. Clinton North, product listing would be for use only in (iii) Polypropylene, polyethylene, Washington, DC 20460, Attention: the fresh and/or saltwater environments polyurethane, and polyester. Product Schedule Manager. for which it was tested and for which it (2) If the product consists of one or (b) Package contents. Your package met the efficacy and toxicity listing more natural organic substances, shall include, in this order: criteria. inorganic/mineral compounds, and/or (1) A cover letter on company (4) Exceptions. If the product consists synthetic compounds not specifically letterhead signed and dated by you solely of: ammonium nitrate, identified in paragraph (g)(1) of this certifying that: ammonium phosphate, ammonium section but you believe the product (i) All testing was conducted on sulfate, calcium ammonium nitrate, meets the definition of a sorbent then, representative product samples; sodium nitrate, potassium nitrate, as applicable under § 300.955(a) and (b), (ii) Testing was conducted at a synthetically-derived urea, sodium you must submit the following nationally or internationally accredited triphosphate (or tripolyphosphate), information for consideration for listing laboratory in accordance with the

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methods specified in Appendix C to the decision within 60 days of receipt of a Federal On-Scene Coordinator (OSC) part 300, and other applicable methods your request, or within 60 days of may authorize use of this product as appropriate; and receipt of requested additional according to the NCP. (iii) All test results and product information. ■ 15. Add § 300.970 to subpart J to read technical data and information are true (e) Changes to a product listing. You as follows: and accurate. must notify EPA in writing within 30 (2) A numbered Table of Contents days of any changes to information § 300.970 Removal of a product from the showing the information and data submitted under § 300.915(a)(1) through Schedule. submitted under § 300.915(a) through (8) and § 300.915(a)(19) through (21) for (a) The EPA Administrator may (g); a product on the Schedule. In the remove your product from the Schedule (3) All required data and information notification, you must detail the specific for reasons including, but not limited to: arranged in the same order as specified changes, the reasons for such changes (1) Misleading, inaccurate, or in § 300.915(a) through (g); and and supporting data and information. incorrect statements within the product (4) A separate envelope containing EPA may request additional information submission to EPA or to any person or Confidential Business Information as and clarification regarding these private or public entity regarding the specified in § 300.950(b), if applicable. changes. If you change the chemical composition or use of the product to (c) EPA Review. EPA shall, within 90 components and/or concentrations, you remove or control oil discharges, days of receiving a submission package: must retest the reformulated product including on labels, advertisements, or (1) Review the package for according to the requirements for the technical literature; or completeness and compliance with all product category and submit a complete (2) Alterations to the chemical data and information requirements in new package for a review and components, concentrations, or use §§ 300.915, 300.950, and this section, consideration for listing on the conditions of the product without verify information, and request Schedule by EPA. proper notification to EPA as required clarification or additional information (f) Transitioning Listed Products from by § 300.955(e); or as necessary; the Current Schedule to the New (3) Failure to print the disclaimer (2) Make a product listing Schedule. All products on the current provided in § 300.965 on all labels, determination based on a technical Schedule as of [EFFECTIVE DATE OF advertisements, or technical literature, evaluation of all data and information FINAL RULE] will remain conditionally or submitted, relevant information on listed until [DATE 24 MONTHS FROM (4) New or previously unknown impacts or potential impacts of the THE EFFECTIVE DATE OF FINAL relevant information concerning the product or any of its components on RULE] at which time all products that impacts or potential impacts of the human health or the environment, and have not submitted and been listed in product to human health or the the intended use of the product. EPA the new Schedule based on the environment. reserves the right to make a amended test and listing criteria will be (b) EPA will notify you in writing, at determination on whether the product removed. Your product will be your address of record, of its reasons for will be listed, and under which transitioned from the current Schedule deciding to remove the product from the category; and to the new Schedule prior to [DATE 24 Schedule. If EPA receives no appeal (3) Notify you, in writing, of its MONTHS FROM THE EFFECTIVE from you in 30 days, the product will decision to list the product on the DATE OF FINAL RULE] after you be removed from the Schedule without Schedule and in which category or submit a new, complete package further notice to you. categories, or of its decision and according to the amended test and (c) You may appeal the decision to supporting rationale to reject the listing criteria and EPA makes a remove your product from the Schedule submission. If your submission is favorable finding to list the product on within 30 days of receipt of EPA’s rejected: the new Schedule. notification. Your appeal must contain a (i) You may revise the submission ■ 14. Add § 300.965 to subpart J to read clear and concise statement with package to address test results, data, or as follows: supporting facts and technical analysis information deficiencies and resubmit demonstrating why you believe EPA’s it. § 300.965 Mandatory product disclaimer. decision was incorrect. The EPA (ii) EPA’s 90-day review will not start The listing of a product on the Administrator will notify you in writing until a complete package is resubmitted. Schedule does not constitute approval of his decision within 60 days of your (d) Request for review of decision. If or recommendation of the product. To appeal, or within 60 days of receipt of your product is rejected for listing on avoid possible misinterpretation or any requested additional information. the Schedule, you may request that the misrepresentation, any label, ■ 16. Revise Appendix C to Part 300 and EPA Administrator review the advertisement, or technical literature for appendix heading to read as follows: determination. Your request must be in the product must display in its entirety writing within 30 days of receipt of the disclaimer shown below. The Appendix C to Part 300—Requirements notification of EPA’s decision not to list disclaimer must be conspicuous and for Product Testing Protocols and the product on the Schedule. Your must be fully reproduced on all product Summary Test Data: Dispersant Baffled request must contain a clear and concise literatures, labels, and electronic media Flask Efficacy and Toxicity Tests; statement with supporting facts and including Web site pages. Standard Acute Toxicity Test for technical analysis demonstrating why DISCLAIMER [PRODUCT NAME] is Bioremediation Agents, Surface you believe EPA’s decision was listed on the National Contingency Plan Washing Agents, Herding Agents, and incorrect. (NCP) Product Schedule. This listing Solidifiers; and Bioremediation Agent (1) The EPA Administrator or does NOT mean that EPA approves, Efficacy Test. designee may request additional recommends, licenses, or certifies the Table of Contents information from you and may offer an use of [PRODUCT NAME] on an oil 1.0 Applicability and Scope opportunity for you to meet with EPA. discharge. This listing means only that 2.0 Baffled Flask Dispersant Efficacy Test (2) The EPA Administrator or his data have been submitted to EPA as (BFT) designee will notify you in writing of required by Subpart J of the NCP. Only 3.0 Dispersant Toxicity Testing

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4.0 Standard Acute Toxicity Testing for 13. Freshwater Nutrient Concentrations spilled on the surface of seawater, using a Surface Washing Agents, Bioremediation 14. Artificial Freshwater Nutrient modified 150-mL screw-cap trypsinizing Agents, Herding Agents, and Solidifiers. Concentration for Bioremediation Agents flask (an Erlenmeyer flask with baffles) with 5.0 Bioremediation Agent Efficacy Test Having No Nutrients Included a glass and Teflon® stopcock near the bottom Protocol 15. Bioremediation Efficacy Test—Summary to allow removal of subsurface water samples of Experimental Setup Illustrations without disturbing the surface oil layer. The 16. Bioremediation Efficacy—Summary of efficacy of a dispersant is measured using Figure Number Analytical Procedures two types of oils (Intermediate Fuel Oil 120 1. A Baffled Trypsinizing Flask 17. QA/QC Checks and Alaska North Slope) at two temperatures ° ° Standard Operating Procedures Tables (5 C and 25 C). Six replicates are required Tables at each condition with two method blank Table Number SOP 3–1 Amount of Stock Solutions replicates at each temperature. A layer of oil Required to Make the Working Standards 1. Constituent Concentrations for GP2 is placed on the surface of artificial seawater, SOP 4–1 Ions Associated With Retention and the dispersant is added to the slick at a Artificial Seawater Time Groups 2. Test Oil Characteristics dispersant:oil ratio (DOR) of 1:25 (4%) by SOP 4–2 Instrumental Conditions for Crude volume. A standard orbital shaker table 3. Stock Solution Preparation Oil Analysis provides turbulent mixing at a speed of 250 4. Dispersant Calibration Example for Both SOP 4–3 Ion Abundance Criteria for DFTPP revolutions per minute (rpm) for 10 minutes, Oils SOP 4–4 Target Compound List immediately after which it is maintained 5. Sample Calculation with ANS 1.0 Applicability and Scope. This stationary for 10 minutes to allow non- 6. Toxicity Testing Requirements for Appendix establishes laboratory protocols dispersed oil to rise to the water’s surface. An Dispersants required under Subpart J (Use of Dispersants undisturbed water sample is removed from 7. Summary of Test Conditions—Dispersant and Other Chemical and Biological Agents) the bottom of the flask through the stopcock, Toxicity of 40 CFR part 300 (National Oil and 8. Toxicity Testing Requirements for Surface Hazardous Substances Pollution Contingency extracted with dichloromethane (DCM), and Washing Agents, Herding Agents, Plan) to make listing determinations for the analyzed for oil content by UV-visible Bioremediation Agents and Solidifiers Product Schedule. The protocols apply, absorption spectrophotometry at wavelengths 9. Summary of Test Conditions—Surface based on product type, to dispersants, ranging between 340 and 400 nm. Washing Agents, Herding Agents, bioremediation agents, surface washing 2.2 Apparatus. All equipment must be Bioremediation Agents and Solidifiers agents, herding agents, and solidifiers as maintained and calibrated per standard Toxicity defined in Subpart A (Introduction) of 40 laboratory procedures. 10. Artificial Seawater Nutrient CFR part 300. 2.2.1 Modified Trypsinizing Flask. A Concentrations modified 150 mL glass screw-capped 11. Artificial Seawater Nutrient 2.0 Baffled Flask Dispersant Efficacy Test Erlenmeyer flask with baffles (e.g., Wheaton Concentrations for Bioremediation Agents (BFT) No. 355394 or equivalent) fitted with a 2 mm Having No Nutrients Included 2.1 Summary. This laboratory protocol bore Teflon® stopcock and glass tubing, the 12. Constituent Concentrations for Artificial establishes procedures to evaluate the degree center of which is no more than 1.3 cm from Freshwater (Bushnell-Haas) to which a product effectively disperses oil the bottom, as shown in Figure 1.

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2.2.2 Orbital Shaker Table. An orbital 2.2.7 Constant temperature rooms or 2.4 Container Handling and Storage ° shaker table with a variable speed control incubators to hold the shaker at 5 C and 25 2.4.1 Glassware. If the glassware has been unit capable of maintaining 250 rpm. The ° C. used with oil before, rinse with DCM to orbital diameter must be approximately 1.0 2.2.8 Analytical Balance. ¥ remove as much of the oil adhering to the inch (2.5 cm) +/ 0.1 inch (0.25 cm). 2.2.9 Chemical fume hood. 2.2.3 Spectrophotometer. A UV-visible sides of the flask as possible; waste DCM may spectrophotometer capable of measuring 2.3 Reagents be used. Soak in warm water with detergent absorbance between 340 and 400 nm (e.g., 2.3.1 Artificial seawater. Use the artificial and individually wash with bristled brushes. Shimadzu UV–1800, Agilent 8453, or seawater GP2 formulation shown in Table 1 First rinse with tap water, then follow with equivalent). Use standard transmission- of this Appendix. two de-ionized water rinses. Dry either on a matched quartz 10-mm path length 2.3.2 Test oils. Use the two EPA standard rack or in a 110 °C drying oven). After drying, rectangular cells with PTFE cover for reference oils, Alaska North Slope oil (ANS) rinse with fresh DCM (use sparingly). absorbance measurements. and Intermediate Fuel Oil 120 (IFO 120). To 2.4.2 Serum bottles and other non- 2.2.4 Glassware. Including: 25-ml obtain these oils at no charge (except for a volumetric glassware. Bake for at least 4 graduated mixing cylinders (a graduated minimal shipping fee), see the instructions at hours in a muffle furnace at 450 °C. cylinder with a ground glass stopper); 50- http://www.epa.gov/emergencies/content/ and 100-ml graduated cylinders; 125-mL 2.5 Calibration Curve for the UV-visible ncp/index.htm. Selected properties are separatory funnels with Teflon stopcocks; 10 spectrophotometer summarized in Table 2 of this Appendix. ml volumetric flasks; 30 ml crimp style glass 2.5.1 Stock Standard Solution serum bottles; 1-, 2-, 5-mL pipettes; other 2.3.3 Dichloromethane (DCM) (also Preparation. Stock standard solution miscellaneous laboratory items. known as methylene chloride), pesticide 2.2.5 Micropipettor. Use a micropipettor quality. concentrations are based on the mass capable of dispensing 4 mL of dispersant and 2.3.4 Positive Control Dispersant. measurements after each addition and 100 mL of oil (e.g., Brinkmann Eppendorf Dispersant sample with a known, density determinations of the oil/dispersant/ repeater pipettor with 100 mL and 5 mL reproducible efficacy. To obtain this control DCM solution using a density bottle or a 1- syringe tip attachments or equivalent). sample at no cost (except for shipping), see mL gas tight syringe. An example calculation 2.2.6 Syringes. 25-, 100-, 250-, 1000-, the instructions at http://www.epa.gov/ is given in Table 3 of this Appendix 2500-, 5000- ml gas-tight syringes. emergencies/content/ncp/index.htm. according to the following equation:

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

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

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

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

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

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

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

where: Vtw = total seawater in Baffled Flask (120 mL)

VDCM = final volume of the DCM extract (mL) Vew = volume seawater extracted (30 mL)

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

where %OD = mean percentage oil dispersed 2.10.2 Method blanks. Analytical method Temp DELCL95 for the n = 6 replicates, S = standard Oil (°C) (%) blanks involve an analysis of artificial th deviation, and t (n-1,1-α) = 100 * (1-a) seawater blanks (artificial seawater without percentile from the t-distribution with ANS ...... 5 ≥ 70 oil or dispersant in a baffled flask) through ≥ n-1 degrees of freedom. For 6 replicates, ANS ...... 25 75 testing and analytical procedures. Analyze IFO120 ...... 5 ≥ 55 t α = 2.015, where a = 0.05. An method blanks with a frequency of at least n-1,1- IFO120 ...... 25 ≥ 65 example of the calculations is given in two per completed test. Oil concentrations in Table 5 of this Appendix. method blanks must be less than detectable 2.10 Quality Control (QC) Procedures for limits. 2.9 Performance Criterion Oil Concentration Measurements The dispersant product tested will remain 2.10.1 Absorbance readings. Perform at 2.10.3 Accuracy. Determine accuracy by in consideration for listing on the NCP least 5% of all UV-visible spectrophotometric using a mid-point standard calibration check Product Schedule if the dispersant efficacy measurements in duplicate as a QC check on after each set of replicate samples analyzed. (DELCL95), as calculated in section 2.8.6 of the analytical measurement method. The The acceptance criterion is based on a this Appendix, is: absorbance values for the duplicates must percent recovery of 90–110% using the agree within ± 5% of their mean value. following equation:

2.10.4 Calibration QC checks. Before TABLE 1—CONSTITUENT CONCENTRA- TABLE 1—CONSTITUENT CONCENTRA- analyzing samples, the spectrophotometer TIONS FOR GP2 ARTIFICIAL SEA- TIONS FOR GP2 ARTIFICIAL SEA- must meet an instrument stability calibration WATER WATER—Continued criterion using the oil standards. The instrument stability for initial calibration is [Based on Spotte et al., 1984] [Based on Spotte et al., 1984] acceptable when the RFs (Equation 5 of this Concentration Appendix) for each of the six standard Concentration Constituent Constituent (g/L) (g/L) concentration levels are less than 10%

different from the overall mean value. NaCl ...... 21.03 SrCl2 ·6H2O * ...... 0.02 Na2SO4 ...... 3.52 NaHCO2 * ...... 0.17 KCl ...... 0.61 * Use Stock Solution, 1 mL/L GP2 for 100X KBr * ...... 0.088 stock solution for Bromide, Borate, and Stron- Na2B4O7 ·10H2O * ...... 0.034 tium. MgCl2 ·6H20 ...... 9.50 10 mL/L GP2 for bicarbonate—10X stock CaCl2 ·2H2O ...... 1.32 solution as it is not soluble in a 100X solution.

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Adjust to pH 8.0 prior to autoclaving.

TABLE 2—TEST OIL CHARACTERISTICS

Category Density, mg/ API gravity Viscosity @ Category by Oil mL @ 15 °C (deg) 15 °C, (cSt) by API kinematic gravity viscosity

ANS ...... 884 28.2 40 Medium .... Light IFO120 ...... 948 17.5 1520 Heavy...... Heavy

TABLE 3—STOCK SOLUTION TABLE 3—STOCK SOLUTION TABLE 3—STOCK SOLUTION PREPARATION PREPARATION—Continued PREPARATION—Continued

Item Amount Item Amount Item Amount

Mass of Bottle, g ...... 29.9666 Mass of disp + oil + DCM, g .... 25.0759 Density of solution, g/mL ...... 1.3216 Mass of Bottle + oil, g ...... 31.5734 Mass of 1 mL syringe, g ...... 14.5563 Volume of solution, mL ...... 18.9740 Mass of bottle + disp + oil + Mass of 1 mL syringe + solu- Conc. Of stock solution, mg/mL 84.6850 DCM, g ...... 55.0425 tion, g ...... 15.8779 Mass of oil, g ...... 1.6068

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2.11 References for Section 2.0 (4) Venosa, A.D., D.W. King, and G.A. 3.0 Dispersant Toxicity Testing (1) U.S. Environmental Protection Agency Sorial. 2002. ‘‘The baffled flask test for 3.1 Summary. This laboratory protocol (1994), ‘‘Swirling Flask Dispersant dispersant effectiveness: A round robin includes testing for: (1) Dispersant standard Effectiveness Test,’’ Title 40 Code of Federal evaluation of reproducibility and static acute toxicity tests for the mysid Regulations, Pt. 300, Appendix C, pp 47458– repeatability.’’ Spill Sci. & Technol. Bulletin shrimp, Americamysis bahia (48-hr duration) 47461. 7(5–6):299–308. and the inland silverside, Menidia beryllina (2) Sorial, G.A., A.D. Venosa, K.M, Koran, (5) Spotte, S., G. Adams, and P.M. Bubucis. (96-hr duration); (2) dispersant/oil mixture E. Holder, and D.W. King. 2004. ‘‘Oil spill 1984. ‘‘GP2 medium is an synthetic seawater static acute toxicity tests for Americamysis dispersant effectiveness protocol: I. Impact of for culture or maintenance of marine bahia and Menidia beryllina (48-hr and 96- operational variables.’’ ASCE J. Env. Eng. hr duration, respectively); (3) dispersant organisms,’’ Zoo Biol, 3:229–240. 130(10):1073–1084. developmental assay for the purple sea (6) Grubbs, F. 1969. ‘‘Sample Criteria for (3) Sorial, G.A., A.D. Venosa, K.M, Koran, urchin, Strongylocentrotus purpuratus, (72- E. Holder, and D.W. King. 2004. ‘‘Oil spill Testing Outlying Observations,’’ Annals of hr duration); and (4) dispersant 7-day static dispersant effectiveness protocol: II. Mathematical Statistics, pp. 27–58. subchronic tests with Americamysis bahia Performance of revised protocol.’’ ASCE J. and Menidia beryllina (Table 6 of this Env. Eng. 130(10):1085–1093. Appendix).

TABLE 6—TOXICITY TESTING REQUIREMENTS FOR DISPERSANTS

Test procedure 96-hr static 48-hr static 72-hr sea 7-day sub- acute: acute: urchin De- chronic: M. Test substance Menidia Americamysis velopmen- beryllina & beryllina Bahia tal Assay A. bahia

Dispersant only ...... yes ...... yes ...... yes ...... yes. Dispersant/Reference Oil Mixture ...... yes ...... yes ...... no ...... no.

3.2 Preparation of Stock Solutions air bubbles on the oil surface slick. Adjust 3.3.2 Exposure Concentrations. Exposure 3.2.1 Dispersant. Prepare a 1000 mL/L the stir plate to obtain an oil vortex of 25% solutions are prepared by adding the primary stock solution prior to test initiation of the total volume of the seawater, then add appropriate amount of stock solution directly by adding 1.1 mL of dispersant to 1100 mL the dispersant to be tested at a ratio of 1:10 to dilution water in each test chamber. Mix of dilution water consisting of salinity dispersant:oil (2.5 g/L). Securely seal the each exposure solution using five rotations in adjusted uncontaminated natural or artificial bottle to reduce the loss of volatiles using a one direction followed by five rotations in seawater, in a glass vessel. Using a laboratory silicon stopper and wraps of Parafilm and stir the opposite direction using a solid glass stir top stirrer equipped with a stainless steel for 18 hours, then allow the solution to settle rod. blade, center the stirrer blade in the mixing for 6 hours. Maintain the temperature at 25 3.3.3 Reference Toxicants. Separate vessel one inch off the bottom. Initially mix °C during stirring and settling. Purge the hose toxicity tests must be performed with a the resulting stock solution for approximately at the base of the bottle of any material reference toxicant for each species tested. five seconds at speeds of < 10,000 rpm to followed by removal of the CE–WAF Conduct additional reference toxicity tests avoid foaming. Thereafter, set the speed to (aqueous phase) into a clean glass container any time a change in the population or provide a 70% vortex. Using a glass pipette, without disturbing the surface oil slick. The source of a test species occurs. Use sodium remove appropriate aliquots of stock solution CE–WAF should be remixed and 1–2 L dodecyl sulfate (SDS), also known as dodecyl from between the mixing vessel wall and removed for chemical analysis of total sodium sulfate (DSS), and sodium lauryl edge of the vortex and place directly into the petroleum hydrocarbons (TPH) following the sulfate (SLS) as the reference toxicant for dilution water within an exposure vessel. procedures outlined in section 3.4 of this exposures conducted with Menidia beryllina Suspend mixing of the stock solution after Appendix. The remaining volume will be and Americamysis bahia. Use copper the removal of each aliquot. Base the used for the preparation of exposure chloride as the reference toxicant for preparation of exposure solutions on the solutions following procedures outlined in exposures conducted with the sea urchin nominal concentration of the stock solution developmental test. Use reagent grade quality and follow procedures outlined in sections section 3.3 of this Appendix. To reduce time and cost, mix sufficient amounts of SDS and copper chloride for tests. 3.5 and 3.6 of this Appendix. Information on procedures for conducting 3.2.2 Dispersant-Reference Oil(s) dispersant product-reference oil mixture CE– reference toxicant tests with these species Mixtures. Use IFO 120 and ANS oils. To WAF to allow preparation of exposure can be found in the specific EPA methods obtain these oils at no charge (except for a solutions for conducting simultaneous acute documents cited in sections 3.5.1, 3.6.1 and minimal shipping fee) see http:// tests with both Americamysis bahia and www.epa.gov/emergencies/content/ncp/ Menidia beryllina. 3.7.1 of this Appendix. 3.4 Chemical Analysis of Stock Solutions. index.htm. Assessment of dispersant- 3.3 Preparation of Exposure Concentrations reference oil mixture (DOM) toxicity is Add the 1L sample of CE–WAF (Section 3.2.2 3.3.1 Concentration Selection. of this Appendix) solutions directly to amber determined for each reference oil using the ® aqueous phase of a chemically enhanced- Preliminary rangefinder tests may be glass bottles with Teflon -lined cap. Collect water accommodated fraction (CE–WAF). necessary using a series of logarithmic a replicate sample in the event of accidental Repeat the following procedure for each concentrations (e.g. 0.1, 1, 10, 100 ml loss or if reanalysis of the stock solution reference oil tested. Fit a glass aspirator dispersant product/L or mg TPH/L) to becomes necessary. Adjust sample to a pH=2 bottle (approximately 23L) equipped with a determine the appropriate exposure using 50% hydrochloric acid, immediately hose bib at the base with a length of silicon concentration range necessary to determine refrigerate and analyze within 48 hours of tubing containing a hose clamp. Fill the LC50 values and 95% confidence intervals. collection. Analyze samples for C9–C32 TPH bottle with 19L of seawater leaving a 20% For definitive tests, conduct a minimum of by gas chromatography-flame ionization headspace above the liquid, place on a five test concentrations using a geometric detection (GC–FID) following EPA SW–846, magnetic stir plate then add and center a stir ratio between 1.5 and 2.0 (e.g. 2, 4, 8, 16, and Method 8015B–DRO (4). Report TPH bar. Add the respective crude oil at 25g/L 32). Note that when testing only the concentration of stock solutions as using a silicon tube attached to a glass funnel dispersant product, the highest test milligrams TPH/L and use in the calculation that reaches just below the water surface. concentration must not exceed the of exposure concentrations for all toxicity Using this method reduces the production of dispersant’s self-dispersibility limit. tests conducted with CE–WAF.

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3.5 Static Acute Tests With M. beryllina and 50% of the embryos) with 95% confidence 3.7.5 Test Acceptability. Requirements of A. bahia intervals are to be determined in place of an the assay are: (i) ≥80% survival in the control 3.5.1 General. Use EPA’s Methods for IC25. The concentration of dispersant causing treatment for each species, (ii) dry weights Measuring the Acute Toxicity of Effluents inhibition of development in 50% of exposed must meet the specific requirements as and Receiving Waters to Freshwater and embryos (IC50) with the lower and upper 95% stipulated in Method 1006.0 for Menidia Marine Organisms (EPA–821–R–02–012) (1) confidence intervals (LCI95 and ULCI95) must beryllina and Method 1007.0 for for testing each species separately with be calculated at the end of the exposure Americamysis bahia, (iii) egg production dispersant product or a mixture of dispersant period. Mortality determinations are not must occur in 50% of female Americamysis required. product and reference oil (DOM). bahia in the replicate control treatments. 3.6.6 Test Acceptability. Requirements of 3.5.2 Test Solutions. Modify procedures 3.7.6 Subchronic Test Summary. A the assay are: (i) ≥ 80% normal larval in EPA–821–R–02–012 specifically dealing summary of required test conditions for each with the handling and toxicity testing of development in the control treatment, (ii) the minimum significant difference (MSD) that species is provided in Table 7 of this effluents or receiving water samples as can be statically detected relative to the Appendix. follows: Prepare stock solutions following control is ≤25%, (iii) test results which 3.8. Laboratory Report. The laboratory section 3.2 of this Appendix and exposure support the determination of a statistically must include, for each toxicity test report, all concentrations following section 3.3 of this valid IC and 95% confidence interval applicable information, data and analyses as Appendix. 50 unless the LC is >1000 ml/L or is greater follows: 3.5.3 Number of Treatments, Replicates 50 than the limits of water solubility of 3.8.1 Test Objective: Protocol title and and Organisms. Conduct a minimum of three dispersibility. source, endpoint(s); replicates of at least five exposure treatments 3.6.7 Urchin Developmental Test 3.8.2 Product Information: Product name, plus a minimum of three replicate dilution Summary. A summary of required test water controls. Expose ten organisms per manufacturer contact information, lot conditions is provided in Table 7 of this number, production date, date received/ replicate treatment. Appendix. 3.5.4 Exposure Period. Test duration is chain of custody; 48-hr for Americamysis bahia and 96-hr for 3.7 Seven-Day Subchronic Tests With M. 3.8.3 Contract Facility: Contact Menidia beryllina. Mortality must be beryllina and A. bahia information; recorded at each 24 hour period of each test. 3.7.1 General. Use Section 13, Method 3.8.4 Dilution Water: Source, 3.5.5 Test Acceptability. For each test 1006.0, ‘‘Inland Silverside (Menidia pretreatment, physical and chemical performed, survival of control animals must beryllina) Larval Survival and Growth characteristics (pH, salinity); be >90% and test results must allow Method,’’ and Section 14, Method 1007.0, 3.8.5 Test Conditions: Date and time of determination of statistically valid LC50 and ‘‘Mysid (Mysidopsis [renamed Americamysis] test (start and end), test chambers type and 95% confidence interval values except in bahia) Survival, Growth, and Fecundity volume, volume of solution per chamber, cases where the LC50 is >1000 ml/L or is Method’’ of EPA’s Short-Term Methods for number of organisms per chamber, number of determined to be greater than the limits of Estimating the Chronic Toxicity of Effluents replicate chambers per treatment, feeding water solubility of dispersibility. and Receiving Waters to Marine and frequency, amount and type of food, test 3.5.6 Static Acute Test Summary. A Estuarine Organisms (EPA–821–R–02–014) concentrations, test temperature (mean and summary of required test conditions is (3) for testing of dispersant product. range), test salinity (mean and range); provided in Table 7 of this Appendix. 3.7.2 Test Solutions. Modify procedures 3.8.6 Test Organisms: Common and 3.6 Sea Urchin Developmental Test With in EPA–821–R–02–014, sections 13 and 14 scientific name, source contact information, specifically dealing with the handling and Dispersant Product age and date purchased, acclimation toxicity testing of effluents or receiving water conditions (e.g., temperature, salinity, both 3.6.1 General. Use Section 15, ‘‘Purple samples as follows: Prepare stock solutions Urchin, Strongylocentrotus purpuratus and following section 3.2.1 of this Appendix and mean and range), age at test start; Sand Dollar, Dendraster excentricus Larval exposure concentrations following section 3.8.7 Reference toxicant: Date received, Development Test Method’’ of EPA’s Short- 3.3 of this Appendix. Exposure solutions lot number, date of most recent test, results Term Methods for Estimating the Chronic should be renewed every 24 hr for the and current Cumulative Sum Chart, dilution Toxicity of Effluents and Receiving Waters to duration of the test. water used, physical and chemical methods West Coast Marine and Estuarine Organisms 3.7.3 Number of Treatments, Replicates used; (EPA/600/R–95–136) (2). and Organisms. (i) Menidia beryllina: 3.8.8 Quality Assurance: Verification of 3.6.2 Test Organism. Tests of dispersant Conduct a minimum of four replicates of at laboratory accreditation, including products are to follow methods for the purple least five exposure treatments plus a subcontractor facilities; urchin only. Tests with the sand dollar are minimum of four replicate dilution water 3.8.9 Test Results: Raw data in tabular not required. controls. Expose ten M. beryllina per and graphical form, daily records of affected 3.6.3 Test Solutions. Modify procedures replicate treatment. (ii) Americamysis bahia: organisms in each concentration replicate in EPA/600/R–95–136, Section 15 Conduct a minimum of eight replicates of at and controls, table of required endpoints (i.e., specifically dealing with the handling and least five exposure treatments plus a LC50 with 95% confidence interval (CI), IC25 toxicity testing of effluents or receiving water minimum of eight replicate dilution water and IC with 95% CI, LOEC and NOEC), samples as follows: Prepare stock solutions 50 controls. Expose five A. bahia per replicate statistical methods used to calculate following section 3.2.1 of this Appendix and treatment. endpoints, summary tables of test conditions exposure concentrations following section 3.7.4 Exposure Duration and Test and QA data; 3.3 of this Appendix. Endpoint. The test duration is seven days for 3.6.4 Number of Treatments and both species. Test endpoints for Menidia 3.8.10 Analytical Results: Method Replicates. Conduct a minimum of four beryllina are survival and growth (dry summary including Limit of Detection replicates of five exposure treatments plus a weight) and for Americamysis bahia is (LOD)/Limit of Quantitation (LOQ), minimum of four replicate dilution water survival, growth (dry weight) and fecundity. deviations and reasons if any, sample controls. Calculate an LC50 and 95% confidence summary, results including chromatograms 3.6.5 Exposure Duration and Test interval for survival and IC25 and IC50 with and data qualifiers, QA summary including Endpoint. Examine the effects of the 95% confidence intervals for growth (and calibration curves, method blank and dispersant product on normal development fecundity for A. bahia only). Report the surrogate recovery, analytical results of sea urchin embryos over a period of 72 lowest observed effect concentration (LOEC) summary; and hours. An IC50 (the exposure concentration at and no observed effect concentration (NOEC) 3.8.11 Conclusions: Relationship between which normal development is inhibited in for each endpoint. test endpoints and threshold limit.

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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 (daily) Static renewal (daily) Static non-renewal. Test duration ...... 96 hours ...... 48 hours ...... 7 days ...... 7 days ...... 72 ± 2 hours. Salinity ...... 20 ± 2‰ ...... 20 ± 2‰ ...... 20 ± 2‰ ...... 20 ± 2‰ ...... 34 ± 2‰.

Temperature ...... 25 ± 1 °C. Test temperatures must not deviate (maximum minus minimum temperature) by for 15 ± 1 °C. than 3 °C during the test.

Light quality ...... Ambient laboratory illumination

Light intensity ...... 10–20 μE/m2/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 vol- 200 mL ...... 200 mL ...... 500–750 mL ...... 150 mL ...... 10 mL. ume 1. Age of test orga- 9–14 days ...... 1–5 days ...... 7–11 days ...... 7 days ...... 1 hr old fertilized eggs. nism 2. No. organisms per 10 ...... 10 ...... 10 ...... 5 ...... 25 embryos per mL. test chamber. No. of replicate 3 ...... 3 ...... 4 ...... 8 ...... 4. chambers per con- centration.

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 (re- ≥90% survival in con- ≥90% survival in For controls: ≥80% For controls: ≥80% ≥80% normal shell de- quired). trols. controls. survival; average survival; average velopment in controls. dry weight ≥0.5mg dry weight ≥0.20 where test starts mg; ≥ 50% of con- with 7 day old lar- trol females vae, or ≥ 0.43 mg produce eggs. 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 (3) U.S. EPA. 2002. Short-Term Methods for 4.0 Standard Acute Toxicity Testing of (1) U.S. EPA. 2002. Methods for Measuring Estimating the Chronic Toxicity of Surface Washing Agents, Bioremediation the Acute Toxicity of Effluents and Effluents and Receiving Waters to Marine Agents, Herding Agents, and Solidifiers. Receiving Waters to Freshwater and and Estuarine Organisms U.S. 4.1 Summary. This laboratory protocol Marine Organisms. Fifth Edition. U.S. Environmental Protection Agency, includes testing for: (1) Saltwater standard Environmental Protection Agency, Washington, DC (EPA–821–R–02–014). static acute toxicity tests for test products Washington, DC (EPA–821–R–02–012). (4) U.S. EPA. 2008. Test Methods for with the mysid shrimp, Americamysis bahia (2) U.S. EPA. 1995. Short-Term Methods for Evaluating Solid Waste, Physical/ (48-hr duration) and the inland silverside, Estimating the Chronic Toxicity of Chemical Methods U.S. Environmental Menidia beryllina (96-hr duration); and (2) Effluents and Receiving Waters to West freshwater standard static acute toxicity tests Protection Agency, Washington, DC Coast Marine and Estuarine Organisms. for test products with the daphnid, (SW–846) http://www.epa.gov/osw/ First Edition. U.S. Environmental Ceriodaphnia dubia (48-hr duration) and the Protection Agency, Washington, DC hazard/testmethods/sw846/online/ fathead minnow, Pimephales promelas (96-hr (EPA/600/R–95–136) index.htm. duration) (see Table 8 of this Appendix).

TABLE 8—TOXICITY TESTING REQUIREMENTS FOR SURFACE WASHING AGENTS, HERDING AGENTS, BIOREMEDIATION AGENTS AND SOLIDFIERS

Test procedure 96-hr static 48-hr static 96-hr static 48-hr static Application environment acute: acute: acute: acute: Menidia Americamysis Pimephales Ceriodaphnia beryllina bahia promelas dubia

Saltwater only ...... yes ...... yes ...... no ...... no. Freshwater only ...... no ...... no ...... yes ...... yes. Freshwater and saltwater use ...... yes ...... yes ...... yes ...... yes.

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4.2 Dilution Water. Use Section 7 of used for the preparation of exposure 4.5.6 Static Acute Test Summary. A EPA’s Methods for Measuring the Acute solutions following procedures outlined in summary of required test conditions is Toxicity of Effluents and Receiving Waters to section 4.4 of this Appendix. provided in Table 9 of this Appendix. Freshwater and Marine Organisms (EPA– 4.4 Preparation of Exposure Concentrations 4.6 Freshwater Static Acute Tests With 821–R–02–012) [1] for preparation of the 4.4.1 Concentration Selection. Pimephales promelas and Ceriodaphnia appropriate dilution water for each species dubia tested. Use of clean natural or synthetic Preliminary rangefinder tests may be seawater for tests conducted with saltwater necessary using a series of logarithmic 4.6.1 General. Use EPA’s Methods for species is acceptable. concentrations (e.g. 0.1, 1, 10, 100 ml test Measuring the Acute Toxicity of Effluents product/L) to determine the appropriate and Receiving Waters to Freshwater and 4.3 Preparation of Stock Solutions exposure concentration range necessary to Marine Organisms (EPA–821–R–02–012) (1) 4.3.1 Liquid Surface Washing Agents determine LC50 values and 95% confidence for testing each species separately with the and/or Herding Agents. Prepare a 1000 mL/ intervals. For definitive tests, conduct a test product. L stock solution prior to test initiation by minimum of five test concentrations using a 4.6.2 Test Solutions. Modify procedures adding 1.1 mL of test product to 1100 mL of geometric ratio between 1.5 and 2.0 (e.g. 2, in EPA–821–R–02–012 specifically dealing dilution water in a glass vessel. Place on a 4, 8, 16, and 32). Note that when testing the with the handling and toxicity testing of magnetic stir plate then add and center a stir product, the highest test concentration effluents or receiving water samples as bar and adjust the stir plate to obtain a vortex should not exceed the test product’s self- follows: Prepare stock solutions following the of 25% of the total volume of the liquid. Mix dispersibility limit. appropriate sections (4.3.1, 4.3.2, or 4.3.3) of the resulting stock solution for approximately 4.4.2 Exposure Concentrations. Exposure this Appendix and exposure concentrations five minutes at room temperature. Using a solutions are prepared by adding the following section 4.4 of this Appendix. glass pipette, remove appropriate aliquots of appropriate amount of stock solution directly 4.6.3 Number of Treatments, Replicates stock solution from between the mixing to dilution water in each test chamber. Mix and Organisms. P. promelas: Conduct a vessel wall and edge of the vortex and place each exposure solution using five rotations in minimum of three replicates of at least five directly into the dilution water within an one direction followed by five rotations in exposure treatments plus a minimum of three exposure vessel. Base the preparation of the opposite direction using a solid glass stir replicate dilution water controls. Expose ten exposure solutions on the nominal rod. organisms per replicate treatment. C. dubia: concentration of the stock solution and 4.4.3 Reference Toxicants. Separate Conduct a minimum of four replicates of at follow procedures outlined in sections 4.6 toxicity tests must be performed with a least five exposure treatments plus a and/or 4.7 of this Appendix, as appropriate. reference toxicant for each species tested. minimum of four replicate dilution water 4.3.2 Bioremediation Agents. For Conduct additional reference toxicity tests controls. Expose five organisms per replicate products consisting of two or more liquid any time a change in the culture population treatment. and/or solid components, prepare the or source of a test species occurs. Use reagent 4.6.4 Exposure Period. Test duration is product following the manufacturers grade quality sodium dodecyl sulfate (SDS), 48-hr for C. dubia and 96-hr for P. promelas. recommended procedure and ensure the test also known as dodecyl sodium sulfate (DSS), Mortality must be recorded at each 24 hour product mixture is completely blended. and sodium lauryl sulfate (SLS) as the period of each test. Prepare a 1000 mL/L stock solution prior to reference toxicant. Information on 4.6.5 Test Acceptability. For each test test initiation by adding 1.1 mL of the test procedures for conducting reference toxicant performed, survival of control animals must product mixture to 1100 mL of dilution water tests with these species can be found in be > 90% and test results must allow in a glass vessel. Place on a magnetic stir section 4 of EPA’s Methods for Measuring the determination of statistically valid LC50 and plate then add and center a stir bar and Acute Toxicity of Effluents and Receiving 95% confidence interval values except in adjust the stir plate to obtain a vortex of 25% Waters to Freshwater and Marine Organisms cases where the LC50 is >1000 ml/L or is of the total volume of the liquid. Mix the (EPA–821–R–02–012) (3). determined to be greater than the limits of resulting stock solution for approximately 4.5 Saltwater Static Acute Tests With water solubility of dispersibility. five minutes at room temperature. Using a Menidia beryllina and Americamysis bahia 4.6.6 Static Acute Test Summary. A glass pipette, remove appropriate aliquots of summary of required test conditions is 4.5.1 General. Use EPA’s Methods for provided in Table 9 of this Appendix. stock solution from between the mixing Measuring the Acute Toxicity of Effluents vessel wall and edge of the vortex and place and Receiving Waters to Freshwater and 4.7 Laboratory Report directly into the dilution water within an Marine Organisms (EPA–821–R–02–012) (1) The laboratory must include, for each exposure vessel. Base the preparation of for testing each species separately with the toxicity test report, all applicable exposure solutions on the nominal test product. information, data and analyses as follows: concentration of the stock solution and 4.5.2 Test Solutions. Modify procedures 4.7.1 Test Objective: Protocol title and follow procedures outlined in sections 4.5 in EPA–821–R–02–012 specifically dealing source, endpoint(s); and/or 4.6 of this Appendix, as appropriate. with the handling and toxicity testing of 4.7.2 Product Information: Product name, 4.3.3 Solid Phase Products. Assessment effluents or receiving water samples as manufacturer contact information, lot of the toxicity of solidifiers and other solid follows: Prepare stock solutions following the number, production date, date received/ phase products are determined using the appropriate sections (4.3.1, 4.3.2, or 4.3.3) of chain of custody; aqueous phase of water-accommodated this Appendix and exposure concentrations 4.7.3 Contract Facility: Contact fractions (WAFs) of the test product. Fit a following section 4.4 of this Appendix. information; glass aspirator bottle (approximately 23L) 4.5.3 Number of Treatments, Replicates 4.7.4 Dilution Water: Source, equipped with a hose bib at the base with a and Organisms. Conduct a minimum of three pretreatment, physical and chemical length of silicon tubing containing a hose replicates of at least five exposure treatments characteristics (pH, salinity); clamp. Fill the bottle with 19L of dilution plus a minimum of three replicate dilution 4.7.5 Test Conditions: Date and time of water leaving a 20% headspace above the water controls. Expose ten organisms per test (start and end), test chambers type and liquid, place on a magnetic stir plate then replicate treatment. volume, volume of solution per chamber, add and center a stir bar. Add the test 4.5.4 Exposure Period. Test duration is number of organisms per chamber, number of product at 25 g/L and securely seal the bottle 48-hr for A. bahia and 96-hr for M. beryllina. replicate chambers per treatment, feeding using a silicon stopper and wraps of Mortality must be recorded at each 24 hour frequency, amount and type of food, test parafilm. Adjust the stir plate to obtain a period of each test. concentrations, test temperature (mean and vortex of 25% of the total fluid volume, stir 4.5.5 Test Acceptability. For each test range), test salinity (mean and range); for 18 hours then settle for 6 hours. Maintain performed, survival of control animals must 4.7.6 Test Organisms: Common and the temperature at 25 °C during stirring and be > 90% and test results must allow scientific name, source contact information, settling. Purge the hose at the base of the determination of statistically valid LC50 and age and date purchased, acclimation bottle of any material followed by removal of 95% confidence interval values except in conditions (e.g., temperature, salinity, both the WAF (aqueous phase) into a clean glass cases where the LC50 is >1000 ml/L or is mean and range), age at test start; container without disturbing the product on determined to be greater than the limits of 4.7.7 Reference toxicant: Date received, the surface. The WAF should be remixed and water solubility or dispersibility. lot number, date of most recent test, results

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

TABLE 9—SUMMARY OF TEST CONDITIONS—SURFACE WASHING AGENTS, HERDING AGENTS, BIOREMEDIATION AGENTS AND SOLIDIFIERS TOXICITY

Saltwater Acute Saltwater Acute Freshwater Acute Freshwater Acute M. beryllina A. bahia P. promelas 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‰ ...... 20 ± 2‰ ...... NA ...... NA.

Temperature ...... 25 ± 1 °C. Test temperatures must not deviate (maximum minus minimum temperature) by more than 3 °C during the test.

Light quality ...... Ambient laboratory illumination

Light intensity ...... 10–20 μE/m2/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 concentration 3 ...... 3 ...... 3 ...... 4. (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 28 is due to biodegradation and not some 5.2.7 Balance accurate to 0.1 mg; (1) U.S. EPA. 2002. Methods for Measuring physical loss such as volatilization. The day 5.2.8 Orbital shaker table with clamps the Acute Toxicity of Effluents and Receiving 28 GC/MS results from the killed control sized to hold flasks securely; Waters to Freshwater and Marine Organisms. must not be less than 90% of the day 0 5.2.9 GC/MS instrument equipped with a Fifth Edition. U.S. Environmental Protection results. The sample preparation procedure DB–5 capillary column (30 m, 0.25 mm ID, Agency, Washington, DC (EPA–821–R–02– extracts the oil phase into the solvent and 0.25 mm film thickness) or equivalent, 012). dichloromethane (DCM) (also known as and a split/splitless injection port operating methylene chloride) with a subsequent in the splitless mode, such as a Agilent 6890 5.0 Bioremediation Agent Efficacy Test solvent exchange into hexane. The hexane GC/5973 MS (or equivalent) equipped with Protocol extracts are analyzed by a high resolution gas an auto-sampler for testing multiple samples; 5.1 Summary. This protocol quantifies chromatograph/mass spectrometer (GC/MS) and changes in weathered Alaska North Slope operated in the selected ion monitoring mode 5.2.10 Fixed Rotor Centrifuge. (ANS) crude oil composition of alkanes and (SIM) at a scan rate of >5 scans per second. 5.3 Reagents and Culture Medium aromatics resulting from the use of a Note to 5.1: Artificially distilled at 521 °F bioremediation agent in either artificial (272 °C) to remove the low molecular weight 5.3.1 Stock Seawater Preparation. seawater or freshwater. The manufacturer hydrocarbons to approximate natural Prepare the artificial seawater GP2 (Spotte et may test either one or both freshwater or weathering processes that occur after a spill. al., 1984) following the procedures in section saltwater, depending on the product’s 2.3 of this Appendix, to obtain the final intended use. Biodegradation of the alkanes 5.2 Apparatus. All equipment must be concentration of the salts listed in Table 1 of and aromatics is monitored for 28 days at 20– maintained and calibrated per standard this Appendix, except for the sodium laboratory procedures. 23 °C. Product flasks at Day 28 are compared bicarbonate (NaHCO3) which is prepared to Day 0 flasks to determine reductions in 5.2.1 Assorted flasks and other glassware; separately. Autoclave the artificial seawater. alkanes and aromatics. A positive control of 5.2.2 Graduated cylinders (100 mL); Filter sterilize the concentrated solution of a known oil-degrading bacterial culture 5.2.3 Deionized water; 250 mL sodium bicarbonate through a 0.45 mm supplied by EPA is tested. A negative, sterile borosilicate glass Erlenmeyer flasks; membrane filter and add to the autoclaved control is also set up containing exposure 5.2.4 Pasteur pipettes; and cooled artificial seawater GP2 to obtain water, weathered crude oil, product, and a 5.2.5 Multichannel pipettor (5–50 mL and the final concentration listed in Table 1 of sterilant, sodium azide. The purpose of the 50–200 mL); this Appendix. negative, killed control is to make sure the 5.2.6 Autoclave; environmental room or 5.3.2 Seawater for the positive control disappearance of the oil constituents at day incubator; flasks. Prepare sodium triphosphate (a.k.a.,

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sodium tripolyphosphate) (Na5P3O10), 5.3.4 Freshwater Preparation. The 5.3.6 Freshwater for bioremediation potassium nitrate (KNO3), and ferric chloride artificial freshwater, which is a modification agents that contain living microorganisms hexahydrate (FeCl3 ·6H2O) as a concentrated of Bushnell-Haas medium (Haines et al., but not nutrients or limiting concentrations solution. Filter sterilize through a 0.45 mm 2005), is prepared following the of nutrients. If a bioremediation agent does membrane filter and add to autoclaved concentrations listed in Table 12 of this not include nutrients, then nutrients may be artificial seawater to obtain the final nutrient Appendix and then autoclaved. The pH is added. However, the total concentration of concentrations listed in Table 10 of this adjusted to 7.4 before autoclaving. the nutrients added to the bioremediation Appendix. Calibrate the pH meter at room Constituents removed from the original temperature (approximately 20–23 °C) using agent must not exceed the final formulation are KNO3, K2HPO4 and KH2PO4. commercial buffers of pH 4.0, 7.0, and 10.0, concentrations provided in Table 14 of this as appropriate, prior to use. Adjust the pH of Appendix. the artificial seawater with concentrated TABLE 12—CONSTITUENT CON- hydrochloric acid (HCl) or 10 normality CENTRATIONS FOR ARTIFICIAL TABLE 14—ARTIFICIAL FRESHWATER sodium hydroxide (10 N NaOH), as FRESHWATER NUTRIENT CONCENTRATIONS FOR appropriate. [Bushnell-Haas] BIOREMEDIATION AGENTS HAVING NO NUTRIENTS INCLUDED TABLE 10—ARTIFICIAL SEAWATER Final con- NUTRIENT CONCENTRATIONS Constituent centration (mg/L) Constituent Final concentra- tion, g/L 1 Constituent Final con- centration, g/L MgSO4 · 7H2O ...... 200 as Iron (Fe) ...... not added since CaCl2 · 2H2O ...... 20 iron is already * FeCl3 ·6H2O ...... 0.050 FeCl3 · 6H2O ...... 50 in the fresh- KNO3 ...... 2.890 MnSO4 · H2O ...... 0.0302 water solution. *Na5P3O10 ...... 0.297 H3BO3 ...... 0.0572 as Nitrogen (N) ...... 0.400. ZnSO4 · 7H2O ...... 0.0428 * Added aseptically after the GP2 has been as Phosphorus (P) ...... 0.400. autoclaved to limit phosphorus and iron (NH4)6Mo7O2 ...... 0.0347 precipitation. 1 Adjust to pH 7.4 prior to autoclaving. 5.3.5 Freshwater for the positive control. 5.3.3 Seawater for bioremediation agents To prepare the freshwater for the positive If nutrients are supplied by the product that do not include nutrients. If a controls, prepare the nutrients potassium vendor, the specific composition and bioremediation agent contains living phosphate monobasic (KH PO ), potassium concentration used in the efficacy testing microorganisms but not nutrients (or limiting 2 4 phosphate dibasic (K HPO ) and potassium concentrations of nutrients), then nutrients 2 4 must be submitted. nitrate (KNO ) as a concentrated solution. may be added by the manufacturer. However, 3 5.3.7 Oil Preparation. The test oil, the total concentration of the nutrients added Filter sterilize and add to autoclaved weathered ANS521 crude oil, can be to the bioremediation agent must not exceed artificial freshwater to obtain the final obtained from EPA at no charge (except for the final concentrations listed in Table 11 of concentrations given in Table 13 of this a minimal shipping fee). See http:// this Appendix. Appendix. Calibrate the pH meter at room www.epa.gov/emergencies/content/ncp/ ° temperature (approximately 20–23 C) using index.htm for more information. commercial buffers of pH 4.0, 7.0, and 10.0, TABLE 11—ARTIFICIAL SEAWATER NU- 5.3.8 Sodium azide sterilant. Prepare a as appropriate, prior to use. Adjust the pH of stock solution of NaN for addition to the TRIENT CONCENTRATIONS FOR BIO- the artificial freshwater to 7.4 with 1 N HCl 3 negative killed control. The final REMEDIATION AGENTS HAVING NO or 1 N NaOH, as appropriate. concentration in the killed controls will be NUTRIENTS INCLUDED 0.5 g/L. TABLE 13—FRESHWATER NUTRIENT 5.4 Experimental Setup and Procedure Constituent Final con- CONCENTRATIONS centration, g/L 5.4.1 Autoclave clean borosilicate glass as Iron (Fe) ...... 0.010 Final con- Erlenmeyer flasks (250 mL) for 20 minutes at Constituent centration 121 °C at 15 psig. as Nitrogen (N) ...... 0.400 (g/L) 1 as Phosphorus (P) ...... 0.075 5.4.2 Label flasks with the appropriate code (negative control, positive control, or KNO3 ...... 2.89 If nutrients are supplied by the product product; day to be sampled (0 or 28); letter KH2PO4 ...... 1.00 manufacturer, the specific composition and indicating replicate number) to reflect the K2HPO4 ...... 1.00 concentration used in the efficacy testing following treatment design in Table 15 of this must be submitted. 1 Adjust pH to 7.4 prior to autoclaving Appendix:

TABLE 15—BIOREMEDIATION EFFICACY TEST—SUMMARY OF EXPERIMENTAL SETUP

Number of replicates at Treatment sampling times Analysis Day 0 Day 28

Negative (killed) Control (oil + exposure water + product + EPA culture + NaN3 sterilant) ...... 0 3 GC/MS *Positive control (oil + exposure water + nutrients + EPA culture) ...... 6 6 GC/MS Test Type 1: Product containing living microorganisms (oil + exposure water + living product + sup- 6 6 GC/MS plemented nutrients (if necessary)). Test Type 2: Product containing proprietary nutrients but no live microorganisms (oil + exposure 6 6 GC/MS water + product + EPA culture). Test Type 3: Product (such as an enzyme) containing no live microorganisms and no nutrients (oil + 6 6 GC/MS 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.

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5.4.3 Aseptically dispense 100 mL of pre- 5.4.6 Positive control flasks contain be reported and must not exceed the sterilized artificial exposure water (seawater exposure water, oil, nutrients, and the EPA concentration limits in Table 10 (for or freshwater) into each flask. For the culture. seawater) and 13 (for freshwater) of this positive control flasks, use exposure water 5.4.7 Negative killed control flasks for all Appendix, as applicable. containing nutrients. Alternatively, the products shall contain exposure water, oil, 5.4.11 Cap all flasks either with cotton artificial exposure water can be dispensed product, the EPA culture for products not stoppers or loosely applied aluminum foil to into clean flasks and then autoclaved. containing a living culture, and the sodium allow gas exchange with the atmosphere. Set 5.4.4 Tare the labeled flasks containing azide sterilant at a final concentration of 0.5 aside the T=0 flasks for immediate extraction exposure water and other additions, as g/L. Add the sodium azide sterilant prior to and analysis. Place the rest of the flasks onto necessary, on the balance with a minimum adding any product or EPA culture. For the the orbital shaker table. Do not tip the flasks accuracy of 0.01 g. Add drop-wise 0.50 g oil negative killed control flasks and product excessively to avoid stranding oil above the (this results in a final oil concentration of 5 flasks, prepare and add the product to the mixing area of the flask. Set the orbital shaker g/L) using a sterile Pasteur pipette to the flasks in a concentration specified by the to 200 rpm and shake the flasks for 28 days center of the flask taking care to avoid manufacturer or vendor. at 20–23° C. splashing the oil onto the sides of the flasks. 5.4.8 For non-living products that contain 5.4.12 Submit all information on added Record the precise weight. ANS521 may be nutrient only, use the EPA culture as the cultures and nutrients for testing in the data previously warmed in a hot water bath to inoculum. report. facilitate its flow. Take precautions when 5.4.9 For other non-living products (e.g., handling and charging the flasks to minimize enzymes), do not add nutrients or the EPA 5.5 Sampling and Chemical Analysis the likelihood of contamination by culture as the inoculum as they are not 5.5.1 Summary. At each sampling event exogenous microbes, including using a new needed. (Days 0 and 28), product and control flasks sterile pipette for each series of flasks. 5.4.10 For products containing microbial are sacrificed for analysis of residual oil 5.4.5 Preparation of the EPA culture for cultures, prepare 6 flasks the same way as in concentrations (SOP 4 of this Appendix). both the positive control flasks and the flasks Steps a-d, but without the EPA culture. A Record all physical observations for each containing non-living bio-stimulation product that contains its own nutrients must flask (such as degree of emulsification, products. Use two vials containing not be amended with nutrients, unless the whether the oil has congealed into tar balls, approximately 5 mL of the known EPA product contains insufficient nutrients. Since wall growth, color, etc.) at each sampling. culture frozen in glycerol. Thaw both vials at this is a closed flask test, nutrients could be The analytical procedure is summarized in room temperature, transfer the contents of limiting if they are at the same concentration Table 16 of this Appendix. Dichloromethane both thawed vials to a single sterile as used in the field. This could cause the (DCM) is the solvent used for the initial centrifuge tube, rinse tubes with two volumes product to fail the test. Thus, the extraction. Solvent-exchange the extract into each of sterile exposure water, centrifuge at manufacturer has the option to supplement hexane prior to injection into the gas between 6,000 and 7,000 ×s gravity (6,000– its product with a higher concentration of chromatograph. The solvent exchange is 7,000 × g) for 15 minutes using a fixed rotor nutrients than that contained in the product. done to prevent asphaltenes from to fully pellet the cells. Any nutrient supplements to a product must contaminating the column.

TABLE 16—BIOREMEDIATION EFFICACY—SUMMARY OF ANALYTICAL PROCEDURES

Preserva- Matrix Measurement Sampling/measurement Analysis Sample container/quantity of tion/stor- Holding method method sample age times

DCM ...... N/A ...... Solvent Exchange to N/A ...... Capped Vial with Teflon 4 °C ...... 6 months. Hexane. septa, 30 mL. Hexane ..... Hydrocarbon Concentration SOP 4 ...... GC/MS ..... Capped Vial with Teflon 4 °C ...... 6 months. septa, 10 mL.

5.5.2 Hydrocarbon Extraction. To lined screw caps. Place the test tubes in a 37° 5.6 Quality Assurance/Quality Control (QA/ measure extraction efficiency, 500 mL of the C water bath under a stream of dry nitrogen QC) surrogate recovery standard (compounds and gas. Reduce the sample to 1 mL and return 5.6.1 Objectives. The critical variables to concentrations described in SOP 1 in this to volume with hexane. Repeat the blow be analyzed for each set of experimental Appendix) is added to each flask. Add 50 mL down and re-suspension twice to exchange conditions are the individual petroleum DCM to each flask. Use magnetic stir bars to the hydrocarbons from DCM into the hexane. hydrocarbons, i.e., the alkanes ranging in stir the flasks for 20 minutes to transfer the 5.5.4 Hydrocarbon Analysis. Quantify the carbon number from nC–14 to nC–35, plus oil into the DCM phase. Allow the flasks to concentrations of 25 alkanes (including pristane and phytane, and the 2- to 4-ring stand one hour for phase separation. If an hopane) and 31 aromatics (SOP 4, Table SOP emulsion remains after one hour, centrifuge polycyclic aromatic hydrocarbons (PAHs) ® 4.1 of this Appendix) using an Agilent 6890 and their alkylated homologs as listed in SOP the emulsion in Teflon centrifuge tubes for GC/5973 MS or equivalent equipped with a at least ten minutes in a low speed centrifuge 4 of this Appendix. The quality assurance 30-m × 0.25-mm ID × 0.25-mm film thickness at 3,000 × gravity (3,000 × g) to break the objectives for precision, accuracy, and DB–5 or equivalent fused silica column. To ± emulsion and recover the DCM phase. Pass detection limits are 20%, 75–125% the DCM extract through a funnel plugged prepare the samples, transfer 1.0 mL of the recovery, and 22.5 mg/L, respectively. For with glass wool and containing hexane extract into a 2 mL autosampler vial more details, refer to the SOPs of this approximately 20 g anhydrous, granular with Teflon lined cap. Add 20 mL of internal Appendix. sodium sulfate (Na2SO4) to remove water. standard solution to each vial with a syringe 5.6.2 Precision Objectives. Precision is Collect the extract in 30 mL serum vials, or positive displacement pipettor. SOP 2 of presented as relative percent difference (RPD) capped with Teflon lined septa and this Appendix outlines the procedure for for duplicate measurements and as relative aluminum crimp seals, and store at 4 °C for preparing the internal standard solution. standard deviation (RSD, or coefficient of up to 6 months. Load vials onto the autosampler tray and variance) for triplicate measurements, 5.5.3 Solvent Exchange. Perform a solvent analyze in selected ion monitoring mode applicable to replication of treatments as exchange (DCM to hexane) prior to GC/MS (SIM). Sum the individual alkane separate samples. analysis to prevent injection of asphaltenes concentrations for the total alkane 5.6.3 Accuracy Objectives. These are into the GC/MS column. Using a Class A concentration and the individual aromatic based on the check standards and standard volumetric pipette, transfer10 mL of DCM concentrations for total aromatic oil samples run concurrently with the sample extract to 16 x 125 mm test tubes with Teflon concentrations in each flask. analyses for GC/MS analysis of critical

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

TABLE 17—QA/QC CHECKS

Sample matrix Measurement QA/QC check Frequency Acceptance criteria Corrective action

DCM ...... GC/MS hydrocarbon Blanks ...... Once per calibrated run Peak area of interfering Flush with solvent, analysis. peaks <10% of lowest clean injection port, standard peak area. and/or bake column. DCM ...... GC/MS hydrocarbon DFTPP Check Standard Once per calibrated run Must pass all DFTPP If any criteria fail, retune analysis. criteria. and rerun DFTPP check standard. DCM ...... GC/MS hydrocarbon Initial Calibration Sam- Once per calibrated run Response Factor RSD If RSD for any one analysis. ples. ≤25%. compound >25%, re- calibrate. DCM ...... GC/MS hydrocarbon Calibration Check Every 10–15 samples ... ± 25% of expected val- If >5 compounds are analysis. Standards. ues. out of range, recali- brate and rerun sam- ples. Hexane ..... GC/MS hydrocarbon Surrogates ...... Every Sample ...... ± 30% of expected val- Re-inject. analysis. ues. Hexane ..... GC/MS hydrocarbon Biomarker Concentra- Every Sample ...... ± 25% of average val- Re-inject. analysis. tion. ues.

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

Where: t95,5df= the 95% one-tailed t-value with 5 5.7.3 Using Equation 12 of this Appendix, degrees of freedom (2.015), calculate the % reduction of each oil fraction xt28 = total hopane-normalized alkane or total hopane-normalized aromatic mean of 6 s = the standard deviation of the 6 replicates from day 0 to day 28, using the day 0 and at day 0 and 28, and 28 UCL hopane-normalized values for each replicates at days 0 and 28, 95 n = no. of replicates = 6. fraction:

Where: For freshwater, a product is successful if the 5.8 Data Verification and Reporting. GC/

t28(UCL95) = UCL95 of the hopane-normalized % reduction of total alkanes and total MS data files are generated by MS total alkane or total aromatic mean of 6 aromatics is greater than or equal to 95% and ChemStation software (the Agilent standard replicates on day 28, and 40%, respectively. The benchmark reduction software for GC/MS) or equivalent for each t0(UCL95) = UCL95 of the hopane-normalized ranges in aliphatic and aromatic fractions for injection. Data files contain summed ion total alkane or total aromatic mean of 6 the positive control are the same as for the chromatograms and selected ion replicates on day 0. products specified above. The average chromatograms. Calibration curves are 5.7.4 A product is successful in saltwater concentration of the biomarker hopane at day generated within MS ChemStation software, if the % reduction of total alkanes (aliphatic 28 must not differ from the average and all data files are calculated against the fraction) from the GC/MS analysis is greater concentration at day 0 by more than 12% in calibration curve by MS ChemStation. Data than or equal to 95% and the % reduction the positive control. If the conditions for the verification would be done by crosschecking of total aromatics (aromatic fraction) is greater than or equal to 70% at day 28 based positive control are not met, the entire between analysts for 10% of the raw data and procedure must be repeated. its reduction process. on the UCL95 (Equation 12 of this Appendix).

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5.9 Laboratory Report. The summary of 5.10.1.3 Quality Control: Inject 20 mL of 5.10.2.2.9 Before using, allow the findings from a product test must include the the surrogate stock solution into 1 mL DCM. solution to come to room temperature, and data listings for each analyte that was Add 20 mL of the internal standard solution then shake it well. analyzed (i.e., all individual alkanes and (SOP 2 of this Appendix). Analyze this 5.10.2.2.10 Weigh the vial before using it, aromatics in the list of required analytes). solution by GC/MS using a calibrated method and compare the weight with the last weight Express all concentrations as mg analyte/L (SOPs 3 and 4 of this Appendix). The recorded on the vial. exposure water. expected concentration of each of the 5.10.2.2.11 If the weights are consistent, ± 5.10 Standard Operating Procedures (SOPs) corresponding surrogate compounds is 8 2 the integrity of the solution can be assumed. 1–4 mg/L. If the measured value does not fall If not, investigate and resolve the cause. within this range, prepare and measure 5.10.1 SOP 1. Preparation of Surrogate Prepare a new solution if the integrity has another independent surrogate solution. If been compromised. Recovery Standards the measured concentration of the second 5.10.1.1 Preparation: 5.10.2.3 Quality Control: Inject 20 mL of surrogate solution is within the allowable the internal standard solution into 1 mL 5.10.1.1.1 Solvents: Dichloromethane tolerance range, the calibration and DCM. Analyze this solution by GC/MS. The (DCM), Optima (Fisher) grade or equivalent. instrument conditions are acceptable; only peaks corresponding to the internal 5.10.1.1.2 Reagents: D36-Heptadecane properly discard the first surrogate solution. standards must appear. If other peaks appear, (C17), D50-Tetracosane (C24), D66- If the concentration of the second surrogate particularly close to the internal standard Dotriacontane (C32), D10–1- solution is also out of range, then clean and peaks, discard the internal standard solution Methylnaphthalene, D10-Phenanthrene, D10- recalibrate the instrument until the problem Pyrene, 5-beta-cholestane (coprostane). is resolved. and prepare a new solution. Note: Deuterated reagents are available 5.10.2 SOP 2. Preparation of Internal 5.10.3 SOP 3. Preparation of Working from Cambridge Isotope Laboratories, Standard Solution Standards, Check Standards, and Oil Andover, MA. Standards for GC/MS Consistency. 5.10.1.1.3 Equipment: Micro-spatula, 5.10.2.1 Preparation 5.10.3.1 Preparation: Small beakers, Glass funnel, Analytical 5.10.2.1.1 Solvents: Dichloromethane 5.10.3.1.1 Solvent: Dichloromethane balance (0.0001g), Vials with Teflon-lined (DCM), Optima (Fisher) grade or equivalent. (DCM), Optima (Fisher) grade or equivalent. caps, Teflon wash bottle with Optima grade 5.10.2.1.2 Reagents: D34 n-Hexadecane 5.10.3.1.2 Stock solutions: DCM, Volumetric flask (250 mL), class A, (C16), D42 n-Eicosane (C20), D62 n- 5.10.3.1.2.1 Oil analysis standard: 44 Pasteur pipettes. Triacontane (C30), D8-Naphthalene, D10- compounds, 100 mg/L in hexane/DCM (9:1), 5.10.1.2 Procedure: Anthracene, D12-Chrysene, 5-alpha- four, 1-mL vials required. Available from 5.10.1.2.1 Using a calibrated analytical Androstane. Absolute Standards, Inc., Hamden, CT, Part balance, weigh 100 mg (0.100 g) of each Note: Deuterated reagents are available # 90311. reagent into separate 10–25 mL beakers. from Cambridge Isotope Laboratories, 5.10.3.1.2.2 Nine compound PAH 5.10.1.2.2 Dissolve the reagents in their Andover, MA. standard: 1,000 mg/L in DCM, one vial. beakers by adding 10 mL DCM. Use a Pasteur 5.10.2.1.3 Equipment: Micro-spatula, Available from Absolute Standards, Inc., pipette to transfer the solutions to a single Small beakers, Glass funnel, Analytical Hamden, CT, Part # 90822. 250 mL volumetric flask. balance (0.0001g), calibrated and checked for 5.10.3.1.2.3 1,2-Benzodiphenylene 5.10.1.2.3 Wash the beakers 3 or 4 times accuracy, Amber vials with Teflon-lined sulfide, (synonym for with DCM. Use a Pasteur pipette to transfer caps, labeled, Teflon wash bottle with DCM, naphthobenzothiophene). Prepare a 2 mg/mL each of the washings to the 250 mL Volumetric flask (200 mL), class A, Pasteur stock solution. Available from Sigma-Aldrich volumetric flask. pipettes. Co., Part # 255122, purity 99%. 5.10.1.2.4 Dilute the solution to the 250 5.10.2.2 Procedure: 5.10.3.1.2.4 Hopane solution (17 b (H), mL volume mark on the volumetric flask 5.10.2.2.1 Using a calibrated analytical b with DCM. balance, weigh 100 mg (0.100 g) of each of 21 (H), 0.1 mg/mL in isooctane. Available 5.10.1.2.5 Use a glass stopper to seal the the reagents into separate small beakers. from Sigma-Aldrich Co. Part # 07562. flask and homogenize the solution by 5.10.2.2.2 Dissolve the reagents in their 5.10.3.1.2.5 Surrogate solution: 400 mg/L inverting the flask 5 or more times. The final beakers by adding 10 mL DCM; using a of each reagent in DCM (see SOP 1 of this concentration of this solution is 400 mg/L for Pasteur pipette, transfer the solutions to a Appendix). each of the reagents. single 200 mL volumetric flask. 5.10.3.1.2.6 Internal standard solution, 5.10.1.2.6 Transfer the solution into 40 5.10.2.2.3 Wash the beakers 3 or 4 times 500 mg/L in DCM (see SOP 2 of this mL storage vials and cap with Teflon-lined with DCM; use a Pasteur pipette to transfer Appendix). caps and label each with the date of each of the washings to the 200 mL volume 5.10.3.1.3 Alaska North Slope Crude Oil preparation, operator, sample names, and mark on the volumetric flask. 521 (ANS521). concentrations. 5.10.2.2.4 Dilute the solution with DCM 5.10.3.1.4 Equipment: 5.10.1.2.7 Weigh each vial and record its to the 200 mL volume. 5.10.3.1.4.1 Glass storage vials with weight on the label. This weight is used to 5.10.2.2.5 Seal the flask with a glass Teflon-lined caps (2 mL and 40 mL capacity); monitor possible evaporation during storage. stopper and homogenize the solution by 5.10.3.1.4.2 Volumetric flasks, Class A, 5 5.10.1.2.8 Store these vials at 0 °C or inverting the flask a minimum of 5 times. mL, 10 mL, and 100 mL. lower. The final concentration of this solution is 500 5.10.3.1.4.3 Glass syringes capable of 5.10.1.2.9 Before using, allow the mg/L of each reagent. dispensing 25–500 mL with an accuracy and solution to come to room temperature, and 5.10.2.2.6 Transfer the solution into 40 precision of ± 1%, or equivalent. then shake it well. mL storage vials and cap with Teflon-lined 5.10.3.1.4.4 Wheaton repetitive 5.10.1.2.10 Weigh the vial before using it, caps. Label each vial with the date of dispenser, Model 411 STEP–PETTE or and compare the weight with the last weight preparation, operator, sample names, and equivalent. recorded on the vial. concentrations. 5.10.3.1.4.5 Teflon wash bottle filled with 5.10.1.2.11 If the weights are consistent, 5.10.2.2.7 Weigh each vial, and record its Optima grade DCM or equivalent grade DCM. the integrity of the solution can be assumed. weight on the label. This weight is used to 5.10.3.1.4.6 Pasteur pipettes. If not, investigate and resolve the cause. monitor possible evaporation during storage. The volumes of stock solutions required to Prepare a new solution if the integrity has 5.10.2.2.8 Store this solution at 0 °C or make the working standards are listed in been compromised. lower. Table SOP 3.1 of this Appendix.

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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- Mix (44 Mix (9 com- diphenylene Surrogate Hopane so- Volumetric ISTD (500 Working standards concentration, mg/L compounds, pounds, sulfide solution lution (100 Flask Volume mg/L) 100 mg/L) 1000 mg/L) (NBT) (2 (100 mg/L) mg/L) mL μL μ μ mg/mL) μL μL L L μL

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

5.10.3.4.2 The RSD of the RRFs for all either in the SIM (selected ion monitoring) TABLE SOP 4–1—IONS ASSOCIATED analytes must be 25% or less according to mode for quantitative analysis or in SCAN WITH RETENTION TIME GROUPS EPA Method 525.2. mode for qualitative analysis. In SIM mode, 5.10.4 SOP 4. GC/MS Method for the the dwell time of each ion is set to be 10 Group Ions Analysis of Crude Oil Samples. milliseconds and the ions are split up into 5.10.4.1 Instrument Specifications: groups by retention time. One way to divide 1 ...... 57, 66, 128, 136, 142, 152, 156, 5.10.4.1.1 Use an Agilent 6890 GC the ions is by retention time grouping as 166, 170, 184 coupled with an Agilent 5973 mass selective shown in Table SOP 4–1 of this Appendix. 2 ...... 57, 66, 166, 170, 178, 180, 184, detector (MSD) and an Agilent 6890 series The number of ions in each ion group must 188, 192, 194, 198, 208 auto sampler or equivalent, equipped with a be constant, yielding the same scan rate for 3 ...... 57, 66, 178, 184, 188, 192, 194, DB–5 capillary column (30 m, 0.25 mm I.D., each group. 198, 202, 206, 208, 212, 220, and 0.25 mm film thickness) or equivalent, 226 and a split/splitless injection port operating in the splitless mode. Data acquisition occurs

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TABLE SOP 4–1—IONS ASSOCIATED TABLE SOP 4.2—INSTRUMENTAL CON- 5.10.4.3.2.2 Mass assignments within ± WITH RETENTION TIME GROUPS— DITIONS FOR CRUDE OIL ANALYSIS— 0.2 amu’s from 69, 219, and 502; 5.10.4.3.2.3 Peak widths within 0.5 ± 0.1 Continued Continued amu’s; 5.10.4.3.2.4 Relative abundance is 100% Group Ions Flow Rate ...... Constant flow at 1mL/ min. Linear velocity: for ion 69, at least 35% for ion 219, and at least 1% for ion 502; 4 ...... 57, 66, 192, 198, 202, 206, 208, 36.2 cm/sec. μ 5.10.4.3.2.5 Relative abundances for 212, 216, 220, 226, 230, 234, Injection Volume .... 1 L. ± Split/Splitless Mode Splitless. isotope masses 70, 220, and 503 0.2 amu’s 245 are 0.5–1.5%, 2–8%, and 5–15%, Total Run Time ...... 59.18 minutes. 5 ...... 57, 66, 191, 217, 228, 240, 242, respectively; and 248, 256, 262, 264, 270, 276, 5.10.4.3.2.6 Air and water peaks at m/z = 284 5.10.4.2 Procedure for preparing the 18, 28, 32, and 44 amu’s must be very small instrument: and consistent with historical values. 5.10.4.2.1 Lower the injection port 5.10.4.1.2 Table SOP 4.2 of this Appendix 5.10.4.4 Maintaining a log book. Maintain temperature and the oven temperature to 50° summarizes the instrumental conditions for an instrument logbook, and make entries for C or less to avoid oxidation of the column. crude oil analysis. Use only ultra-high purity each use. Include the following information 5.10.4.2.2 Replace the liner with a clean, in the logbook: operator name, helium helium (99.999% pure) as the carrier gas. In silanized liner. Do not touch the liner with series, connect a moisture trap, an oxygen cylinder tank pressure and outlet pressure, bare fingers. A small piece of muffled glass vacuum gauge reading, any maintenance trap, and an organic trap to the carrier gas wool may be inserted to protect the column. performed on the instrument (such as line before it enters the column. 5.10.4.2.3 Return the injection port and changing the injection port liner, gold seal, oven to the appropriate temperatures. guard column, source cleaning), sequence TABLE SOP 4.2—INSTRUMENTAL 5.10.4.2.4 Wait five minutes after the name, data path, samples in order of CONDITIONS FOR CRUDE OIL ANALYSIS temperature equilibrates before using the injection, method information, GC column instrument. number, and the Standard Auto Tune report 5.10.4.3 Procedure for tuning the MSD: and DFTPP Tune report. Instrument ...... Agilent 6890 Series II 5.10.4.3.1 Perform an air/water check. Gas Chromatograph 5.10.4.5 Running a Solvent Blank: The value reported for the relative abundance Following a liner change or at the start of a (GC) with an Agilent of water (m/z 18), nitrogen (m/z 28), oxygen 5973MSD and an new run, run an injection of a pure solvent (m/z 32), or carbon dioxide (m/z 44) shall be to confirm that the system is free of excessive Agilent 6890 auto less than 5% of the base peak for the system sampler, or equiva- or interfering contamination. Analyze the to be considered leak free. solvent in SCAN mode using the same lent. 5.10.4.3.2 Tune the MSD using the Column ...... DB–5 capillary column temperature program used for sample Standard Autotune program and the analysis. If contamination is present, analyze (30 m, 0.25 mm I.D., decafluorotriphenylphosphine (DFTPP) Tune and 0.25-μm film additional samples of fresh solvent until the program to reduce instrument variability. interfering contamination is removed. thickness) or equiva- The Autotune report file is referenced by the lent. 5.10.4.6 Checking the DFTPP Tune: Prior instrument when performing an air/water to running the first calibration standard, Carrier Gas ...... Helium, ultra-high purity check and thus must be run at least once per verify the instrument tune conditions by grade (99.999%). month. Run standards and samples using m ° running a 10 ng/ L DFTPP check standard to Inlet Temperature .. 300 C. DFTPP Tune parameters, and retune the check the mass measuring accuracy of the ° Transfer Line (de- 310 C. instrument using DFTPP Tune at least once MS, the resolution sensitivity, the baseline tector) Tempera- per week. The tune programs use three threshold, and the ion abundance ranges. ture. fragment ions of perfluorotributylamine Run the standard using the DFTPP method Oven Temperature 50 °C for 4 minutes, (PFTBA) as a standard for tuning: m/z 69, provided with the instrument. Each of the Program. then 7 °C/min to 310 219, and 502. Tune reports must meet the criteria identified in Table SOP 4.2 of this °C, hold for 18 min- following criteria: Appendix must be met before using the utes. 5.10.4.3.2.1 Symmetrical peaks; 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 corresponding deuterated internal standard the calibration standards to validate the Calibration Curve. A 5- or 6-point calibration as indicated in Table SOP 4.3 of this accuracy of the calibration curve. curve is obtained by running 5 or 6 working Appendix. The relative standard deviation 5.10.4.8 Running Samples. Once the standards (see SOP 3) on the tuned GC/MS (RSD) of the RRFs for each compound must calibration curve has been validated, samples instrument. Calculate the relative response be less than 25%. Run an independently can be analyzed. Dispense 1,000 mL of sample factor (RRF) for each compound relative to its prepared check standard immediately after extract into labeled auto-sampler vials. Add

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

TABLE SOP 4.4—TARGET COMPOUND LIST

Quantitation Compound name ion Reference compound for response factor Internal standard for 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.

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TABLE SOP 4.4—TARGET COMPOUND LIST—Continued

Quantitation Compound name ion Reference compound for response factor Internal standard for quantitation

C2 Chrysene * ...... 256 Chrysene. C3 Chrysene * ...... 270 Chrysene. C4 Chrysene * ...... 284 Chrysene. 5a-androstane ...... 245 5a-androstane ...... 5a-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 mg/g oil added:

where: their concentrations are measured in a Concentrations of the analytes in the control

Aanalyte = the peak area of the analyte, consistent way throughout the analysis. chart must be no more than 25% different Cistd = the concentration of the internal 5.10.4.12 Concentration calculations for from their historical averages. standard, all target compounds are performed using 5.10.5.6 Relative response factors for Aistd = the area of the internal standard, EnviroQuant software or equivalent. Data for analytes in the check standards inserted RRF = the relative response factor, and each sample can be printed directly using a between every 10 samples must be no more 100 is the conversion factor to convert mg/ customized report template. Data can also be than 25 percent different from the average L DCM to mg/g oil added. automatically entered into a spreadsheet RRF of those same analytes in the calibration 5.10.4.11 If some analytes are not within the EnviroQuant software. curve. Peak shapes must be symmetrical. 5.10.5 Quality Assurance/Quality commercially available, the RRFs of other 5.11 References for Section 5 Control. The following criteria must be met compounds (usually the parent compound) (1) Haines, J.R., E.J. Kleiner, K.A. McClellan, are used to quantify those analytes. For before any samples are analyzed: K.M. Koran, E.L. Holder, D.W. King, and example, the RRF of C3-naphthalene may be 5.10.5.1 Air/water check to verify the A.D. Venosa. 2005. ‘‘Laboratory used to calculate the concentrations of C3- system is leak free. evaluation of oil spill bioremediation and C4-naphthalenes. See Table SOP 4.4 of 5.10.5.2 AutoTune and DFTPP Tune pass products in salt and freshwater systems.’’ this Appendix for details. The quantification all criteria. J. Ind. Microbiol. Biotech 32: 171–185. of these alkylated PAHs is relative because it 5.10.5.3 DFTPP check standard passes all is assumed that the molecular ions of the criteria. Appendix E to Part 300 [Removed] 5.10.5.4 Solvent blank scan indicates the alkylated PAHs have the same RRFs as the ■ 17. Remove Appendix E to Part 300. parent compound ions. Nevertheless, these GC/MS system is free of interfering relative concentrations are useful for contamination. [FR Doc. 2015–00544 Filed 1–21–15; 8:45 am] 5.10.5.5 Prepare and monitor a control monitoring the fate of these compounds BILLING CODE 6560–50–P during the course of any analysis, as long as chart of a standard oil analysis.

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