3380 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

ENVIRONMENTAL PROTECTION 

AGENCY 

40 CFR Parts 110 and 300 

[EPA–HQ–OPA–2006–0090; FRL–9689–9– 

OSWER] 

RIN 2050–AE87 

National Oil and Hazardous 

Substances Pollution Contingency 

Plan 

AGENCY: U.S. Environmental Protection 

Agency (EPA). 

ACTION: Proposed rule. 

SUMMARY: The Environmental Protection 

Agency (EPA or the Agency) proposes to 

amend the requirements in Subpart J of 

the National Oil and Hazardous 

Substances Pollution Contingency Plan 

(NCP) that govern the use of dispersants, 

other chemical and biological agents, 

and other spill mitigating substances 

when responding to oil discharges into 

waters of the United States (U.S.). The 

proposal addresses the efficacy, toxicity, 

environmental monitoring of 

dispersants, and other chemical and 

biological agents, as well as public, 

state, local, and federal officials’ 

concerns regarding their use. 

Specifically, the proposal amends the 

Subpart J regulatory requirements for 

the NCP Product Schedule (Schedule) 

by adding new listing criteria, revising 

the efficacy and toxicity testing 

protocols, and clarifying the evaluation 

criteria for removing products from the 

Schedule. The Agency also proposes 

amended requirements for the 

authorities, notifications, monitoring, 

and data reporting when using chemical 

or biological agents in response to oil 

discharges to the navigable waters of the 

United States and adjoining shorelines, 

the waters of the contiguous zone, and 

the high seas beyond the contiguous 

zone in connection with activities under 

the Outer Continental Shelf Lands Act, 

activities under the Deepwater Port Act 

of 1974, or activities that may affect 

natural resources belonging to, 

appertaining to, or under the exclusive 

management authority of the United 

States, including resources under the 

Magnuson Fishery Conservation and 

Management Act of 1976. These 

requirements are anticipated to 

encourage the development of safer and 

more effective spill mitigating products, 

and would better target the use of these 

products to reduce the risks to human 

health and the environment. Further, 

the amendments are intended to ensure 

that On-Scene Coordinators (OSCs), 

Regional Response Teams (RRTs), and 

Area Committees have sufficient 

information to support agent 

preauthorization or authorization of use 

decisions. 

DATES: Comments must be received on 

or before April 22, 2015. 

ADDRESSES: Submit your comments, 

identified by Docket ID No. EPA–HQ– 

OPA–2006–0090, by one of the 

following methods: 

• Federal Rulemaking Portal: http://

www.regulations.gov. Follow the on-line 

instructions for submitting comments. 

• Mail: The mailing address of the 

docket for this rulemaking is EPA 

Docket Center (EPA/DC), Docket ID No. 

EPA–HQ–OPA–2006–0090, 1200 

Pennsylvania Avenue NW., Washington, 

DC 20460. 

• Hand Delivery: Such deliveries are 

only accepted during the Docket’s 

normal hours of operation, and special 

arrangements should be made for 

deliveries of boxed information. 

Instructions: Direct your comments to 

Docket ID No. EPA–HQ–OPA–2006– 

0090. EPA’s policy is that all comments 

received will be included in the public 

docket without change and may be 

made available online at http:// 

www.regulations.gov, including any 

personal information provided, unless 

the comment includes information 

claimed to be Confidential Business 

Information (CBI) or other information 

whose disclosure is restricted by statute. 

Do not submit information that you 

consider to be CBI or otherwise 

protected through 

http://www.regulations.gov. The http:// 

www.regulations.gov Web site is an 

‘‘anonymous access’’ system, which 

means EPA will not know your identity 

or contact information unless you 

provide it in the body of your comment. 

If you submit an electronic comment, 

EPA recommends that you include your 

name and other contact information in 

the body of the comment and with any 

disk or CD–ROM you submit. If EPA 

cannot read your comment due to 

technical difficulties and cannot contact 

you for clarification, EPA may not be 

able to consider your comment. 

Electronic files should avoid the use of 

special characters, any form of 

encryption, and be free of any defects or 

viruses. Comments and suggestions 

regarding the scope of any future 

rulemaking should be clearly 

differentiated from comments specific to 

this proposal (e.g., label Suggestions for 

Future Rulemaking and Comments on 

Current Proposal). 

Docket: All documents in the docket 

are listed in the http://

www.regulations.gov index. Although 

listed in the index, some information is 

not publicly available, e.g., CBI or other 

information whose disclosure is 

restricted by statute. Certain other 

material, such as copyrighted material, 

will be publicly available only in hard 

copy. Publicly available docket 

materials are available either 

electronically in http:// 

www.regulations.gov or in hard copy at 

the EPA Docket, EPA/DC, EPA West, 

Room 3334, 1301 Constitution Avenue 

NW., Washington, DC. The Public 

Reading Room is open from 8:30 a.m. to 

4:30 p.m., Monday through Friday, 

excluding legal holidays. The telephone 

number for the Public Reading Room is 

202–566–1744 to make an appointment 

to view the docket. 

FOR FURTHER INFORMATION CONTACT: For 

general information, contact the 

Superfund, TRI, EPCRA, RMP, and Oil 

Information Center at 800–424–9346 or 

TDD at 800–553–7672 (hearing 

impaired). In the Washington, DC 

metropolitan area, contact the 

Superfund, TRI, EPCRA, RMP, and Oil 

Information Center at 703–412–9810 or 

TDD 703–412–3323. For more detailed 

information on this proposed rule 

contact Gregory Wilson at 202–564– 

7989 (wilson.gregory@epa.gov) or 

Vanessa Principe at 202–564–7913 

(principe.vanessa@epa.gov). The 

contacts address is: U.S. Environmental 

Protection Agency, Office of Emergency 

Management, Regulations 

Implementation Division, 1200 

Pennsylvania Avenue NW., Washington, 

DC 20460–0002, Mail Code 5104A, or 

visit the Office of Emergency 

Management Web site at http://

www.epa.gov/oem/. 

SUPPLEMENTARY INFORMATION: The 

contents of this preamble are: 

I. General Information 

II. Entities Potentially Affected by This 

Proposed Rule 

III. Statutory Authority and Delegation of 

Authority 

IV. Background 

A. Historical Background 

B. Current Statute and Regulation 

C. Advanced Response Planning 

V. This Action 

A. Discharge of Oil 

B. Subpart A—Introduction 

1. Definitions 

C. Subpart J—Use of Dispersants, and 

Other Chemical and Biological Agents 

1. General 

2. Authorization of Use 

3. Monitoring the Use of Dispersants 

4. Data and Information Requirements for 

Product Schedule Listing 

5. Submission of Confidential Business 

Information (CBI) 

6. Addition of a Product to the Schedule 

7. Mandatory Product Disclaimer 

8. Removal of a Product From the Schedule 

9. Appendix C to Part 300 

10. Appendix E to Part 300 

VI. Summary of Proposed Rule Provisions 


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VII. Statutory and Executive Order Reviews 

A. Executive Order 12866: Regulatory 

Planning and Review and Executive 

Order 13563: Improving Regulation and 

Regulatory Review 

B. Paperwork Reduction Act 

C. Regulatory Flexibility Act (RFA) 

D. Unfunded Mandates Reform Act 

E. Executive Order 13132: Federalism 

F. Executive Order 13175: Consultation 

and Coordination With Indian Tribal 

Governments 

G. Executive Order 13045: Protection of 

Children From Environmental Health 

Risks and Safety Risks 

H. Executive Order 13211: Actions That 

Significantly Affect Energy Supply, 

Distribution or Use 

I. National Technology Transfer and 

Advancement Act 

J. Executive Order 12898: Environmental 

Justice 

I. General Information 

In April 2010, the Deepwater Horizon 

underwater oil well blowout discharged 

significant quantities of oil into the Gulf 

of Mexico. The blowout discharged oil 

from one mile below the sea surface. 

Approximately one million gallons of 

dispersants over a three-month period 

were deployed on surface slicks over 

thousands of square miles of the Gulf, 

and approximately three quarters of a 

million gallons of dispersants were, for 

the first time, injected directly into the 

oil gushing from the well riser. This use 

of dispersants raised many questions 

about efficacy, toxicity, environmental 

trade-offs, and monitoring challenges 

that EPA seeks to address through the 

proposed revisions to Subpart J. 

The proposed revisions to Subpart J 

address the use of dispersants and other 

chemical and biological agents to 

respond to oil discharges into waters of 

the U.S. Over the past several years, 

EPA’s Office of Research and 

Development (ORD) has conducted 

research on improved laboratory 

protocols for dispersant and 

bioremediation efficacy, and revisions 

to Subpart J to address these new 

protocols were under consideration. As 

a result of this research and the 

Deepwater Horizon event, the new 

protocols in the proposed revisions, in 

addition to increasing the overall 

scientific soundness of the data, take 

into consideration not only the efficacy 

but also the toxicity, long-term 

environmental impacts, endangered 

species protection, and human health 

concerns raised during responses to oil 

discharges, including the Deepwater 

Horizon blowout. Additionally, area 

planning requirements for dispersant 

use authorization, toxicity thresholds 

and advanced monitoring techniques 

are also proposed. The proposed 

amendments are a major component of 

EPA’s effort to inform the use of 

dispersants and other chemical or 

biological agents when responding to oil 

discharges. They incorporate lessons 

learned from the federal government’s 

experiences in the Gulf, and address 

recommendations specific to agent 

testing and use in response to oil 

discharges from the National 

Commission on the BP Deepwater 

Horizon Oil Spill and Offshore Drilling 

Report to the President. 

The proposed amendments would 

help to ensure that only products that 

perform effectively in laboratory testing 

would be listed on the NCP Product 

Schedule (Schedule) for use in 

mitigating the effects of oil discharges in 

the environment. Manufacturers would 

be required to provide more detailed 

product application materials, 

ecological toxicity data, and human 

health and safety information, including 

more detailed instructions for product 

application in the field. Prohibitions on 

using products in certain areas under 

certain conditions determined by OnScene Coordinators (OSCs), Regional 

Response Teams (RRTs), and EPA 

would help ensure that first responders 

are better able to mitigate environmental 

effects when spills occur. The required 

submission of additional product 

toxicity information would aid OSCs 

and RRTs when evaluating specific 

product information and when deciding 

whether and which products to use to 

mitigate hazards to the environment and 

human health caused by discharges or 

threatened discharges of oil. 

Specifically in this action, the Agency 

proposes, for the following areas: 

• Definitions. Amend definitions for 

Bioremediation agents, Burning agents, 

Chemical agents, Dispersants, Sinking 

agents, Sorbents, and Surface washing 

agents; add new definitions for 

Bioaccumulation, Bioconcentration, 

Biodegradation, Biological agents, 

Bioremediation, Herding agents, 

Products, and Solidifiers; and remove 

definitions for Miscellaneous Oil Spill 

Control Agents (MOSCA) and Surface 

collecting agents. 

• General Requirements. Revise to 

reflect new and amended regulatory 

definitions. 

• Authorization of Use. Revise to 

clarify planning and preauthorization 

responsibilities, establish limitations 

and prohibitions on the use of certain 

agents, establish requirements for 

storage and use of agents, clarify 

authorities for requiring supplemental 

testing, monitoring and information on 

agents, establish requirements for agent 

recovery from the environment, and 

establish reporting requirements for 

agent use. 

• Monitoring the Use of Dispersant. 

Establish monitoring requirements for 

dispersant use in response to major 

discharges and/or certain dispersant use 

situations. 

• General Product Information for 

Schedule Listing. Revise and establish 

requirements, including designation of 

and testing for all product categories 

under which the listing is requested, 

Safety Data Sheets, sample product 

labels, shelf life, collection and 

recovery, persistence in the 

environment, storage and use 

conditions, physical and chemical 

properties, component identities, 

concentration limits on National Water 

Quality Criteria and Standards 

contaminants, laboratory accreditations, 

submission of all testing data and 

calculations, production capabilities, 

and any other data or certification 

informing the product’s performance 

capabilities or environmental benefits. 

• Dispersant Testing and Listing 

Requirements. Revise the efficacy 

testing methodology using a baffled 

flask test, establish new developmental 

and sub-chronic toxicity testing 

requirements, revise the acute toxicity 

testing methodologies, revise the listing 

criteria, and establish use limitations to 

saltwater environments. 

• Surface Washing Agent Testing and 

Listing Requirements. Revise the acute 

toxicity testing methodology and listing 

requirements, establish efficacy testing 

requirements and listing criteria, and 

establish use limitations based on 

product testing for salt and/or 

freshwater environments. 

• Bioremediation Agent Testing and 

Listing Requirements. Revise the 

efficacy and acute toxicity testing 

methodologies and listing criteria, 

establish exceptions for specified nonproprietary products, and establish use 

limitations based on product testing for 

salt and/or freshwater environments. 

• Solidifier and Herding Agent 

Testing and Listing Requirements. 

Revise the acute toxicity testing 

methodology and listing criteria, and 

establish use limitations based on 

product testing for salt and/or 

freshwater environments. 

• Sorbent Requirements. Establish a 

list of known, non-proprietary sorbents 

to be made publicly available in lieu of 

listing sorbents on the Schedule, and 

requirements for data and information 

for sorbent products with components 

other than those specifically identified 

in the rule. 

• Submissions of Confidential 

Business Information. Revise the 

allowable confidential business 

information claims and reporting 

procedures. 


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• Addition of a Product to the 

Schedule. Revise the submission 

requirements including the package 

contents, EPA’s review of submission 

package, request for review of decision, 

changes to a product listing, and 

transitioning of listed products from the 

current Schedule to the new Schedule. 

• Mandatory Product Disclaimer. 

Revise the product disclaimer 

requirements. 

• Removal of a Product from the 

Schedule. Revise the basis for removal 

and appeals process. 

• Appendix C to part 300. Revise the 

requirements for product testing 

protocols and summary test data 

including new dispersant baffled flask 

efficacy and toxicity tests; new standard 

acute toxicity tests for bioremediation 

agents, surface washing agents, herding 

agents, and solidifiers; and revised 

bioremediation agent efficacy test. 

• Appendix E to Part 300—Oil Spill 

Response. Remove this appendix from 

the NCP. 

EPA estimates industry may incur 

total incremental costs of approximately 

$668,000 to $694,000 annually. The 

benefits of the Subpart J amendments 

are assessed qualitatively. Such benefits 

include, for example, greater clarity of 

regulatory requirements, as well as less 

toxic products. This action does not 

pose significant impacts on a substantial 

number of small entities. The 

Regulatory Impact analysis, which can 

be found in the docket, provides more 

detail on the cost methodology and 

benefits of this action. 

COST OF THE PROPOSED RULE

Annualized costs, 20 years 

Annualized at 

3% 

Annualized at 

7% 

Costs ......... $667,610 $694,343 

II. Entities Potentially Affected by This 

Proposed Rule 

Industrial category NAICS code 

Chemical Manufacturing ....... 325 

Merchant Wholesalers, Nondurable Goods .................. 424 

Professional, Scientific, and 

Technical Services ............ 541 

Waste Management and Remediation Services ............ 562 

Oil and Gas Extraction ......... 211 

The list of potentially affected entities 

in the above table includes 

manufacturers and users of chemical 

and biological agents, and other oil spill 

mitigating devices and substances used 

as countermeasures against oil 

discharges. The Agency’s goal is to 

provide a guide for readers to consider 

regarding entities that potentially could 

be affected by this action. However, this 

action may affect other entities not 

listed in this table. If you have questions 

regarding the applicability of this action 

to a particular entity, consult the 

person(s) listed in the preceding section 

entitled FOR FURTHER INFORMATION

CONTACT. 

III. Statutory Authority and Delegation 

of Authority 

Under sections 311(d) and 311(j) of 

the Clean Water Act (CWA), as amended 

by section 4201 of the Oil Pollution Act 

of 1990 (OPA), Public Law 101–380, the 

President is directed to prepare and 

publish the National Oil and Hazardous 

Substances Pollution Contingency Plan 

(NCP) for removal of oil and hazardous 

substances. Specifically, section 

311(d)(2)(G) requires the President to 

include a schedule identifying 

‘‘dispersants, other chemicals, and other 

spill mitigating devices and substances, 

if any, that may be used in carrying out’’ 

the NCP. The authority of the President 

to implement this portion of the CWA 

is currently delegated to EPA in 

Executive Order 12777 (56 FR 54757, 

October 22, 1991). Subpart J of the NCP 

governs the use of dispersants, and any 

other chemical or biological agent to 

respond to oil discharges (40 CFR part 

300 series 900). 

IV. Background 

A. Historical Background 

The Council on Environmental 

Quality (CEQ) first published the 

National Oil and Hazardous Materials 

Pollution Contingency Plan in 1970 (35 

FR 8508). Among its elements was 

Annex X—Schedule of Dispersants and 

other Chemicals to Treat Oil Spills. 

Annex X provided a basic regulatory 

framework that included authorization 

of use, restrictions, and information 

requirements to be submitted to the 

Federal Water Quality Administration 

(FWQA). This initial schedule 

advocated mechanical and other control 

methods, and the removal and proper 

disposal of oil from the environment. It 

also specified that dispersants might be 

used in accordance with the schedule if 

other control methods are judged to be 

inadequate or infeasible, and if certain 

information requirements and usage 

requirements were met. As a listing 

requirement, manufacturers had to 

provide the FWQA with methods for 

analyzing the chemical components in 

fresh and salt water, or reasons why 

such analytical methods could not be 

provided. Except to prevent or 

substantially reduce the hazard to 

human life or limb, or substantial 

hazard of fire to property, dispersants 

were restricted from use on or in any: 

Distillate fuel oil; spill of oil less than 

200 barrels in quantity; shoreline; 

waters less than 100 feet deep; waters 

containing major populations or 

breeding or passage for species of fish or 

marine life which may be damaged or 

rendered commercially less marketable 

by exposure to the dispersant or 

dispersed oil; waters where the winds 

and/or currents are of such velocity and 

direction that the dispersed oil mixtures 

would likely, in the judgment of the 

FWQA, be carried to shore areas within 

24 hours; and waters where such use 

may affect surface water supplies. The 

CEQ revised the National Oil and 

Hazardous Materials Pollution 

Contingency Plan, renaming it the 

National Oil and Hazardous Substances 

Pollution Contingency Plan (NCP) in 

1971 (36 FR 16215). The NCP was 

amended again in 1971 (36 FR 18411) 

and 1972 (37 FR 28208), with no 

substantive changes to Annex X. 

As a result of the Federal Water 

Pollution Control Act (Pub. L. 92–500) 

of 1972, CEQ again revised the NCP, 

including revisions to Annex X (38 FR 

21887, August 13, 1973). The title of 

Annex X changed to the ‘‘Schedule of 

Chemicals to Remove Oil & Hazardous 

Substances Discharges.’’ While the 

Schedule still advocated mechanical 

and other control methods, and the 

removal and proper disposal of oil from 

the environment, it broadened its 

applicability to chemical agents, 

including dispersants. It also recognized 

separate authorizations of use for 

chemical agents on minor, medium and 

major discharges. In addition, the 

revised schedule required an official 

report from a recognized laboratory with 

a description of the analytical methods 

employed and results obtained in 

determining the chemical and biological 

characteristics of the chemical agent, 

but no longer required the submission of 

those analytical methods. Biological and 

burning agents were not part of the 

Schedule, which expressed caution on 

their use. 

In 1975 CEQ again revised the NCP, 

including Annex X (40 FR 6282). Annex 

X was now the ‘‘Schedule of Chemicals 

and Other Additives to Remove Oil & 

Hazardous Substances Discharges,’’ and 

it was ‘‘. . . revised and expanded to 

provide more precise and definitive 

information, concerning substances 

which may be employed to remove 

discharges.’’ Additionally, Executive 

Order 11735 (38 FR 21243, August 3, 

1973) made EPA responsible for Annex 

X. Chemical agents or any other 

substance not specifically defined in the 


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Schedule were to be considered for use 

on a case-by-case basis. The Schedule 

advocated the development and 

utilization of mechanical control 

methods to remove or mitigate oil, and 

to remove, mitigate, or neutralize 

hazardous substances discharges from 

the environment, with subsequent 

proper disposal. The Schedule intended 

that no harmful quantities of any 

substance were to be applied to waters 

to remove or mitigate the effects of oil 

or hazardous substances discharges. The 

Schedule also provided procedures for 

authorization of use for different agent 

categories, and separate regulatory 

authorization of use for dispersants or 

other chemical agents was established 

for minor, medium, and major 

discharges. Product shelf life, toxicity 

and effectiveness, and analytical 

methods needed to obtain such data 

were among the technical data 

requirements. Similar provisions were 

tailored to surface collecting agents and 

biological additives. 

In 1982, EPA amended the NCP; the 

revision included rewriting of Annex X 

as Subpart H of 40 CFR part 300 of the 

revised Plan (47 FR 31180). The Agency 

allowed OSCs to authorize the use of 

dispersants or other chemicals to treat 

discharges of oil, provided they were 

listed in the previous Annex X, with the 

following limitations: 

• Authorization applies only to 

discharges of oil, not to releases of 

hazardous substances. 

• OSCs may only authorize the use of 

dispersant or other chemicals on EPA’s 

Acceptance list, which included the 

twenty-eight products tested and found 

acceptable for their intended purpose in 

the previous Annex X. 

• State consultation provisions 

regarding the use of any dispersant or 

other chemicals in its waters required 

the OSC to obtain concurrence from the 

EPA representative to the RRT. 

The new Subpart H of 40 CFR part 

300 also provided for a case-by-case 

authorization by the EPA Administrator 

(‘‘Administrator’’) or designee of the use 

of dispersants or other chemicals not on 

EPA’s Acceptance list in treating oil 

discharges or hazardous substances 

releases. However, EPA did not include 

testing procedures or a process for 

designation of dispersants or other 

chemicals as acceptable for use. 

In 1984, EPA published amendments 

to Subpart H, including adding 

Appendix C (49 FR 29192). The 

amendments specified testing and data 

requirements for listing of dispersants, 

surface collecting agents, or biological 

additives on the Schedule to ensure 

sufficient data was available for the 

OSC. Standardized testing procedures 

generated comparable data regarding the 

products’ effectiveness and toxicity. 

Appendix C detailed the methods and 

types of apparatus to be used in carrying 

out the revised standard dispersant 

effectiveness and toxicity tests, as well 

as the format required for summary 

presentation of product test data. Listing 

of a product on the Schedule was 

neither a recommendation nor 

authorization for use on an oil 

discharge, but rather a confirmation that 

data submission requirements had been 

satisfied. EPA’s listing on the Schedule 

did not confirm its safety or 

effectiveness or constitute an 

endorsement; in fact, a new requirement 

was established that either a written 

disclaimer to this effect or EPA’s written 

disclaimer be included in all product 

technical literature or advertisements. 

Products previously listed under Annex 

X were included on the new Schedule 

as the previous data requirements were 

sufficient to permit OSCs to make 

informed decisions about product use. 

The amendments also provided for 

OSC authorization for use of burning 

agents on a case-by-case basis with the 

concurrence of the EPA RRT 

representative and the States, and 

prohibited the use of sinking agents in 

waters of the United States. They 

encouraged advance planning by 

allowing the OSC to act without the 

concurrence of the RRT and affected 

States if these parties have approved a 

plan identifying the products that may 

be used in specific contexts. The 

amendments also allowed the OSC to 

authorize the use of any product 

(including products not on the 

Schedule) without obtaining the 

concurrence of the EPA representative 

to the RRT or the affected States if the 

use of a dispersant, surface collecting 

agent, or biological additive is necessary 

to prevent or substantially reduce 

hazard to human life, and there is not 

sufficient time to obtain concurrence. 

However, the OSC was to inform the 

EPA RRT representative and the affected 

States of the use of a product as soon as 

possible, and obtain their concurrences 

for the product’s continued use in the 

situation once the threat to human life 

had subsided. These provisions were 

designed to eliminate delays in life 

threatening situations, such as spills of 

highly flammable petroleum products in 

harbors or near inhabited areas. Subpart 

H was re-designated as Subpart J with 

minor changes in 1990 (55 FR 8666), 

with those definitions present in 

Subpart H moved to Subpart A, and a 

new definition and data requirements 

for miscellaneous spill control agents 

added. 

In 1994, EPA revised the NCP in 

response to the passage of the Oil 

Pollution Act in 1990 (59 FR 47384). 

The final rule significantly revised 

Subpart J to its current regulatory 

requirements with respect to 

authorization of use, data requirements, 

dispersant effectiveness and toxicity 

testing protocols, surface washing agent 

toxicity testing protocol, bioremediation 

agent effectiveness testing protocol, and 

requirements for adding products to the 

Schedule. As a result, several 

dispersants were re-classified as surface 

washing agents because they did not 

pass the dispersant efficacy test 

threshold, but were effective in 

removing oil from solid surfaces. 

B. Current Statute and Regulation 

Section 300.910 of Subpart J 

addresses the authorization of the use of 

products on the Schedule and specifies 

the conditions under which OSCs may 

authorize the use of dispersants, other 

chemicals, and other spill mitigating 

substances. Sections 300.915 and 

300.920 describe the data requirements 

and the process for adding products to 

the Schedule. To list a product on the 

Schedule, Subpart J currently requires 

the submission of technical data on the 

product to EPA. Data on dispersants, 

surface collecting agents, surface 

washing agents, and miscellaneous oil 

spill control agents must include the 

results of the toxicity test set for these 

products in Appendix C of the NCP. 

Data on dispersants must also include 

the results of the dispersant 

effectiveness test, while bioremediation 

agents must include results of the 

bioremediation effectiveness test, also 

set forth in Appendix C. These tests are 

conducted at the expense of the product 

manufacturers and must be performed 

by laboratories experienced with 

Appendix C protocols. 

The raw data and a summary of the 

results from these tests are then 

submitted to EPA, where they are 

reviewed to confirm that the data are 

complete and that the specified 

procedures were followed. The data 

requirements for placement of a product 

on the Schedule are designed to provide 

sufficient data for the OSCs to judge 

whether and in what quantities a 

product may be used to control a 

particular discharge. Inclusion of a 

product on the Schedule means only 

that the data submission requirements 

have been satisfied. The listing of a 

product on the Schedule does not mean 

that the product is recommended or 

authorized for use on any specific oil 

discharge nor does it imply that EPA 

has in any other way endorsed the 

product for the use listed or for other 


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uses. The standardized testing 

procedures set forth in Appendix C 

provide OSCs comparable data 

regarding the toxicity, effectiveness, and 

other characteristics of different 

products. 

C. Advanced Response Planning 

Under the current 300.910(a) 

regulation, RRTs and the Area 

Committees (ACs) are required to 

address, as part of their planning 

activities, the desirability of using 

appropriate dispersants, and other 

chemical or biological agents. The RRTs 

and ACs generally develop 

‘‘preauthorization plans’’ which address 

the specific context in which products 

can be used under OSC direction. 

Preauthorization plans are approved 

with concurrences from EPA, 

Department of Interior (DOI) and 

Department of Commerce (DOC) natural 

resource trustees, and the state(s) with 

jurisdiction over the water to the area, 

which they apply. When a 

preauthorization plan approves in 

advance the use of certain products 

under specified circumstances, the OSC 

may authorize the use of the products 

without obtaining the specific 

concurrences described elsewhere in 

that section of the regulation. The use of 

chemical or biological agents is only one 

approach of many available, such as 

mechanical collection or in-situ 

burning, and decisions about their use 

should be weighed to achieve greater 

overall environmental protection. 

To facilitate the best possible 

response, it is important that the 

regional-level and area-level 

contingency planning efforts of the 

RRTs and ACs, respectively, are 

coordinated closely with each other and 

are consistent. Section 300.910(a) 

authorizes the RRTs to review and 

either approve, disapprove, or approve 

with modification the preauthorization 

plans developed by Area Committees 

that addresses dispersants or other spill 

mitigating substances. This advanced 

planning has allowed the OSC to 

authorize the use of products without 

obtaining the specific concurrences, if 

the RRT representatives from EPA and 

the states with jurisdiction over waters 

to which a preauthorization plan 

applies, and DOC and DOI natural 

resource trustees approve their use in 

advance. The OSC primarily uses the 

Schedule to confirm if a product is 

listed, analyze toxicity and efficacy 

data, note worker health and safety 

precautions, understand proper product 

application, and compare one product 

to another in order to make the most 

informed decision on how to mitigate an 

oil discharge. 

AC responsibilities include enhancing 

contingency planning; ensuring 

preplanning of joint federal, state, and 

local response efforts; and expediting 

decisions on the use of dispersants and 

other spill mitigating devices and 

substances. The Area Contingency Plan 

(ACP) must list the equipment, 

dispersants or other spill mitigating 

substances, and personnel available to 

ensure effective and immediate removal 

of a discharge. ACPs must also ensure 

the mitigation or prevention of a 

substantial threat of a discharge; provide 

a description of the procedures to be 

followed for obtaining an expedited 

decision regarding the use of 

dispersants (which may be addressed in 

applicable preauthorization plans); and 

identify the means to monitor use of 

chemical countermeasures. Many 

coastal ACPs include some type of 

preauthorization zones for dispersants, 

while most Regional Contingency Plans 

(RCPs) address other product categories, 

such as bioremediation and surface 

washing agents. RRTs, in cooperation 

with the states and federal agencies, 

have addressed the requirements for the 

conduct of in-situ burns (ISB) of oil 

discharges in their RCPs. 

This planning has allowed 

consideration of chemical agent use on 

oil discharges as a viable response tool 

in combination with other mitigation 

measures. These agents have 

increasingly been considered and used 

in the field, as evidenced by research 

and case studies presented at national 

and international oil spill conferences, 

research and development funding from 

private and government stakeholders, 

RRT efforts to plan for their use, 

requests for EPA and other federal 

experts to advise field personnel on the 

use of such products, and by the 

response to the Deepwater Horizon oil 

spill. While many research efforts have 

helped to clarify issues and added 

information on the toxicity, efficacy, 

proper use, and human health impacts 

of these response technologies, 

uncertainties still arise. The Agency has 

an interest in resolving the issues that 

arise from the use of chemical and 

biological agents in spill responses, as 

its representatives are asked to concur 

with chemical and biological agent use 

for marine and freshwater spills. 

The use of non-mechanical oil spill 

mitigating technologies, such as 

dispersants, surface washing agents, 

sorbents, solidifiers, bioremediation 

agents, and others are among the 

available oil response options that 

responders may consider in the United 

States and the world. The National 

Academies’ National Research Council 

report titled ‘‘Oil Spill Dispersants: 

Efficacy and Effects’’ (2005), 

recommends that steps be taken to 

better support policymakers and spill 

responders faced with making choices 

regarding the use of dispersants as part 

of spill contingency planning efforts or 

during actual spills. The United States 

Coast Guard has promulgated new 

requirements for certain vessels to have 

only Schedule listed dispersant 

response capabilities while operating in 

designated dispersant preauthorization 

zones (74 FR 45004, August 31, 2009). 

The proposed amendments are aimed 

at ensuring that chemical and biological 

agents have met efficacy and toxicity 

requirements, that product 

manufacturers provide important use 

and safety information, and that the 

planning and response community is 

equipped with the proper information to 

authorize and use the products in a 

judicious and effective manner. 

V. This Action 

This proposal addresses the efficacy, 

toxicity, environmental monitoring of 

dispersants, other chemical and 

biological agents, and other spill 

mitigating substances, as well as public, 

state, local, and federal officials 

concerns on their authorization and use. 

The sections below explain the 

proposed requirements and revisions, 

and EPA is requesting comments by 

section. Alternatives offered should 

include rationale and supporting 

information in order for the Agency to 

include the alternative in any final rule. 

A. Discharge of Oil 

The Agency is proposing revisions to 

harmonize 40 CFR part 110.4 with the 

definitions for chemical and biological 

agents proposed for Subpart J. The 

current language in § 110.4 is specific to 

dispersants and emulsifiers. The 

proposal replaces the terms ‘‘dispersants 

and emulsifiers’’ with the broader terms 

of ‘‘chemical agent’’ and ‘‘biological 

agent’’ as proposed to be amended in 

§ 300.5. The proposed definition for 

chemical agents includes elements, 

compounds, or mixtures designed to 

facilitate the removal of oil from a 

contaminated environment and mitigate 

any deleterious effects. The proposed 

definition for biological agents includes 

microorganisms (typically bacteria, 

fungi, or algae) or biological catalysts, 

such as enzymes, able to enhance the 

biodegradation of a contaminated 

environment. Chemical and biological 

agents would include both the 

dispersants and emulsifiers cited in 

§ 110.4. By revising 40 CFR part 110, the 

Agency is clarifying that any chemical 

or biological agent added to a discharge 

of oil with the intent to circumvent any 


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1Fingas, Mervin, (Ed) (2011), Oil Spill Science 

and Technology, Gulf Professional Publishing, pp. 

836, ISBN: 978–1–85617–943–0. 

provision of 40 CFR part 110 is 

prohibited. To further reflect the 

proposed revisions, the Agency is 

proposing to also amend the section title 

to ‘‘Chemical or biological agents.’’ EPA 

believes the proposed amendment is 

consistent with U.S. Coast Guard 

(USCG) regulations, which prohibit the 

discharge of chemicals or other 

substances into the sea that circumvent 

discharge conditions specified in their 

regulation (33 CFR 151.10(g)). EPA 

requests comment on these revisions. 

B. Subpart A—Introduction 

1. Definitions 

The Agency is proposing revisions to 

§ 300.5 that amend the definitions for 

Bioremediation agents, Burning agents, 

Chemical agents, Dispersants, Sinking 

agents, and Sorbents. The Agency 

proposes to revise the term Surface 

washing agent and amend its definition. 

Additionally, the proposal includes new 

definitions for Bioaccumulation, 

Bioconcentration, Biodegradation, 

Biological agents, Bioremediation, 

Herding agents, Products, and 

Solidifiers. Finally, the Agency is 

removing the definitions for 

Miscellaneous Oil Spill Control Agent 

(MOSCA) and Surface collecting agents. 

(a) Revised Definitions 

Bioremediation agent—The Agency is 

proposing to revise the definition of 

bioremediation agents to identify as 

such biological agents and/or nutrient 

additives. These agents would be 

deliberately introduced into a 

contaminated environment to increase 

the rate of biodegradation, which in turn 

would assist in mitigating deleterious 

effects caused by contaminants. The 

proposed definition identifies as 

bioremediation agents microorganisms 

and enzymes. It also identifies nutrient 

additives such as fertilizers containing 

bio-available forms of nitrogen, 

phosphorus, and potassium. The 

proposed definition clarifies the current 

definition and adds specific examples of 

bioremediation agents. This clarification 

will help manufacturers of products in 

identifying the type of product, and 

hence, what testing requirements they 

will need to comply with to have a 

product listed on the Schedule. 

Burning agents—The Agency 

proposes to revise the definition of 

burning agents to identify as such those 

additives that improve the 

combustibility of the materials to which 

they are applied. This could be achieved 

through either physical or chemical 

means. Burning agents include 

inorganic compounds in the form of 

gelling agents, such as aluminum soap. 

For example, the fuel used in helitorch 

systems is a mixture of powdered 

gelling agents with either gasoline, jet 

fuel, or a diesel/gas mixture, which are 

organic compounds.1 The Agency 

believes both the inorganic gelling agent 

and the organic fuel (e.g., gasoline) meet 

the burning agent definition by 

improving the combustibility of the 

materials to which they are applied 

through physical or chemical means. 

The Agency considered including 

ignition devices in the definition of 

burning agent because improving the 

combustibility of oil and igniting that 

oil could be considered one and the 

same. The intent would be to clarify the 

potential that not only substances, but 

also the devices holding those 

substances, be considered in the caseby-case authorization of use of such 

agents. The Agency rejected this 

approach since many devices either 

deliver the agent to the oil to be burned 

and do not enter the water, or are 

consumed in the burn along with the 

agent. The Agency requests comment on 

whether it should add ignition devices 

to the definition of a burning agent. 

Chemical agents—The Agency 

proposes to revise the definition of 

chemical agents to identify as such 

those elements, compounds, or mixtures 

that are designed to facilitate the 

removal of oil. These agents may be 

used to mitigate deleterious effects of 

the oil on a contaminated environment. 

The proposed definition would include 

under the chemical agent category 

burning agents, dispersants, herding 

agents, sinking agents, solidifiers, 

surface washing agents, and those 

bioremediation agents that consist of 

nutrient additives. The proposed 

language reflects the distinction the 

Agency is now making between 

chemical and biological agents, allowing 

product manufacturers to better target 

the testing requirements and OSCs to 

better inform their authorization of 

agent use in specific situations. The 

proposal also removes from the 

definition agent categories that are 

either being eliminated, prohibited or 

amended to conform to the changes, as 

discussed below. 

Dispersants—The Agency is 

proposing to revise the definition of 

dispersants to identify them as those 

agents that promote the formation of 

small droplets of oil in the water 

column by reducing the oil-water 

interfacial tension. Dispersants are 

proposed to be defined as typically 

mixtures of solvents, surfactants 

(including biosurfactants), and 

additives. The proposed definition 

specifically addresses the process 

through which these agents assist in 

mitigating the consequences of a 

discharge, clarifying for manufacturers 

which testing requirements they will be 

subject to when seeking to list a product 

on the Schedule. 

Sinking agents—The Agency is 

proposing to revise the definition of 

sinking agents to identify them as those 

substances deliberately introduced into 

an oil discharge to submerge the oil to 

the bottom of a water body. The current 

definition is ambiguous in regards to 

how much sinking below the water 

surface would qualify as a sinking agent, 

as some submersion below the surface 

but generally not to the bottom of the 

water body can also be associated with 

other agents, such as dispersants. The 

proposed definition specifies these 

agents purposely sink the oil to the 

bottom of a water body. The Agency is 

prohibiting the use of sinking agents in 

the remediation of oil discharges in 

water because of their potential for 

causing adverse effects on benthic 

organisms vital to the food chain of the 

aquatic environment. 

Sorbents—The Agency is proposing to 

revise the definition of sorbents to 

identify them as inert, insoluble 

substances that readily absorb and/or 

adsorb oil or hazardous substances. The 

proposed definition specifies that 

sorbents are not combined with or act as 

any other chemical or biological agent. 

The proposed definition also specifies 

that sorbents are generally collected and 

recovered from the environment and 

that they may be used in their natural 

bulk form, or as manufactured products 

in particulate form, sheets, rolls, 

pillows, or booms. The proposed 

definition identifies sorbents as 

substances consisting of: (1) Natural 

organic substances (e.g., feathers, cork, 

peat moss, and cellulose fibers such as 

bagasse, corncobs, and straw); (2) 

inorganic/mineral compounds (e.g., 

volcanic ash, perlite, vermiculite, 

zeolite, clay); and (3) synthetic 

compounds (e.g., polypropylene, 

polyethylene, polyurethane, polyester). 

The proposed changes simplify the 

definition by removing the definitions 

of absorption and adsorption that are 

embedded in the current definition of 

sorbents. The Agency believes this is 

appropriate given these are generally 

recognized scientific terms and the 

proposal does not distinguish sorbents 

or in any way restrict their use based on 

whether they absorb or adsorb the oil. 

The definition also adds the ‘‘natural’’ 

qualifier to organic substances, 

indicating that organic substances that 


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have been treated with other substances 

would not necessarily fall under this 

category of agents and should not 

immediately be considered a sorbent. It 

also expands on and simplifies the 

examples by removing the references to 

the type of birds that feathers could 

come from, by adding bagasse to the 

examples for natural organic substances, 

and by adding clay to the examples for 

inorganic/mineral compounds. The 

Agency requests comments on whether 

the definition is appropriate or if there 

are other materials that should also be 

included. 

Additionally, the Agency requests 

comments on particulate materials (e.g., 

clay) as sorbents. There is concern that 

particulate materials with densities 

greater than the seawater (or freshwater 

depending on where they may be used) 

have the potential to become sinking 

agents, settling to the seabed and posing 

potential risks to benthic organisms. 

This question is also relevant when 

considering emerging response 

technologies such as the use of 

particulate materials to form oil-mineral 

aggregates (OMAs) to promote 

dispersion. OMAs are stable 

microscopic entities formed when 

particulate materials interact with the 

oil droplets resulting in distinct oil and 

mineral phases. These fine mineral 

particles could be intentionally 

introduced by themselves to promote 

physical dispersion by preventing the 

oil to re-coalesce, or can also be used in 

conjunction with dispersants to enhance 

chemical dispersion. However, any 

particulate material that by itself, or 

when combined with oil (e.g., OMA), 

results in overall densities less than the 

waters where it may be used, would not 

be prohibited as a sinking agent. The 

Agency requests comment on whether 

the use of sorbent materials in 

particulate form should be specified for 

use only in booms or other contained 

manufactured products, and whether 

there should be limitations on the 

authorization of use on water for 

sorbents in loose particulate form. 

Alternatively, the Agency also requests 

comment and supporting rationale on 

other approaches, including whether 

particulate materials in loose form, or 

specifically OMA technologies, should 

be excluded from the regulatory 

definition of sorbents. 

Finally, EPA also requests comments 

on the qualifier phrase ‘‘that are 

generally collected and recovered from 

the environment.’’ For example, a 

natural organic and biodegradable 

sorbent (e.g., bagasse) may not 

necessarily need to be removed after it 

has absorbed/adsorbed the oil when 

used in a wetland or salt marsh. Such 

removal may cause more harm than the 

oil itself due to trampling in the wetland 

or salt marsh. Once the oil is brought to 

the surface by the sorbent, 

biodegradation of both the oil and the 

sorbent can take place, especially if 

nutrients are added to enhance 

biodegradation. Another example would 

be the use of OMA technology to 

promote dispersion, which might not 

lend itself to collect or remove the 

aggregates from the environment. Thus, 

the Agency is requesting comment on 

whether testing and/or authorization of 

use requirements should be considered 

for particulate materials in loose form or 

OMA technologies that may be used in 

discharge situations where they would 

not be collected and recovered from the 

environment. 

Surface washing agents—The Agency 

is proposing to revise the term surface 

washing agent and the definition for 

surface washing agents. The proposed 

definition would identify surface 

washing agents as those substances that 

separate oil from solid surfaces (e.g., 

beaches, rocks, metals, or concrete) 

through a detergency mechanism. This 

detergency mechanism would lift and 

float the oil for collection and recovery 

from the environment. The use of these 

agents results in minimal dissolution, 

dispersion, or transfer of oil into the 

water column. The proposed changes 

revise the term from singular to plural 

to be consistent with the other agent 

definitions and clarifies that these 

agents are to be recovered from the 

environment along with the oil being 

treated. 

(b) New Definitions 

The Agency is proposing to add 

several new definitions that serve as the 

foundation for the new proposed 

biological agent classification: 

Bioaccumulation, Bioconcentration, 

Biodegradation, Biological agents, and 

Bioremediation. The proposed 

definitions include basic terminology 

and are consistent with definitions of 

these terms generally understood by the 

scientific community. 

The Agency is also proposing new 

definitions for the terms herding agents 

and solidifiers. The proposed 

definitions address types of agents 

originally captured under the surface 

collecting agent or the miscellaneous oil 

spill control agent categories 

respectively, and are terms that are more 

commonly used in industry. The 

definitions more specifically describe 

the specific process through which the 

product affects the oil for the categories 

and are consistent with definitions of 

these terms generally understood by the 

scientific community. 

Finally, the Agency is proposing a 

new definition for the term product to 

clarify the difference between a specific 

product and an agent type or category. 

All of the proposed new definitions can 

be found in the § 300.5 of this action. 

(c) Removed Definitions 

The Agency is proposing to remove 

the definitions for surface collecting 

agent and for miscellaneous oil spill 

control agent (MOSCA). The surface 

collecting agent definition is being 

removed and replaced with a new 

herding agent definition to better reflect 

the common terminology used in 

industry for these agents. The MOSCA 

definition is being removed and 

replaced with a number of new and/or 

revised definitions for types of agents. 

The original MOSCA category was used 

as a catchall for all types of products 

that did not meet other agent 

definitions. As the Agency adds new, 

more stringent testing requirements for 

listing products on the Schedule, there 

is a need for more specific category 

definitions to assist manufacturers in 

determining which of those testing 

requirements apply to their products. 

The Agency believes it has identified 

categories that capture all products to be 

listed on the Schedule; we request 

comment on whether the MOSCA 

category should be retained, and 

whether the proposed categories are 

appropriate, including sufficient 

information and rationale to support the 

addition of any new categories. 

C. Subpart J—Use of Dispersants, and 

Other Chemical and Biological Agents 

1. General 

EPA is proposing to amend § 300.900 

by revising paragraphs (a) and (c), and 

by adding paragraph (d) to reserve for 

‘‘Releases of Hazardous Substances’’. 

The proposed revisions clarify that 

Subpart J addresses not only chemical 

agents, but also those agents that now 

fall under the newly proposed biological 

agent category. The revisions reaffirms 

the notion that Subpart J is not only 

comprised of a Schedule of chemical 

and biological agents, but also includes 

testing requirements and authorization 

of use procedures. Consistent with 

current Subpart J regulatory 

requirements the Agency is proposing to 

reserve a section for ‘‘Releases of 

Hazardous Substances’’ to take place of 

the current placeholder in § 300.905, 

which is proposed to be removed. Based 

on all relevant circumstances, testing 

data and information, and in accordance 

with the authorization of use procedures 

(including the appropriate concurrences 

and consultations), the waters and 


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2Tulis, Dana S., EPA Chair and Caplis, Captain 

John, USCG Vice-Chair, National Response Team, 

‘‘Use of Dispersants on Oil Spills—Interim 

Actions;’’ Memorandum to NRT Members and RRT 

Co-Chairs; December 16, 2010. 

3Stanislaus, Mathy; Assistant Administrator, 

OSWER EPA; ‘‘Revision of Area Contingency Plans/ 

Regional Contingency Plans Regarding Use of 

Dispersants on Oil Spills—Interim Actions;’’ 

Memorandum to EPA Regional Administrators, 

November 2, 2010. 

quantities in which a dispersant, or 

other chemical or biological agents may 

be safely used are to be determined in 

each case by the OSC. When taken 

together, these testing requirements, 

listing of agents and authorization of use 

procedures address the types of waters 

and the quantities of listed agents that 

may be used in response to discharges 

of oil or hazardous substances. The 

wide variability in waters, weather 

conditions, organisms living in the 

waters, and types of oil that might be 

discharged requires this approach. 

2. Authorization of Use 

Section 300.910 sets forth the 

provisions for the authorization of use 

of products on the Schedule in response 

to oil discharges. Subpart J does not 

state or imply that chemical or 

biological agents are preferred over 

other response options such as 

mechanical recovery devices. EPA 

believes that the circumstances 

surrounding oil discharges and the 

factors influencing the choice of 

response methods are many. During the 

DWH response, a priority 

countermeasures scheme was 

established to first use mechanical 

recovery via skimming/booming or insitu burning followed by subsea 

dispersant and lastly surface dispersant 

use. Following DWH, EPA and the NRT 

issued Interim Actions regarding the use 

of dispersants on oil spills to NRT 

members and RRT co-chairs 2 and to 

EPA Regional Administrators 3 for 

consideration during response planning. 

While response actions are incident 

specific, the availability of response 

methods that address the specific 

discharge situation depends largely on 

contingency planning activities and on 

how these requirements are 

implemented through the RCPs, ACPs 

and vessel and facility response plans. 

In order for a response to be effective, 

the NCP requires coordination between 

the regulatory and planning entities 

responsible for all these response plans. 

The Agency believes that 

preauthorization or expedited decision 

making plans are critical elements of 

contingency planning activities. 

Regularly reviewing or revising 

preauthorization or expedited decision 

making plans provides those agencies in 

charge of preparedness planning the 

opportunity to identify and resolve 

concerns in advance, leading to quick 

and effective operations during removal 

actions. The Agency believes these 

proposed revisions to the authorization 

of use provisions will assist OSCs, 

RRTs, and ACs in their advanced 

planning activities as they consider 

response methods that result in the 

greatest environmental protection. The 

goal is to ensure that preauthorization or 

expedited decision making plans are 

developed and maintained to effectively 

support decisions by OSCs during 

removal actions. In carrying out 

advanced planning activities, the 

Agency believes the NRT can assist 

RRTs by providing guidance on national 

level issues that may arise during 

planning activities. 

EPA is amending § 300.910 by 

revising paragraphs (a) through (f); and 

by adding paragraphs (g), (h) and (i). 

EPA is not proposing major changes to 

the current authorities granted to OSCs, 

RRT representatives to the RRTs, States, 

DOC, DOI, or other National Response 

Team decision makers with regards to 

the authorization and application of 

chemical or biological agents. However, 

EPA recognizes that the planning for 

and prolonged use and monitoring of 

chemical agents, especially dispersants, 

may require additional planning 

activities and monitoring requirements. 

Thus, the Agency is proposing to 

reorganize this section; to add titles to 

the paragraphs for ease of use; to add 

several requirements addressing the 

storage and use of agents, notification of 

agent use and recovery from the 

environment; and to revise language to 

clarify established EPA policy. The 

proposed revisions and clarifications are 

highlighted for each paragraph under 

§ 300.910. 

EPA is also confirming, consistent 

with the intent of the NCP, that use of 

chemical or biological agents in 

response to oil discharges to waters of 

the U.S. or its adjoining shorelines must 

be authorized by an OSC in accordance 

with Subpart J. The unauthorized use 

can result in violations of section 301 

and 311 of the CWA. Section 301(a) 

makes unlawful ‘‘the discharge of any 

pollutant by any person,’’ except in 

compliance with certain provisions of 

the CWA. In addition, section 311(b) 

establishes penalties for persons who 

fail or refuse to comply with any 

regulation issued under section 311(j) of 

the CWA. 

(a) Use of Agents Identified on the 

Schedule on Oil Discharges Addressed 

by a Preauthorization Plan 

The Agency is proposing revisions to 

§ 300.910(a) of Subpart J to address the 

preauthorized use of chemical and 

biological agents identified on the 

Schedule. The proposed revisions 

clarify the process for preauthorization, 

the responsibilities of all involved 

parties, and the factors to consider 

during the preauthorization process, 

including the authorization for the use 

of agents by the OSC at the time of a 

discharge. EPA is also proposing to 

reorganize paragraph (a) to provide 

greater clarity by making the regulatory 

text easier to read and follow. The 

Agency believes that the proposed 

revisions do not change its fundamental 

policies regarding roles of Federal, state 

and local representatives involved in 

planning for and responding to an oil 

discharge, but rather clarify the current 

requirements and further explain the 

responsibilities for each party. The 

Agency is also proposing added 

procedures and review requirements 

intended to ensure preauthorization 

plans are up-to-date so they are most 

effective when implemented in case of 

a discharge. 

EPA believes RRTs and ACs must 

work together in order to effectively and 

successfully manage contingency 

planning. Thus, the proposed revisions 

continue to require that, as part of their 

planning activities, RRTs and ACs 

address in the preauthorization plan 

whether the use of chemical and 

biological agents listed on the Schedule 

on certain oil discharges is appropriate. 

The Agency believes that the proposed 

revision clarifies the meaning of the 

desirability of using appropriate 

chemical or biological agents. The 

Agency is removing ‘‘. . . the 

desirability of using appropriate burning 

agents.’’ from paragraph (a) and 

addressing the use of burning agents 

under paragraph (c) to provide greater 

flexibility to OSCs for authorization of 

use. 

Under the current paragraph (a), ACs 

are responsible for developing 

preauthorization plans. ACs are also 

responsible for developing ACPs, 

providing a forum to evaluate the 

environments within a jurisdiction and 

establishing protection priorities. The 

information gathered during the ACP 

development process should inform the 

development of preauthorization plans. 

Identified representatives from the RRTs 

are responsible for approving or 

requesting modifications of 

preauthorization plans developed by the 

ACs. ACs can advocate for local 


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concerns to be reflected in the 

preauthorization plans they develop, 

and the RRTs will decide if the plans 

are adequate and address region-wide 

and cross-regional issues. Since the 

RRTs should be in a position to provide 

guidance to ACs on common attributes 

within a region, EPA continues to 

believe RRTs and ACs should work 

together to develop preauthorization 

plans, particularly when identifying 

discharge situations where chemical or 

biological agents may be used. There 

may be circumstances where it is 

appropriate to allow either the RRTs 

and/or ACs to develop preauthorization 

plans. Preauthorization plans developed 

by an RRT would allow for these plans 

to better reflect overarching regional 

circumstances. Therefore, the Agency is 

proposing to include RRTs as another 

planning entity with responsibility for 

developing preauthorization plans, and 

is requesting comment on this change, 

and on the advantages or disadvantages 

of keeping the development of these 

plans at the AC level. 

ACPs generally describe discharge 

situations for the geographical area for 

which they apply. Discharge situations 

developed as part of area contingency 

planning activities may consider likely 

scenarios from vessels, and onshore or 

offshore facilities. While RRTs and ACs 

should consider the discharge scenarios 

described in ACPs when identifying 

discharge situations in developing 

preauthorization plans, the Agency 

believes they should also have the 

flexibility to consider other discharge 

scenarios. The proposed language states 

preauthorization plans must specify 

limits for the quantities and duration of 

use, and use parameters for water depth, 

distance to shoreline, and proximity to 

populated areas for discharge situations 

identified in which agents may be used. 

The Agency believes that clearly stating 

the use parameters in a preauthorization 

plan will make it easier for planners to 

address concerns of preauthorizing 

agent use and in turn for responders to 

authorize their use. 

In meeting these provisions, the 

preauthorization plans should 

document how both regional and 

logistical factors were addressed when 

establishing dispersant use limits and 

parameters. Regional factors include the 

likely sources and types of oil that 

might be discharged, various discharge 

scenarios, and the existence and 

location of environmentally sensitive 

resources or restricted areas that might 

be impacted by discharged oil. 

Logistical factors include inventory, 

storage locations and manufacturing 

capability of available agents, 

availability of equipment needed for 

agent use, availability of adequately 

trained operators, and the availability of 

appropriate means to monitor agent use. 

While the proposed revisions simplify 

the language and clarify the 

requirements, the Agency believes it is 

necessary to keep in place the 

fundamental elements that should be 

considered. The proposed factors 

generally parallel those under the 

current 300.910(a) regulation. Several 

revisions include identifying some 

factors as ‘‘regional’’ and others 

‘‘logistical.’’ The Agency is identifying 

‘‘logistical’’ factors to ensure the 

availability of chemical and biological 

agents to address discharge situations 

identified in the preauthorization plan. 

The Agency added ‘‘various discharge 

scenarios’’ as a regional factor to be 

considered because preauthorization 

plans may cover more than one ACP 

with multiple discharge scenarios that 

RRTs and/or ACs may want to consider. 

The Agency also added the existence 

and location of ‘‘restricted areas’’ along 

with ‘‘environmentally sensitive 

resources’’ as a factor to consider. 

Environmentally sensitive resources 

would include fish, wildlife and their 

habitats, and other special areas of 

ecological sensitivity that may be 

adversely affected by a discharge. While 

‘‘restricted areas’’ may include 

‘‘environmentally sensitive resources’’ 

some areas may be restricted from 

certain activities because of biologically 

sensitive topographic features or critical 

habitats, such as submerged rock 

formations colonized by species (e.g., 

coral) and the organisms they interact 

with and support. NOAA’s 

Environmental Sensitivity Index maps, 

the Fish and Wildlife and Sensitive 

(FWS) Environments Plan in ACPs, or 

environmental impact statements, may 

contain relevant information on 

‘‘environmentally sensitive resources’’ 

for the RRTs and ACs to consider. 

The proposal revises the phrase 

‘‘potential sources and types of oil that 

might be spilled’’ to ‘‘likely sources and 

types of oil that might be discharged.’’ 

EPA believes the phrase ‘‘likely sources 

and types of oil’’ better focuses on the 

sources and types of oil specific to the 

preauthorization plan for which agents 

may be used. In addition, the proposal 

revises ‘‘spill’’ to ‘‘discharge’’ to be 

consistent with terminology in the NCP. 

The proposal also revises the phrase 

‘‘the available means to monitor product 

application and effectiveness’’ to 

‘‘means to monitor agent use in the 

environment’’ as the Agency believes it 

provides for additional flexibility for the 

RRTs and/or the ACs to consider the 

scope of the monitoring, and to include 

other endpoints beyond product 

application and effectiveness. The 

Agency is proposing to eliminate the 

‘‘available’’ qualifier, as it believes it is 

unnecessary. Likewise, the Agency 

proposes to eliminate the ‘‘available’’ 

qualifier before ‘‘product and storage 

locations’’ and revise the phrase 

‘‘product and storage location’’ to the 

broader ‘‘inventory, storage locations 

and manufacturing capability of 

available agents’’ to address lessons 

learned from the Deepwater Horizon 

incident, including the challenges posed 

by the potential sustained use of 

dispersants. 

When developing preauthorization 

plans, RRTs and ACs should use the 

best available scientific information to 

assess environmental trade-offs, 

including those identified by 

conducting an ecological risk 

assessment. Environmental trade-offs 

should be considered in determining 

response options that provide the 

greatest environmental protection. The 

RRTs and ACs should identify the 

affected biological resources and their 

habitats likely to be negatively 

impacted, as well as those that are 

expected to benefit. The natural 

resource trustees are critical partners 

that can assist in conducting these 

analyses. 

As previously stated, all members of 

the RRT are afforded an opportunity to 

review and provide input on a draft 

preauthorization plan. However, only 

the RRT representatives from EPA and 

the state(s) with jurisdiction over the 

waters and adjoining shorelines within 

the preauthorization plan area and the 

DOC and DOI natural resource trustees 

may approve, disapprove, or approve 

with modification the draft 

preauthorization plan. The Agency 

believes this remains the correct 

approach. Given preauthorization plans 

are developed during the contingency 

planning phase, the Agency believes 

that DOC and DOI natural resource 

trustee concurrence is preferred over 

just consultation because it provides for 

sufficient time to identify and resolve 

natural resource concerns. As noted in 

the 1994 NCP final rule, the requirement 

for concurrence during the advanced 

planning phase ensures trustee 

involvement in decision-making (59 FR 

47398). Addressing in advance concerns 

that might otherwise slow the action 

ensures that operations during a 

removal action can be carried out 

quickly and effectively. EPA believes 

natural resource trustee concurrence 

with preauthorization plans satisfies the 

consultation obligation since the 

preauthorization plans specify the use 

parameters for chemical or biological 


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agents. Thus, the Agency is retaining 

this concurrence requirement for 

preauthorization plans. 

The Agency is proposing to revise the 

‘‘Approved preauthorization plans shall 

be included in the appropriate RCPs and 

ACPs’’ in the current § 300.910(a) 

regulation to ‘‘RRTs and ACs shall, as 

appropriate, include applicable 

approved preauthorization plans in 

RCPs and ACPs.’’ The Agency is 

proposing to modify the qualifier 

‘‘approved’’ with ‘‘applicable’’ to clarify 

that RRTs and ACs need to include the 

preauthorization plans only in those 

RCPs and ACPs to which they apply, 

and remains consistent with current 

requirements. 

The Agency considered adding 

specifically the EPA Administrator and 

the senior EPA representative to the 

NRT (e.g. NRT Chair) to § 300.910(a) 

and other paragraphs to make clear the 

EPA Administrator’s and senior EPA 

NRT representative’s existing authority 

under section 311(d)(2)(G) of FWPCA 

and Executive Order 12777, along with 

the OSC to authorize any chemical or 

biological agent use. The Agency is 

clarifying that if the preauthorization 

plan is approved in advance for 

chemical or biological agent use under 

specified discharge circumstances, then 

the OSC may authorize the use of the 

agents on the Schedule for their 

intended purpose without the incident 

specific concurrences and consultations 

described in paragraphs (b) of this 

section unless otherwise directed by the 

Administrator in accordance with 

current concurrence authority. The 

Agency believes this clarification would 

not impede rapid decision-making on 

the part of the OSC, and that for the 

majority of discharge situations, the 

OSC will remain as the sole authorizing 

entity for discharge situations covered 

by preauthorization plans. Note that in 

situations like a spill of national 

significance (SONS) or an event of 

extended duration, the Administrator 

already has the authority for, and is 

likely to have a more direct role in 

chemical or biological agent use 

decisions. The authority, jurisdiction, 

and implementation provisions in the 

NCP flow from section 311 of the Clean 

Water Act and are reflected in Executive 

Order 12777. All authorities under CWA 

311 are delegated either directly to the 

Administrator by Congress, or by 

Executive Order 12777 from the 

President to the Administrator. While 

the Administrator’s authority may be 

further delegated through senior 

management on down to the RRT 

representative, the Administrator (and 

other delegatees) retain the authority to 

act. The mere delegation of authority 

does not prohibit the delegator from 

exercising said authority. However, 

given these situations are rare and that 

this is an existing authority, the Agency 

is not proposing a regulatory 

amendment to clarify the 

Administrator’s authority at this time. 

We request comment on this issue. 

The Agency is clarifying that 

chemical or biological agents may only 

be used for their intended use, given the 

different listing requirements proposed 

for the various categories of chemical or 

biological agents. For example, a 

chemical agent that is listed on the 

Schedule solely as a surface washing 

agent cannot be authorized for use as a 

dispersant, nor can a chemical agent 

that is listed on the Schedule solely as 

a dispersant for use under saltwater 

conditions be used in freshwater. 

The Agency is proposing specific 

procedures for concurrence 

withdrawals, allowing agencies to do so 

if they believe the preauthorization plan 

no longer addresses or reflects existing 

situations if it were to be implemented. 

While an agency with concurrence 

authority may now decide to withdraw 

concurrence from an approved 

preauthorization plan, there are 

currently no set procedures to promptly 

address those situations. The proposal 

would require the RRT and the ACs to 

address the withdrawal of approval of 

the preauthorization plan within 30 

days of the withdrawal, allowing an 

opportunity to address the concerns. 

The proposal also calls for the RRT to 

notify the NRT of the final status of the 

preauthorization plan within 30 days 

from the withdrawal. The Agency 

requests comments on whether this 30 

day notification requirement should 

also include notification to the public. 

In the event of an Agency withdrawing 

its concurrence from an approved 

preauthorization plan, EPA believes the 

advanced planning process should 

continue with consideration for all the 

elements specified in paragraph (a) of 

this section. While the absence of a 

preauthorization plan requires that 

authorizations for agent use be 

conducted according to paragraph (b) of 

this section, the Agency continues to 

believe that preauthorization plans 

serve as a valuable advanced planning 

tool that provides a strong foundation to 

support decision-making and strongly 

encourages the resolution of any 

withdrawal. 

Finally, EPA proposes a new 

requirement for RRTs and/or ACs to 

review, and revise as needed, 

preauthorization plans: (a) At least 

every 5 years to address revisions of the 

Schedule; (b) after a major discharge or 

a spill of national significance (SONS); 

(c) to reflect new listings of threatened 

and/or endangered species or; (d) after 

any other change such as a new or 

revised worst case discharge estimate 

that may impact the conditions under 

which the use of chemical and 

biological agents is preauthorized. A 5- 

year review cycle is consistent with 

facility response planning requirements; 

as those plans are revised and updated, 

it seems reasonable that 

preauthorization plans should be 

reviewed and revised accordingly. The 

Agency recognizes that development of 

preauthorization plans can be resource 

intensive; however, once developed, a 

periodic review and revision as needed 

should require much less effort. EPA 

welcomes comment on this timeframe 

and suggestions with supporting 

information for alternatives. 

This review requirement is intended 

to ensure that preauthorization plans are 

actively maintained and updated to 

reflect revisions to the Schedule. 

Preauthorization plans, as well as the 

facility and vessel response plans 

reflected in them, may include 

information on products listed on the 

Schedule. A review at least every 5 

years is expected to provide greater 

consistency not only between any 

Schedule revisions, but also between 

any ACPs, facility, and vessel response 

plans. For example, an ACP revision 

that results in a change in the worst-case 

discharge scenario could trigger a 

preauthorization plan review. 

Additionally, the requirement 

specifically includes plan review and 

revision requirements as appropriate to 

reflect new listings of threatened and/or 

endangered species that may occur. The 

EPA RRT representative, the DOC and 

DOI natural resource trustees, and, as 

appropriate, the RRT representative 

from the state(s) with jurisdiction over 

the waters of the area to which a 

preauthorization plan applies must 

review and either approve, approve 

with modification, or disapprove any 

revisions to the preauthorization plans. 

This review and approval is intended to 

focus on any revisions, and is not 

intended as a requirement for review 

and approval for those portions that do 

not require modifications. 

(b) Use of Agents Identified on the 

Schedule on Oil Discharges Not 

Addressed by a Preauthorization Plan 

The Agency is proposing revisions to 

§ 300.910(b) of Subpart J to address use 

of chemical or biological agents 

identified on the Schedule for discharge 

situations that have not been addressed 

in preauthorization plans. The proposed 

revisions clarify the authorities and 

responsibilities of all involved parties, 


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3390 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

4http://www.epaosc.org/sites/5083/files/rrt6_

nearshore_dispersant_eap_031605.pdf. 

5http://www.restorethegulf.gov/release/2011/08/

19/operations-and-ongoing-response-august-17- 

2011. 

and the factors to consider when 

authorizing the use of listed chemical or 

biological agents in these situations. The 

Agency believes the proposed revisions 

do not change its fundamental policies 

regarding the roles of Federal, state and 

local representatives involved in an oil 

discharge response. 

The proposed revisions maintain, 

with the appropriate concurrences and 

consultations, the OSC’s authority to 

authorize the use of chemical or 

biological agents on the oil discharge, 

provided that the agents are listed on 

the NCP Product Schedule. The 

concurrence of the EPA representative 

to the RRT and, as appropriate, the 

concurrence of the RRT representatives 

from the states with jurisdiction over 

the waters and adjoining shorelines 

threatened by the release or discharge is 

maintained. The requirement for 

consultation with the DOC and DOI 

natural resource trustees is also 

maintained. However, the language is 

amended by removing ‘‘when 

practicable’’ with respect to 

consultation with the DOC and DOI 

natural resource trustees. The Agency 

believes that the case-by-case decision 

making should include consultations 

with natural resource trustees since 

these discharge situations may present 

unique challenges when selecting a 

response option that involves chemical 

or biological agents. While the Agency 

recognizes the time-critical nature of 

decision making during a response, 

advances in communication technology 

(e.g., smart phones, email) provide OSCs 

with increased capabilities to 

communicate quickly. Therefore, the 

Agency believes it is reasonable to 

expect an OSC to be able to notify and 

explain the circumstances requiring use 

of the certain agents to natural resource 

trustees in a timely manner. Of note, 

while consultation with the trustees on 

removal actions as required by OPA 

does not equate to a concurrence 

requirement, the Agency believes that 

such concurrence is highly desirable. 

The Agency is also proposing to revise 

the term ‘‘navigable waters threatened’’ 

to ‘‘waters and adjoining shorelines 

threatened’’ to be consistent with the 

provisions in paragraph (a) of this 

section. 

The preauthorization plan 

requirements in paragraph (a) proposes 

to remove the term ‘‘specific context’’ 

currently used and instead clearly 

establish what the term refers to. The 

proposal specifically identifies the 

parameters that must be considered by 

the OSC for authorizing agent use. 

Similar requirements are proposed 

under paragraph (b). Thus, in meeting 

the provisions of § 300.910(b), the OSC 

must consider and document the 

parameters for the use of agents 

including, but not limited to, quantities 

to be used, the duration of use, the 

depth of water, the distance to shoreline 

and proximity to populated areas, and 

should address factors such as 

environmentally sensitive resources or 

restricted areas that might be impacted, 

agent inventory and storage locations, 

agent manufacturing capability, 

availability of equipment needed for 

agent use, availability of adequately 

trained operators and appropriate means 

to monitor agent use in the 

environment. These considerations are 

parallel to those proposed under 

paragraph (a) for preauthorization and 

planning purposes. While the Agency is 

not including other factors that may 

inform preauthorization planning 

development, such as various discharge 

scenarios, this does not mean these 

factors cannot or should not be 

considered if RRTs and/or ACs choose 

to develop expedited decision making 

plans. The Agency believes these are 

fundamental elements that would 

inform an assessment of the overall 

ecological risks for the OSC to consider 

when authorizing the use of chemical or 

biological agents. 

Finally, while not required, EPA 

strongly recommends advanced 

planning for expedited decision making 

for cases where the discharge situation 

is not addressed in the preauthorization 

plans. Some RRTs have developed 

expedited approval guidelines that are 

not part of the preauthorization plans, 

but that offer an opportunity for 

advanced contingency planning by 

gathering information on the key 

parameters discussed above. Because 

discharge situations not covered by 

preauthorization plans need incident 

specific (i.e., case-by-case) authorization 

concurrence,4 expedited approval 

guidelines can be used to support 

expedited incident specific 

authorizations. For chemical or 

biological agents listed on the Schedule 

that are not authorized for use under a 

preauthorization plan, the ACs and 

RRTs should work together to outline 

the process for expedited authorization 

decisions regarding their use. It is 

important to note that while the NCP 

requires that the ACPs include 

procedures for expedited decisions, 

these procedures can include 

disapproving the use of agents, or 

approving the use of agents with certain 

operational conditions. For example, 

areas may be designated in which the 

use of certain agents or other discharge 

mitigating devices is prohibited, 

situations where limits are placed on 

the quantities of agents used, or 

situations that require certain 

monitoring requirements be in place. 

(c) Burning Agents 

The Agency is proposing to replace 

the current authorization of use for 

burning agents in § 300.910(c) with a 

provision that provides greater 

flexibility to OSCs for authorizing the 

use of burning agents. Specifically, the 

Agency proposes that OSCs may 

authorize the use of burning agents for 

authorized in-situ burns. The proposed 

amendments recognize that relatively 

small quantities of burning agents are 

ignited prior to or immediately after 

they are introduced to an oil discharge. 

Furthermore, they are composed of 

substances that are expected to rapidly 

burn off during use, which serves to 

remove them from the water. The 

Agency also recognizes that ISB has 

become an important response option 

that is used more frequently and the 

proposed revisions would allow OSCs 

to authorize the use of burning agents 

for authorized burns. For example, a 

significant number of ISBs were 

conducted during the Deepwater 

Horizon oil spill,5 and ISBs appear to be 

gaining a more prominent role as a 

response option in federal waters in 

remote locations, such as the Arctic. 

Therefore the Agency believes the 

proposed revisions better address OSC 

authorities for these situations, without 

compromising environmental concerns. 

Further, because of the nature of 

burning agents and the proposed 

revisions to the authorization of use for 

these products, the Agency continues to 

believe it is not necessary to require 

product submissions for burning agents. 

Thus, the proposal removes the 

provisions for burning agents under the 

current data requirements. The Agency 

requests comments on this approach. 

(d) Exceptions 

The proposed rule maintains the 

provision allowing OSCs to authorize 

the use of any agent, including products 

not on the Schedule, when it is 

determined that the use of the agent is 

necessary to prevent or substantially 

reduce a threat to human life. The 

proposed revisions do not change 

previous policy, but rather clarify the 

intent of the exception. The Agency 

believes that the protection of human 

life is the primary consideration in 

responding to an oil discharge. LifeVerDate Sep<11>2014 19:42 Jan 21, 2015 Jkt 235001 PO 00000 Frm 00012 Fmt 4701 Sfmt 4702 E:\FR\FM\22JAP3.SGM 22JAP3

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6For more information, refer to http://

www.epa.gov/oppt/existingchemicals/pubs/

actionplans/np-npe.html. 

7For more background information on endocrine 

disrupting compounds and their human health and 

environmental effects, please see http://

www.epa.gov/endo/pubs/edspoverview/index.htm. 

threatening oil discharges (e.g., spills of 

highly flammable petroleum products in 

harbors or near inhabited areas) may 

occur at locations where chemical 

agents on the Schedule are not 

immediately available. The Agency 

believes that in such cases, an OSC must 

have the ability to use agents that, in his 

professional judgment, would 

effectively and expeditiously mitigate 

the threat to human life. Allowing this 

authorization to occur without the 

required concurrences for 

preauthorization or authorization of use 

for products on the Schedule under 

paragraphs (a) and (b) respectively, 

eliminates delays in responding to 

potentially life-threatening situations. 

The Agency is proposing to include 

‘‘without obtaining the immediate 

concurrence’’ to clarify the scope of the 

exception. The proposed revisions are 

consistent with the intent of the current 

regulation which recognizes that once 

the threat to human life has subsided, 

the continued use of a product shall be 

in accordance with authorization of use 

paragraphs (a) and (b) of the section. In 

addition, this exception is intended for 

those extraordinary situations in which 

time is of the essence to mitigate the 

threat to human life; revising the 

language to replace ‘‘hazard’’ with 

‘‘threat’’ clearly establishes this. The 

Agency emphasizes this authority is not 

intended to circumvent the 

authorization of use provisions in 

paragraphs (a) and (b) of this section, 

which serve to address all other 

situations. 

The proposed revisions also specify 

that the OSC immediately notify, and 

document the reasons for the use of an 

agent to the EPA RRT representative and 

the affected states as soon as possible, 

and must obtain their concurrences 

where continued use of chemical or 

biological agents extends beyond 48 

hours. The Agency believes that 

advances in communication 

technologies (e.g., smart phones, email) 

provide OSCs the increased capabilities 

to communicate quickly. Therefore, it is 

reasonable to expect that the OSC notify 

and explain the circumstances requiring 

use of the agent to the designated EPA 

RRT representative and, as appropriate, 

the RRT representatives from the 

affected states and the DOC/DOI natural 

resources trustees within 48 hours. The 

Agency is requesting comments on these 

revisions, and specifically on the 48 

hour timeframe within which the OSC 

shall be operating in accordance with 

authorization of use paragraphs (a) and 

(b) of the section. 

(e) Prohibited Agents 

The Agency is maintaining the 

current prohibition for the authorization 

of use of sinking agents, and is 

clarifying that this prohibition also 

applies to any other chemical agent, 

biological agent, or any substance that 

acts as a sinking agent when mixed with 

oil. While certain chemical and 

biological agents may submerge oil 

below the water surface (e.g. dispersants 

are designed to break up oil into small, 

near neutrally buoyant particles that are 

entrained in the water column between 

the surface and the bottom), they would 

not be considered ‘‘sinking agents’’ for 

purposes of the proposed definition and 

this prohibition, given that they do not 

completely submerge oil to the bottom 

of the water body when applied to an oil 

discharge. Sinking agents, when applied 

to oil discharges, function by sinking 

floating oil to the bottom of any body of 

water where used, potentially causing 

adverse effects on benthic organisms 

vital to the food chain of the aquatic 

environment. Additionally, the oil and 

these agents are very difficult to remove. 

The Agency has similar concerns 

regarding substances that could directly 

cause the oil to submerge to the bottom 

of the water body when used in an oil 

spill response, and thus it is specifically 

proposing to exclude their use. 

The Agency is also proposing to add 

a prohibition from listing on the 

Schedule and from authorizing use of 

any chemical or biological agents that 

contain nonylphenol (NP) or 

nonylphenol ethoxylates (NPEs) as 

components. This prohibition reflects 

the Agency’s concern for these 

substances, as presented in the EPA 

Nonylphenol and Nonylphenol 

Ethoxylates Action Plan, released 

August 18, 2010. The Action Plan 

specifically addresses nonylphenol (NP) 

and nonylphenol ethoxylates (NPEs). 

NP and NPEs are produced in large 

volumes, with uses that currently lead 

to widespread release to the aquatic 

environment. NP is persistent in the 

aquatic environment, moderately 

bioaccumulative, and extremely toxic to 

aquatic organisms. NP’s main use is in 

the manufacture of NPEs. NPEs are 

nonionic surfactants that are used in a 

wide variety of industrial applications 

and consumer products. Many of these, 

such as laundry detergents, are ‘‘downthe-drain’’ applications. Some others, 

such as dust-control agents and deicers, 

lead to direct release to the 

environment. NPEs, though less toxic 

and persistent than NP, are also highly 

toxic to aquatic organisms, and, in the 

environment, degrade into NP. Both NP 

and NPEs have been found in 

environmental samples taken from 

freshwater, saltwater, groundwater, 

sediment, soil and aquatic biota. NP has 

also been detected in human breast 

milk, blood, and urine and is associated 

with reproductive and developmental 

effects in rodents. EPA has encouraged 

the ongoing voluntary phase-out of 

NPEs in industrial laundry detergents, 

and intends to evaluate how releases 

and exposures are mitigated through the 

phase-out action prior to taking any 

final regulatory action under the Toxic 

Substances Control Act.6 The Agency 

believes this prohibition would not 

adversely affect product manufacturers 

given there are viable alternatives to the 

use of NP and NPEs in product 

formulations. However, we are 

requesting comment on the potential 

impacts of modifying existing products 

to meet this new requirement, including 

cost. 

Alternatively, EPA considered a 

broader prohibition from listing and 

from authorizing the use of chemical or 

biological agents formulated with any 

endocrine disrupting compounds (EDC). 

EDCs impact exposed organisms by 

altering the hormonal and homeostatic 

systems that allow them to interact with 

and respond to their environment. The 

group of molecules identified as 

potential endocrine disruptors is highly 

varied and may be present in chemicals 

used as industrial solvents or 

surfactants that can be found in 

dispersants and surface washing agents. 

Because of the common properties of 

these compounds and the similarities of 

the receptors and enzymes involved in 

the synthesis, release, and degradation 

of hormones, no endocrine system is 

immune to endocrine disrupting 

compounds.7

The 1996 Food Quality Protection Act 

directed EPA to develop a screening 

program, using appropriate validated 

test systems and other scientifically 

relevant information, to determine 

whether certain substances may have 

hormonal effects in humans; the 1996 

amendments to the Safe Drinking Water 

Act authorized EPA to screen 

substances that may be found in sources 

of drinking water for endocrine 

disruption potential. In response to 

these mandates, the Agency’s Endocrine 

Disruptor Screening Program is 

developing requirements for the 

screening and testing of pesticides, 

commercial chemicals, and 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
3392 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

8http://www.epa.gov/endo/pubs/edspoverview/

background.htm. 

9http://www.epa.gov/endo/pubs/assayvalidation/

index.htm. 

10Responsible party is defined in the NCP under 

40 CFR 300.5. 

environmental contaminants for their 

potential to disrupt the endocrine 

system.8 The science related to 

measuring and demonstrating endocrine 

disruption is relatively new and 

validated testing methods are still being 

developed. When complete, EPA will 

use these validated methods or assays to 

identify and characterize the endocrine 

activity of pesticides, commercial 

chemicals, and environmental 

contaminants, specifically in relation to 

estrogen, androgen, and thyroid 

hormones. EPA plans to use the assays 

in a two-tiered screening and testing 

process: Tier 1 will serve to identify 

chemicals that have the potential to 

interact with the endocrine system; and 

Tier 2 will determine the endocrinerelated effects caused by each chemical 

and obtain information about effects at 

various doses. With this two-tiered 

approach, the Agency will gather 

information needed to identify 

endocrine-active substances and take 

appropriate action, as mandated by 

Congress. To date, EPA has developed 

and validated 11 assays that comprise 

the Tier 1 Screening Battery. EPA’s 

validation effort continues with the 

current focus on Tier 2 tests and 

potential replacement assays for Tier 1.9

When all tests are finalized and 

chemical information begins to be 

collected, EPA may further consider 

how to incorporate that information into 

the Subpart J NCP requirements, 

including additional testing and listing 

requirements. Because validated testing 

methods are still being developed, the 

agency is not proposing any test 

requirements with respect to endocrine 

disruption for products to be listed on 

the Schedule. 

However, because NP and the NPE are 

extremely or highly toxic to aquatic 

organisms, the Agency is proposing a 

prohibition specific to Subpart J 

products containing NP and NPE as 

components. The Agency is not 

proposing to include a broad 

prohibition on Subpart J products that 

contain substances in which at least part 

of the toxic mode of action may include 

disruption of the organism’s endocrine 

system, but is requesting comments on 

prohibiting similar substances that may 

be found in products/agents that could 

be listed on the Schedule, or to what the 

criteria should be in order to make that 

determination. As an alternative, the 

Agency could require that all product 

components be tested for a toxic mode 

of action that includes disruption of the 

organism’s endocrine system and is 

requesting comment on this approach as 

well. 

The Agency believes the proposed 

prohibitions are appropriate in all cases, 

notwithstanding the proposed 

provisions for case-by-case use 

authorization of burning agents under 

§ 300.910(c), or for authorization of use 

of any chemical or biological agent 

when it is necessary to prevent or 

substantially reduce an immediate 

threat to human life under § 300.910(d). 

There are chemical and biological agent 

alternatives to sinking agents and to 

agents containing NP or NPE, as well as 

mechanical methods for responding to 

oil discharges, including those 

situations that pose extreme threats or 

are time critical. 

(f) Storage and Use of Agents 

Section 300.915 currently requires 

that information be provided on 

recommended conditions of storage and 

use for each product at the time an 

application for listing a product under 

Subpart J is submitted to the Agency. 

This information is summarized in 

EPA’s NCP Product Schedule Technical 

Notebook. Specifically, this information 

includes: Special handling and worker 

precautions for storage and field 

application; maximum and minimum 

storage temperatures (optimum ranges 

and temperatures that will cause phase 

separations, chemical changes, or other 

alterations to product efficacy); shelf life 

of the product; recommended 

application rates and procedures, 

concentrations and conditions 

(considering water temperatures, 

salinity, types and ages of the oil); and 

any other application restrictions. 

The Agency proposes to add a new 

paragraph (f) to this section that 

complements the existing information 

requirements for the person or entity 

submitting a product for listing 

(‘‘submitter’’). The proposed 

requirements focus on the use of this 

information by the responder and the 

OSC. Specifically, the revised 

provisions require the OSC to only 

authorize for use those products that are 

stored under the conditions specified by 

the submitter of the product for listing, 

including the maximum, minimum and 

optimum temperatures, humidity and 

any other relevant conditions. 

Additionally, the Agency proposes to 

require that the OSC only authorize for 

use those products whose date of use 

does not exceed the expiration date 

listed on the container’s label at the 

time of an incident, unless the 

responsible party 10 provides the OSC 

documentation, developed in 

consultation with the submitter of the 

product for listing, prior to product use, 

affirming the product has maintained its 

integrity, including no changes in the 

composition, storage conditions, 

efficacy, and toxicity of any product. In 

such cases where the product expiration 

date has passed but the owner or 

operator of the facility/vessel storing the 

product still wants to be able to use the 

product inventory, EPA proposes that 

samples of the expired product lot 

representative of all storage conditions 

at any end user location be tested 

following the applicable testing 

protocols in Appendix C. The testing 

documentation is to include laboratory 

information (i.e., contacts, 

accreditations) and all test data and 

calculations (i.e., raw data and 

replicates, notes and observations, 

calculated means and standard 

deviations, stock solution preparations, 

source and preparations of test 

organisms, test conditions, chain of 

custody forms, and summary reports). 

Only if the owner or operator can 

demonstrate that the product has 

maintained its integrity is the OSC 

allowed to authorize the use of that 

product inventory. The owner or 

operator of the facility/vessel, or their 

representative, must re-label the tested 

product lots and maintain 

documentation of the test results until 

those lots are used or discarded, and 

must retest the expired product lot 

representative of the product at least 

once every 5 years to ensure efficacy 

and to allow an OSC to authorize the 

product for use. The intent of these 

proposed revisions is to ensure that 

products being authorized and used 

have maintained their efficacy, even 

though storage beyond the products’ 

original shelf life may have occurred. 

The Agency believes it is the owner or 

operator’s responsibility to ensure that 

any product it stockpiles for future use 

has maintained its efficacy and has not 

changed from its listed composition, 

including the possibility of degrading 

into more toxic byproducts, once the 

manufacturer’s expiration date has 

passed. This retesting provision is 

supported by the proposed requirements 

that the submitter of the product for 

listing provide not only the 

recommended storage conditions, but 

the anticipated shelf life of a product at 

those conditions, and that the product 

label include both the manufacture and 

expiration dates, and conditions for 

storage. The flexibility in this proposed 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 3393 

revision allows for the use of available 

product inventory that may still be 

viable. To alleviate concerns that 

applications are submitted that establish 

an extended or indefinite shelf life for 

a product, the Agency is requesting 

comments on whether any additional 

data or information requirements should 

be included for product listing 

determinations specific to a product’s 

shelf life, or whether alternative 

approaches, such as limiting the shelf 

life for product categories to a given 

timeframe, should be considered. 

(g) Supplemental Testing, Monitoring, 

and Information 

This proposal maintains RRT 

authority in that they may require 

supplementary toxicity and efficacy 

testing, or available data or information 

that addresses site, area, or ecosystem 

specific concerns relative to the use of 

a product for both planning and 

authorization of use. While parallel to 

the current provisions, the proposed 

revisions provide added flexibility. The 

current provisions allow RRTs to 

require supplementary toxicity and 

efficacy testing of products, in addition 

to those specified as technical 

requirements following the test methods 

described in Appendix C to part 300, 

due to existing site-specific or areaspecific concerns when developing 

preauthorization plans. EPA proposes to 

remove the qualifier ‘‘When developing 

preauthorization plans’’ to provide 

greater flexibility for RRTs to require 

supplementary toxicity and efficacy 

testing, or available data or information 

that addresses site, area, or ecosystem 

specific concerns relative to the use of 

a product for situations even when 

preauthorization plans are not being 

developed. For example, RRTs may 

need additional testing or information 

for situations that fall under paragraph 

(b) of this section, including when 

developing an expedited decision 

making plan. The proposed revision 

also allows for RRTs to require 

supplementary product toxicity and 

efficacy testing, or available data or 

information for both planning and 

authorization of use situations, and 

based on that information may consider 

establishing limitations for the use of 

products in certain areas. The Agency is 

including ‘‘available data and 

information’’ to compliment the 

supplementary toxicity and efficacy 

testing provision recognizing that 

existing data or information that 

addresses site, area, or ecosystem 

specific concerns relative to the use of 

a product may be available. The Agency 

is also proposing to include 

‘‘ecosystem’’ with area and site specific 

concerns, as RRTs may want to gather 

additional information on the use of 

certain products when assessing the use 

of a product relative to the biological 

communities specific to their area. The 

proposal removes ‘‘in addition to the 

test methods specified in § 300.915 and 

described in appendix C to part 300.’’ 

While RRTs may want to use the 

efficacy and toxicity testing protocols 

specified in Appendix C of the NCP for 

comparative purposes, the proposed 

revisions clearly establish the RRTs 

authority to require tests using 

parameters beyond those specified in 

Appendix C. Furthermore, there may be 

supplementary toxicity and efficacy 

testing information based on recognized 

standard testing methods already 

available that RRTs may want to 

consider when addressing site, area, or 

ecosystem specific concerns. 

This proposal also provides the RRT 

authority to request that the OSC require 

a responsible party to conduct 

additional monitoring associated with 

the use of a product during a discharge 

incident. The proposed revision 

compliments the proposed monitoring 

requirements for dispersant use, but also 

including other chemical or biological 

agents, or other testing endpoints. The 

Agency believes the RRT must be 

afforded the ability to request that the 

OSC direct the responsible party to 

conduct additional monitoring under 

Subpart J for the use of a product in the 

environment. The RRT may request that 

the OSC consider additional monitoring 

during an oil discharge response to 

support operational decisions on 

dispersant use. For example, the RRT 

may want to monitor the exposure of 

marine mammals to oil constituents, 

including dispersed oil, or to monitor 

toxicity in the water column using 

biological assays. The Agency requests 

comments on these proposed revisions. 

(h) Recovery of Agents From the 

Environment 

The proposal identifies certain agent 

categories and substances intended to be 

removed from the environment 

following their use: Solidifiers, sorbents 

and surface washing agents. For those 

categories, the Agency expects the 

agents to be recovered from the 

environment to minimize any potential 

adverse impact. The proposal adds a 

new requirement that charges the 

responsible party, under OSC oversight, 

to recover these products from the 

environment. Recovery activities after 

the use of these agents would include 

containment of the agents in the water, 

collection of the agents mixed with oil 

or any residual agent, storage of the oilagent waste prior to disposal, and 

disposal of that oil-agent waste. The 

Agency also recognizes there may be 

situations where the safety of response 

personnel is threatened, or where 

additional harm to the environment 

could occur during recovery operations. 

Consequently, we are proposing these 

factors be considered when initiating 

recovery actions. While it is appropriate 

to have the OSC ensure these activities 

take place, it is ultimately the 

responsibility of the responsible party to 

conduct these activities and ensure that 

the agents are recovered from the 

environment. The Agency requests 

comments on this proposed 

requirement. 

(i) Reporting of Agent Use 

The proposal includes a new 

requirement for the OSC to provide to 

the RRT certain information after the 

use of a chemical or biological agent 

within 30 days of completion of agent 

operations. The information required in 

this report includes the information on 

any chemical or biological agent used, 

including product name, the quantity 

and concentration of the agent used 

during the response, the duration of use, 

the locations where the agent was used, 

and any data collected and analysis of 

efficacy or environmental effects. The 

proposal allows this information to be 

provided in the OSC report to the NRT 

or RRT as required under section 

300.165 of the NCP, if such a report has 

been requested. While other existing 

notification requirements serve to 

activate an immediate response to an 

event, the proposed requirement gathers 

information that will be useful in 

specifically evaluating the use of 

chemical or biological agents in the 

response. It will also inform the review 

of preauthorization plans and provide a 

basis for any necessary changes to 

improve environmental protection. 

Given that response and removal actions 

can greatly vary depending on the 

discharge situation, the Agency requests 

comments on whether it would be 

appropriate to allow the timeframe for 

submitting the report to be agreed upon 

by the RRT, rather than establishing a 

set timeframe. The Agency is requesting 

comments on this proposed new 

requirement, including on the proposed 

timeframe. 

3. Monitoring the Use of Dispersants 

The goal of establishing a Schedule 

under the NCP is to protect the 

environment from possible damage 

related to spill mitigating products used 

in response to oil discharges. The 

proposal establishes a regulatory 

approach under Subpart J that includes 

test data and information requirements 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
3394 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

11http://marinewellcontainment.com/expanded_

system.php. 12NRC, (2005), Oil Spill Dispersants: Efficacy and 

Effects, The National Academies Press, pp. 138, 

http://www.nap.edu/catalog.php?record_id=11283. 13 Ibid. 

for certain chemical and biological 

agents, procedures for authorizing the 

use of those agents, and monitoring 

requirements for certain discharge 

situations. 

Each oil discharge represents a unique 

situation with distinct conditions, 

which may require various response 

methods. When dispersants are applied 

to an oil discharge, field monitoring can 

be used to inform operational decisions 

by gathering site-specific information on 

the overall effectiveness, including the 

transport and environmental effects of 

the dispersant and the dispersed oil. 

The revisions to product test data and 

information requirements are intended 

to provide OSCs, RRTs, and ACs with 

the best information available when 

selecting products for use on an oil 

discharge. While laboratory test 

protocols allow for comparison between 

different products under standardized 

laboratory conditions and may be useful 

during the monitoring and assessment 

of a discharge event and/or for selection 

of the agents used in the response, they 

do not necessarily reflect field 

conditions. Monitoring of agents in the 

field informs the OSC and other 

agencies on the overall effectiveness of 

dispersant use, including the 

environmental effects and transport of 

dispersed oil. 

The Agency believes that 

comprehensive monitoring in certain 

discharge situations is necessary to 

determine the overall effectiveness of 

dispersants and should transcend from 

the initial dispersant application to 

include the transport and environmental 

effects of the dispersant and dispersed 

oil in the water column. Monitoring the 

overall effectiveness of dispersant use in 

the field provides those Agencies with 

responsibility for authorizing the use of 

dispersant product information for 

decision-making during subsurface or 

prolonged surface dispersant 

applications. Adverse effects on 

ecological receptors from exposures to 

dispersed oil depend on the length of 

time and concentration of the exposure, 

which in turn is dependent on the 

transport of dispersed oil. Because these 

exposures may vary depending on the 

discharge situation, the Agency believes 

comprehensive monitoring is important 

for certain discharge situations. This 

monitoring data will enhance the 

information needed for an effective 

response without delaying the use of 

agents under these conditions. 

Equipment is being contemplated to 

inject dispersants subsurface, directly 

into the oil near the source of the 

discharge.11 This type of application is 

intended to minimize dispersant 

dilution in the water before the 

dispersant has had an opportunity to 

interact with the oil.12 This application 

approach that is closer to the source is 

expected to reduce potential adverse 

environmental consequences from the 

use of excessive quantities of 

dispersants.13 However, applying 

dispersant to an oil discharge does not 

result in the physical recovery of oil 

from the environment. Instead, 

dispersing oil increases the potential 

exposure of aquatic organisms to the 

dispersant-oil mixture, at least 

transiently, and subsurface application 

has the potential to more immediately 

and effectively increase these exposures 

near the discharge. The Agency believes 

this new subsurface application 

approach requires new environmental 

monitoring capabilities to support 

operational decision-making. These new 

monitoring capabilities must be able to 

meet the operational conditions (e.g., 

water depths, temperatures) and be 

supported by knowledgeable personnel 

familiar with them. 

The proposed rule adds § 300.913 

establishing requirements for the 

responsible party to monitor any 

subsurface use of dispersant in response 

to an oil discharge, surface use of 

dispersants in response to oil discharges 

of more than 100,000 U.S. gallons 

occurring within 24 hours, and surface 

use of dispersants for more than 96 

hours in response to an oil discharge, as 

directed by the OSC. The purpose of 

monitoring subsurface application is to 

characterize the dispersed oil, follow 

the plume integrity and transport with 

the underwater current, and identify 

and assess the potential adverse effects 

from the dispersed oil. The proposal 

requires the responsible party to 

implement monitoring for any 

subsurface dispersant use in response to 

an oil discharge upon initiation and for 

the duration of subsurface dispersant 

use. The Agency believes monitoring 

subsurface use of dispersants is critical 

to inform response actions to minimize 

potential environmental effects. 

While surface application of 

dispersants is not a new approach and 

understood for small, short duration 

discharges, the Agency believes it is 

appropriate to require comprehensive 

monitoring for situations where 

dispersants are used for an extended 

period of time or in cases of major oil 

discharges. The Agency chose 100,000 

U.S. gallons as a threshold criterion for 

a major oil discharge because the NCP 

classifies a discharge of more than this 

quantity to coastal waters as major. In 

addition, EPA is proposing to this 

quantity monitoring of dispersant use in 

response to major oil discharges 

occurring within 24 hours since a larger 

quantity of dispersant may be required 

in a short time frame for an incident of 

this scale. The Agency also believes 

comprehensive monitoring should be 

required when surface dispersant is 

used for more than 96 hours because of 

potentially longer exposures of 

biological aquatic resources to 

dispersant and dispersed oil. Further, 

many acute toxicity studies use 96-hour 

exposure durations, including the acute 

toxicity tests using Menidia beryllina 

described in this proposal. While other 

toxicity tests have shorter exposure 

durations (e.g., 24, 48, or 72 hours), the 

Agency believes 96 hours is a 

reasonable threshold given its 

commonality of use in the toxicology 

field. Therefore, the proposal requires a 

responsible party to implement 

monitoring for surface dispersant use in 

response to an oil discharge under these 

discharge conditions and for the 

duration of dispersant use. The proposal 

also requires the submission of a 

Quality Assurance Project Plan for 

approval to the OSC covering the 

collection of all environmental data to 

ensure and maximize its quality, 

objectivity, utility, and integrity. The 

Agency welcomes comments on the 

proposed monitoring requirements, 

including the thresholds. Specifically, 

the Agency requests comments on 

whether it should also consider a 

threshold for surface use of dispersants 

that is based on the quantity of 

dispersant used within a given 

timeframe. Alternative thresholds must 

include a rationale in order for the EPA 

to consider them for final action. 

(a) Dispersant Application 

The proposal requires the responsible 

party to document the characteristics of 

the source oil; best estimate of the oil 

discharge flow rate, periodically 

reevaluated as conditions dictate, 

including a description of the method, 

associated uncertainties, and materials; 

dispersant(s) product used, rationale for 

dispersant choice(s), including the 

results of any efficacy and toxicity tests, 

recommended dispersant-to-oil ratio; 

and the application method and 

procedures, including a description of 

the equipment to be used, hourly 

application rates, capacities, and total 

amount of dispersant needed. For 

subsurface discharges, the proposal also 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 3395 

14http://www.epa.gov/quality/qa_docs.html. 

15http://www2.epa.gov/region8/environmentalsampling. 

requires the responsible party to 

document the best estimate of the 

discharge flow rate of any associated 

volatile petroleum hydrocarbons, 

periodically reevaluated as conditions 

dictate, including as description of the 

method, associated uncertainties, and 

materials. This would provide the OSC 

with the necessary information for 

operational decision-making and 

coordination of the dispersant 

application monitoring. 

Because of the many factors that 

influence the selection of a dispersant 

product (e.g., its availability, the type of 

oil it will be used on, the prevalent 

weather conditions, and the particular 

discharge situations) the Agency 

proposes that the responsible party 

document its product choice and 

selection rationale. Documenting the 

characteristics of the source oil provides 

specific chemical data to identify the oil 

associated with discharge and to inform 

decisions on dispersant use. 

Documenting application methods and 

procedures ensures that dispersant use 

is consistent with the dispersant 

manufacturer’s recommended 

concentrations, and conditions provided 

as part of the data requirements for 

listing the product on the Schedule. 

Documenting results of any additional 

efficacy and toxicity testing, or available 

data or information specific to the area 

or site conditions will assist the OSC in 

establishing the appropriateness of the 

dispersant choice. Documentation and 

clear understanding of the estimated 

daily oil discharge flow rate and the 

recommended dispersant-to-oil ratio 

(DOR) allows a dispersant rate to be 

established that would aid the OSC in 

determining the adequate dispersant 

usage. The OSC can compare the 

recommended DOR to the 

manufacturer’s recommended 

application concentration to ensure it is 

within the recommended range or to 

provide an opportunity for the 

responsible party to explain any 

deviations that may arise due to 

operational considerations. 

The biodegradation of petroleum 

constituents may result in a reduction in 

the dissolved oxygen concentration in 

the water column that could lead to 

hypoxia, which could be detrimental to 

marine organisms. The best estimate of 

the oil discharge flow rate, periodically 

reevaluated as conditions dictate, is an 

important consideration for monitoring 

dispersant use since the estimated 

amount of oil discharged may be used 

to provide insight into the potential 

oxygen demand exerted on the water 

column and to characterize the potential 

oil distribution. The proposal would 

also require the responsible party to 

document the best estimate of the 

discharge flow rate of any associated 

volatile petroleum hydrocarbons for 

subsurface applications. Volatile 

petroleum hydrocarbons (e.g., methane, 

and low molecular weight alkanes such 

as ethane, propane, and butane) 

associated with the discharge could 

contribute to a reduction in dissolved 

oxygen as a result of microbial 

degradation. The Agency is not 

proposing this requirement for surface 

applications given these compounds are 

expected to readily evaporate, making it 

unlikely they would be incorporated 

into the water column in quantities that 

would result in hypoxia. 

The proposal requires the 

documentation of the dispersant 

application method and procedures to 

include a description of the equipment 

to be used, including hourly application 

rates, capacities, and total amount of 

dispersant needed. Dispersant and 

equipment should be available to 

maintain the hourly dispersant 

application rate without significant 

deviation from the set rate. The Agency 

believes this information will assist in 

ensuring a consistent dispersant 

application rate. Dispersant application 

rates outside of established parameters 

may result in their over or under use, 

altering their effectiveness. Significant 

fluctuations in dispersant application 

rates could also indicate equipment 

malfunctions, requiring a reassessment 

of the response technique. EPA 

welcomes comment on the proposed 

requirements for dispersant application. 

Alternatives must include a rationale in 

order for the Agency to consider them 

for final action. 

(b) Water Column Sampling 

The proposal requires the responsible 

party to collect representative 

background samples from the water 

column at the closest safe distance 

determined by the OSC from the 

discharge, and in any direction of likely 

transport. The sampling should consider 

surface and subsurface currents and oil 

properties. Establishing background 

information prior to oil contamination 

from the discharge source provides 

reference data to compare against the 

results from water samples taken during 

the response. In establishing the 

background information, the responsible 

party should consider other potential 

sources of petroleum hydrocarbons (e.g., 

natural seeps) in the water column. The 

background samples would be collected 

in areas not affected by the discharge of 

oil throughout the water column upon 

initiation of dispersant use, at the 

closest safe distance as determined by 

the OSC from the oil discharge. 

Sampling would be conducted in any 

direction of likely transport considering 

surface and subsurface currents and the 

oil properties in those areas. The 

responsible party should consider using 

trajectory models that incorporate 

relevant factors such as oil type to 

determine the likely direction of the 

dispersed oil to inform where the water 

samples should be collected. 

The Agency is requiring that sample 

collection follow established standard 

operating and quality assurance 

procedures that are reliable and 

defensible. An accurate assessment of 

environmental data depends on the 

reliability, timeliness, and integrity of 

the data collected. Standard operating 

procedures should describe the 

appropriateness of the sampling 

method; the equipment needed for 

sample collection; a description of 

potential interferences, problems that 

may be encountered and corrective 

actions that would be taken; the sample 

collection procedure, including the 

preparation steps, representative 

sampling considerations, and sampling 

steps for each sampling device used; 

sample preservation, containers, 

handling, and storage; decontamination 

of sampling equipment; and record 

keeping and quality control procedures. 

These elements are generally described 

in various guidance documents on 

standard operating and quality 

assurance procedures for environmental 

sampling.14 15

In addition to the background water 

sample collection, the proposal requires 

the responsible party to collect water 

column samples daily in the dispersed 

oil plume at such depths and locations 

where dispersed oil is likely to be 

present. EPA believes the dispersed oil 

plume captures the presence of oil from 

either the subsurface or the surface 

application of dispersant, including 

where oil could be rising to the surface 

from a subsurface discharge or the 

dispersed oil plume at the water surface 

as a result of surface dispersant 

application. The responsible party also 

would need to analyze for: 

• In-situ oil droplet size distribution 

analysis, including the mass or volume 

mean diameters between droplet sizes 

ranging from 2.5 to 2000 mm, with the 

majority of data collected between the 

2.5 and 100 mm sizes. Droplet size 

distribution, which is an important 

component to understanding the 

chemical and hydrodynamic 

effectiveness of dispersants, can be 

measured with devices such as the Laser 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
3396 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

16Li, M. and Garrett, C., (1998) The Relationship 

Between Oil Droplet Size and Upper Ocean 

Turbulence, Mar. Poll. Bull., Vol. 36, pp. 961–970. 

17Li, Z., Lee, K., King, T., Boufadel, M.C., Venosa, 

A.D., (2008) Assessment of Chemical Dispersant 

Effectiveness in a Wave Tank under Regular NonBreaking and Breaking Wave Conditions, Mar Pollut 

Bull, Vol. 56, pp. 903–912. 

18Li, Z., Lee, K., King, T., Boufadel, M.C., Venosa, 

A.D., (2009) Evaluating Chemical Dispersant 

Efficacy in an Experimental Wave Tank: 2— 

Significant Factors Determining In Situ Oil Droplet 

Size Distribution, Env Eng Scien, Vol. 26, pp 1407– 

1418. 

19Henry, C.B., Roberts, P.O., Overton, E.B., A 

Primer on In Situ Fluorometry to Monitor Dispersed 

Oil, IOSC 1999;246. 

20Coble, P.G., (2007) Marine Optical 

Biogeochemistry: The Chemistry of Ocean Color, 

Chem. Rev., Vol. 107, pp. 402–418. 

21Bugden, J.B.C., Yeung, C.W., Kepkay, P.E., Lee, 

K. (2008) Application of Ultraviolet Fluorometry 

and Excitation-Emission Matrix Spectroscopy 

(EEMS) to Fingerprint Oil and Chemically 

Dispersed Oil in Seawater, Mar Pollut Bull, Vol. 56, 

pp. 677–685. 

22Conmy, R.N., Coble, P.G., Farr, J., Wood, A.M., 

Lee, K., Pegau, W.S, Walsh, I.D., Koch, C.R., 

Abercrombie, M.I., Miles, M.S, Lewis, M.R., Ryan, 

S.A., Robinson, B.J., King, T.L., Kelble, C.R., and 

Lacoste, J. (2014) Submersible Optical Sensors 

Exposed to Chemically Dispersed Crude Oil: Wave 

Tank Simulations for Improved Oil Spill 

Monitoring, Environ Sci Technol, Vol. 48, pp. 

1803–1810. 

23Bugden, J.B.C., Yeung, C.W., Kepkay, P.E., Lee, 

K. (2008) Application of Ultraviolet Fluorometry 

and Excitation-Emission Matrix Spectroscopy 

(EEMS) to Fingerprint Oil and Chemically 

Dispersed Oil in Seawater, Mar Pollut Bull, Vol. 56, 

pp. 677–685. 

24 Kepkay, P.E., Yeung, C.W., Bugden, J.C.B., Li, 

Z., and Lee, K. (2008) Ultraviolet Fluorescence 

Spectroscopy (UVFS): A New Means of Determining 

the Effect of Chemical Dispersants on Oil Spills, 

IOSC, pp. 639–644. http://ioscproceedings.org/doi/ 

abs/10.7901/2169-3358-2008-1-639. 

In-Situ Scattering and Transmissometry 

(LISST) instrument or other similar 

instruments. Small oil droplets (e.g., 

diameters in the tens of mm range) have 

such low rise velocities that they tend 

to remain suspended in the water 

column (neutrally buoyant), where they 

can become widely dispersed by 

advective forces, turbulent motion, and 

to a lesser extent diffusion. These small 

droplets are more readily amenable to 

biodegradation due to their higher 

surface area to volume ratio. In contrast, 

large oil droplets (e.g., diameters >100 

mm) will tend to recoalesce and rise 

faster to the surface.16 Effective 

application of dispersants is expected to 

generate a larger number of small 

droplets, reducing the average droplet 

size.17 This will change the trajectory of 

rising oil that is subjected to stratified 

horizontal subsurface currents. Near the 

water surface, hydrodynamic and other 

environmental factors also influence the 

oil droplet size distribution. Mixing 

energy, especially from breaking waves, 

dictates the breakup of large oil droplets 

into smaller droplets and the depth of 

submergence of the droplets. Plunging 

breaking waves under experimental 

conditions produced the smallest oil 

droplets.13 14 Additionally, studies 

indicate that the type of chemical 

dispersant used is an important factor in 

controlling the dispersed oil droplet size 

distributions. Further, wave tank studies 

have shown that the chemically 

dispersed oil may result in a droplet 

size distribution that has not been 

observed without the use of dispersants 

(i.e., physically dispersed oil), both in 

terms of a smaller volumetric mean 

diameter and a bimodal distribution for 

droplet size diameters below 100 mm.18

EPA recognizes that the aforementioned 

studies were conducted under 

conditions characteristic of surface 

waters. However, the effect of the high 

velocities of oil that may occur from a 

discharge from a subsurface oil well on 

the oil droplet size distribution requires 

further scientific investigation to 

understand the contribution of 

physically dispersed oil relative to 

chemically dispersed oil. In either 

event, it is clear droplet size distribution 

analysis provides important data useful 

in optimizing operational guidelines 

and decision making, modeling 

transport and fate, and potentially 

evaluating biological effects of 

chemically dispersed oil. The proposal 

also includes larger oil droplet sizes of 

up to 2000 mm, intended to provide 

information that can inform the oil 

distribution using trajectory modeling 

analysis. 

• In-situ fluorometry. When exposed 

to ultraviolet (UV) light, certain 

compounds absorb energy that can 

elevate electrons into an excited higher 

energy level. The wavelength that 

excites electrons into a higher energy 

state is typically referred to as the 

excitation wavelength. Electrons 

unstable at the higher energy state 

return to a lower energy state, emitting 

energy at longer emission wavelengths 

resulting in fluorescence.19 Many 

organic compounds fluoresce at specific 

excitation and emission wavelengths 

that allow for identifying many of the 

components of dissolved organic matter 

and other compounds (e.g., crude oil) in 

seawater.20 For crude petroleum oils, 

the aromatic fraction is responsible for 

the fluorescence property of petroleum, 

and these compounds are used to 

determine the specific excitation and 

emission wavelengths for monitoring. 

When subject to excitation at certain 

wavelengths in the near ultraviolet 

spectrum, polycyclic aromatic 

hydrocarbons (PAH) fluoresce over a 

range of higher wavelengths, depending 

on the number of aromatic rings in the 

structure.21 Fluorometers can be 

targeted to the type of oil discharged, 

and the excitation and emission 

wavelengths chosen should match the 

aromatic properties of the oil 

discharged. Although this measure does 

not include all oil constituents, 

fluorescence is a valuable screening tool 

deployed during a response,22 providing 

a rapid indication of potential dispersed 

oil in the water column, as well as an 

indicator of dispersion effectiveness as 

discussed in the following section. The 

Agency request comments on alternative 

spectroscopy techniques such as 

absorption measurements that may be 

used to rapidly estimate oil 

concentrations in the water during a 

discharge event. 

• Fluorescence signatures. In addition 

to in-situ fluorometry, the proposal 

requires the responsible party to 

conduct a fluorescence intensity 

analyses on water samples collected to 

determine fluorescence signatures of the 

dispersed oil. EPA proposes to use 

fluorescence signatures as a relatively 

simple and rapid means to assess 

dispersion effectiveness. This includes 

but is not limited to, identifying the 

peak wavelength position, magnitude 

and ratios of fluorescence intensity of 

the dispersed oil. For example, 

measuring the reduction in an intensity 

ratio after applying dispersant to the oil 

in seawater may provide an estimate of 

the effect of chemical dispersion.23 24

Ratios of fluorescence intensity are 

derived from the three dimensional 

excitation/emission matrix spectra 

(EEMS) acquired by combining multiple 

emission spectra obtained from oil 

exposed to individual excitation 

wavelengths typically using a scanning 

spectrofluorometer. If the optimal 

excitation and emission bands are 

known, then these ratios may be derived 

from measuring the fluorescence 

intensity at two different fixed emission 

wavelengths at a single fixed excitation 

wavelength. The ratios are calculated by 

dividing the fluorescence intensity of 

the shorter emission band by the 

fluorescence intensity of the longer 

band. Studies have shown that adding 

dispersants to crude petroleum oil 

increases the fluorescence intensity of 

the longer emission band, driving down 

the value of the ratio. Although 

individual petroleum oils may have 

common spectral characteristics, the 

ideal three-dimensional EEMS for the 

discharged oil should be obtained from 

scanning the source oil. Therefore, the 

monitoring should include procedures 

to obtain the EEMS using the source oil 

to determine the optimal excitationemission wavelengths. The Agency 


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Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 3397 

25Barwise, A. J. G. and Whitehead, E. V. (1980). 

Separation and Structure of Petroporphyrins. In: 

Advances in Organic Geochemistry 1979. (A. G. 

Douglas and J. R. Maxwell, eds.), Pergamon, New 

York, pp. 181–92. 

26Barwise, A. J. G. (1990). Role of Nickel and 

Vanadium in Petroleum Classification. Energy & 

Fuels, 4, 647–52. 

27All, M.F., Bukharl, A., and Saleem, M., (1983) 

Trace Metals in Crude Oils from Saudi Arabia, Ind. 

Eng. Chem. Prod. Res. Dev. 1983, Vol 22, pp. 691– 

694. 

28http://water.epa.gov/type/rsl/monitoring/

vms55.cfm. 

request comments on alternative 

techniques or measurements that may 

be used to rapidly assess dispersion 

effectiveness during a discharge event. 

• Dissolved oxygen (DO). Dissolved 

oxygen is an important variable to 

monitor in the application of 

dispersants, particularity in subsurface 

waters that may inform operational 

decisions. For surface dispersant 

application, dissolved oxygen is 

expected to be higher in the mixed layer 

in the surface water. Dissolved and/or 

dispersed oil represents a readily 

available carbon source for microbial 

oxidation, and this metabolic activity 

can lead to a decrease in the DO content 

in the water column. The oil degrading 

community in the water is an important 

DO sink for the mass transfer of 

hydrocarbons in the subsurface, and 

advantage can be taken of this fact 

during a response. The decline in DO 

due to hydrocarbon biodegradation 

could approach or exceed levels of 

concern (i.e., hypoxia) and thus be 

detrimental to surrounding organisms 

(e.g., invertebrates and vertebrates). 

Dissolved oxygen, which relies on the 

diffusion of molecular oxygen through a 

membrane in the sensor, is commonly 

measured during oceanographic survey 

cruises using an in-situ DO instrument 

that provides real-time results. 

However, a DO sensor instrument that 

passes through a dissolved and/or 

dispersed oil layer is subject to 

contamination by the oil and could lead 

to questionable measurements if such 

fouling of the electrodes occurs, 

particularly at depths where the 

dissolved and/or dispersed plume depth 

are expected to coincide with 

depressions in dissolved oxygen. 

Therefore, the Agency is concerned that 

relying solely on measurements from insitu oxygen instruments may lead to an 

erroneous interpretation of oxygen data. 

Thus, the Agency believes that ex-situ 

confirmatory DO measurements should 

also be conducted using Winkler 

titrations to confirm in-situ dissolved 

oxygen measurements. 

• Total petroleum hydrocarbons, 

individual resolvable constituents, 

including volatile organic compounds, 

aliphatic hydrocarbons, monocyclic, 

polycyclic, and other aromatic 

hydrocarbons, including alkylated 

homologs, and hopane and sterane 

biomarker compounds. The Agency is 

proposing that the responsible party 

analyze each water sample collected for 

total petroleum hydrocarbons (TPHs), 

individual resolvable constituents, 

including volatile petroleum 

hydrocarbons, and branched and normal 

aliphatic hydrocarbons. The analysis 

would also include monocyclic, 

polycyclic and other aromatic 

hydrocarbons (e.g., heterocyclic 

aromatic hydrocarbons), including their 

alkylated homologs, and hopanes and 

steranes biomarker compounds. TPHs 

are best measured using gas 

chromatograph (GC) equipped with a 

flame ionization detector (FID). TPH 

analysis measures total alkanes and 

aromatics, can be obtained relatively 

quickly, and provides a good 

measurement for initial screening. 

Given that PAHs and biomarkers are 

typically measured using GC/MS, the 

proposal includes GC/MS analysis to 

provide the alkanes, PAHs, and 

biomarker (e.g., hopane) specificity 

important in identifying certain oil 

constituents that may be present in the 

oil discharge. Identifying the 

concentrations of PAHs and biomarkers 

assists responders in making informed 

operational decisions regarding the 

dispersant application because these 

compounds can be compared against the 

composition of the source oil, which 

serves as a reference to determine the 

degree of weathering for oil. 

• Carbon Dioxide (subsurface only). 

The aerobic biodegradation of oil 

constituents not only consumes 

dissolved oxygen, but would also 

produce carbon dioxide. Increases in the 

concentration of carbon dioxide that 

coincide with decreases in the 

concentration of dissolved oxygen 

would provide credible evidence that 

biodegradation of oil is occurring. Thus, 

the Agency believes that measuring the 

in-situ carbon dioxide for subsurface 

dispersant applications would be a good 

indicator of microbial oxidation and 

inform the OSC on the potential fate. 

• Methane if present (subsurface 

only). The microbial degradation of 

methane may contribute to a reduction 

in dissolved oxygen. Thus, the Agency 

believes that, when present, subsurface 

in-situ methane measurements are an 

important factor to consider in 

evaluating dissolved oxygen levels. 

• Heavy metals analysis, including 

nickel and vanadium. Crude petroleum 

oil may contain certain heavy metals, 

including nickel and vanadium.25 26 27

Dispersing oil may increase the 

bioavailability of certain associated 

heavy metals to marine organisms. 

Therefore, the Agency is proposing to 

include heavy metal analysis as part of 

the sampling analyses to be conducted. 

• Turbidity. Turbidity is a general 

measure of water clarity. Turbidity is 

determined by measuring how much 

material suspended in water decreases 

the passage of light through the water.28

Suspended materials may include soil 

particles (clay, silt, and sand), algae, 

plankton, microbes, and other 

substances. This measure provides a 

quick assessment of suspended 

materials in receiving waters from other 

water bodies and is useful in 

determining the presence of materials 

that could interfere with oil particle size 

determinations. Alternatively, the 

Agency is requesting comments on 

whether there are other physical 

measurements in the water that would 

provide similar timely information, or 

that can serve as validation for turbidity 

values collected in situ. 

• Water temperature. Water 

temperature typically is measured using 

an electronic thermometer on the 

conductivity-temperature-depth (CTD) 

instrument. When combined with 

salinity and pressure, temperature 

measurements are used to calculate 

water density, which may change along 

the vertical profile. Along with the 

horizontal subsurface currents and the 

rise velocity of the dispersed oil, the 

ambient density gradient is an 

important factor in determining the 

behavior of dispersed oil in the water 

column. Water temperature is also an 

important variable that may influence 

the effectiveness of dispersant 

applications. For example, cold 

temperatures may, among other 

environmental factors, impact the 

effectiveness of dispersants as it affects 

certain oil properties (e.g., viscosity). 

Colder temperatures also may affect the 

degree of oil weathering (e.g., 

evaporation), and the amount of 

dispersant/oil mixing energy (wave 

action) needed to effectively disperse oil 

relative to warmer temperatures. 

• pH. The pH is a simple standard 

measurement used to analyze water 

quality that can affect chemical or 

biological processes in water. pH also 

determines the solubility and biological 

availability of chemical constituents 

such as heavy metals. 

• Conductivity. Conductivity is 

measured by passing a current through 

the water in a CTD instrument, which 

is then compared against known 

salinities to obtain the water salinity. 

When combined with temperature, and 

pressure, salinity measurements are 


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29http://www.epa.gov/emap/nca/. 

30Barron, M.G., Hemmer, M.J., and Jackson, C.R., 

(2013) Development of Aquatic Toxicity 

Benchmarks for Oil Products Using Species 

Sensitivity Distributions, Integr Environ Assess 

Manag, Vol. 9, pp. 610–615. 

31Aldenberg, T. and Jaworska, J.S., (2002) 

Uncertainty of the Hazardous Concentration and 

Fraction Affected for Normal Species Sensitivity 

Distributions, Ecotox and Environ Safety, Vol. 46, 

pp. 1–18. 

32Barron, M.G., and Wharton, S., (2005) Survey 

of Methodologies for Developing Media Screening 

Values for Ecological Risk Assessment, Integrated 

Environmental Assessment and Management, Vol. 

1, pp. 320–332. 

used to calculate water density, which 

may change significantly along the 

vertical profile. Along with the 

horizontal subsurface currents and the 

rise velocity of the dispersed oil, the 

ambient density gradient is an 

important factor in determining the 

behavior of dispersed oil in the water 

column. 

The Agency requests comment on the 

proposed approach to water column 

sampling. Alternatives must include a 

rationale in order for the Agency to 

consider them for final action. 

(c) Oil Distribution Analyses 

The proposal requires that the 

responsible party, in consultation with 

the OSC and using best available 

technologies, characterize the dispersant 

effectiveness and oil distribution, 

considering the condition of the oil, 

dispersant, and dispersed oil 

components from the discharge 

location. EPA believes this is necessary 

to inform sampling locations by 

assessing the horizontal and vertical 

boundaries of the dispersed oil plume 

and the direction of likely transport. 

The majority of the sampling can then 

be focused on known or suspected 

locations and depths of the dispersed 

oil. Based on the initial water sampling 

results to characterize the boundaries of 

the dispersed oil, the sampling design 

can be tailored to optimize sampling. 

The Agency proposes that the 

responsible party characterize the 

dispersant effectiveness to determine 

the changes in the condition of the oil 

due to weathering, which can include 

changes in oil viscosity due to water 

uptake (e.g., mousse). Weathered oil that 

mixes with water may result in 

significant emulsification (e.g., water-inoil emulsions), which in turn may 

decrease the dispersant’s chemical 

effectiveness and diminish 

biodegradability. Therefore, the 

characterization of dispersant 

effectiveness should provide a 

reasonable estimate to the extent (e.g., 

distance from the discharge source) in 

which the dispersant can be applied to 

the oil and still be effective. The Agency 

believes this will result in better 

dispersant applications and minimize 

excessive dispersant use. The Agency 

requests comment on this approach. 

Alternatives posed must include a 

rationale for the Agency to consider 

them for final action. 

(d) Ecological Characterization 

The Agency proposes that the 

responsible party characterize the 

ecological receptors (e.g. aquatic 

species, wildlife, and/or other biological 

resources), their habitats, and exposure 

pathways that may be present in the 

discharge area, in consultation with the 

OSC. Exposure pathways, such as 

ingestion, refer to the way in which 

ecological receptors may come into 

contact with discharged oil and result in 

exposure that would be detrimental to 

ecological receptors. The Agency 

believes that the ecological 

characterization should include those 

species that may be in sensitive life 

stages, transient or migratory species, 

breeding or breeding-related activities 

(e.g., embryo and larvae development), 

and threatened and/or endangered 

species that may be exposed to oil, 

dispersed oil, and dispersant, which in 

turn will assist the OSC in managing 

response actions, including those 

actions that were determined not to be 

needed. In developing the 

characterization of ecological receptors, 

the responsible party may refer to 

relevant sources of information such as 

applicable expedited decision-making 

plans, environmental assessments or 

statements, Federal and state 

environmental databases (e.g., ACP— 

Fish and Wildlife and Sensitive 

Environments Annex; NOAA— 

Environmental Sensitivity Indices; 

NOAA—NMFS Southeast Area 

Monitoring and Assessment Program; 

EPA—National Coastal Assessment 29) 

or through studies conducted by 

universities or other research-oriented 

institutions. 

The proposal requires the responsible 

party to consult with the OSC to 

determine an acute toxicity level of 

concern for the dispersed oil using 

available dose/response information 

relevant to potentially exposed species. 

The envisioned approach would be to 

monitor acute toxicity in the water 

column concurrently with dispersed oil 

sampling for fluorometry, particle size, 

and water quality (e.g., dissolved 

oxygen). The TPH concentrations in 

water samples taken throughout the 

water column could then be compared 

to TPH-based ecotoxicity benchmarks 

(EBs). Water samples collected for 

comparison of aqueous TPH 

concentrations to EBs would be 

analyzed and reported within the 

timeframe necessary to make 

operational decisions (e.g., within 24 

hours of collection). Sampling could 

also be performed in areas without 

dispersant application to distinguish 

toxicity associated with physically 

dispersed oil from that of chemically 

dispersed oil. 

While EBs may have already been 

established during the development of 

contingency plans, they can also be 

derived at the time of an incident. One 

approach is to use a species sensitivity 

distribution (SSD),30 which allows for 

species relevant to the location of the 

discharge to be considered. An SSD is 

a probability distribution of the 

sensitivity of a group of species to a 

toxicant.31 SSDs could be developed for 

representative oils (e.g., crude oils) 

using existing acute toxicity values for 

mortality or immobility (e.g., 48 and 96 

hr LC50) where sufficient species 

diversity are available (e.g., toxicity data 

for 10 or more species). For example, 

the EBs could be computed from the 

fifth percentile of the SSD as the hazard 

concentration 5 percent (HC5), as they 

are considered protective of 95% of 

species, have been used by EPA for 

developing ambient water quality 

criteria, and are generally accepted by 

the international community.32 Chronic 

toxicity benchmarks may be derived 

applying safety factors to the acute 

toxicity EBs. The Agency requests 

comments on the proposed approach to 

ecotoxicity assessment, and whether it 

should consider making SSDs a 

requirement for deriving EBs. If 

alternative approaches are suggested, 

the commenter must include an 

appropriate rationale in order for the 

Agency to consider them for final 

action. 

(e) Immediate Reporting 

The proposal requires the responsible 

party to immediately report to the OSC 

any deviation of more than 10 percent 

of the mean hourly subsurface 

dispersant use rate for the total 

dispersant volume authorized for that 

24 hour use, and the reason for the 

deviation (e.g., equipment malfunction). 

The Agency believes that inconsistent 

dispersant application rates confound 

data sampling interpretation due to 

variations in the DOR. The proposal, 

however, provides a margin for 

variation within 10 percent of the mean 

hourly subsurface dispersant 

application rate to account for 

equipment performance. The Agency 

believes this margin to adequately 

account for variations in dispersant 


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injection equipment without being 

overly restrictive. EPA requests 

comments on whether it should 

consider a similar requirement for 

dispersant surface application. 

The Agency also is proposing to 

require the immediate reporting of 

ecological receptors, including any 

threatened or endangered species that 

may be exposed to dispersed oil based 

on trajectory modeling and the 

estimated acute toxicity level of 

concern. Results from daily sampling 

(e.g., droplet size distribution, TPH) 

would provide input data to refine 

predictions of the likely dispersed oil 

direction using trajectory modeling. 

Further, results may also inform 

decisions to alter dispersant application 

in order to minimize effects on 

biological resources. 

(f) Daily Reporting 

The proposal requires daily reporting 

of sampling and data analyses collected 

within the timeframe necessary to make 

operational decisions (e.g., within 24 

hours of collection), including 

documented observations, photographs, 

video, and any other information related 

to dispersant use, unless an alternate 

timeframe is authorized by the OSC. 

Daily reporting would also include the 

total amount of dispersant used for the 

previous reporting period. Additionally, 

the proposal would require a schedule 

for any data analyses that require time 

beyond 24 hours due to analytical 

methods; this schedule is not to exceed 

120 hours (i.e., 5 days) unless 

authorized by the OSC. Timely sample 

analyses afford the OSC and other 

responders with multiple relevant data 

that can be analyzed together to inform 

situational awareness of dispersant 

operations and adjust dispersant 

application if necessary. The Agency 

believes that a 120-hour window for 

analyses requiring additional time 

provides an adequate opportunity to 

conduct all requested analyses in a 

timely manner without being overly 

restrictive. Finally, the proposal 

requires the responsible party to report 

the estimated daily transport of 

dispersed and non-dispersed oil, and 

associated volatile petroleum 

hydrocarbons if applicable, and 

dispersants, using the best available 

trajectory modeling. This information is 

intended to assist response planners to 

coordinate response activities and to 

schedule monitoring activities based on 

the expected transport of oil and 

dispersed oil. 

4. Data and Information Requirements 

for Product Schedule Listing 

The Agency is proposing to revise the 

data and information requirements for 

listing products on the Schedule in 

§ 300.915 of Subpart J. The proposed 

amendments revise the efficacy and 

toxicity testing protocols and listing 

criteria for all chemical and biological 

agents on the Schedule. Additionally, 

the Agency proposes revisions to the 

requirements for general product 

information, Confidential Business 

Information (CBI) claims, submission 

package contents, EPA review and 

listing procedures, requests for decision 

review, changes to products, 

transitioning products from the current 

Schedule to the new Schedule, 

mandatory product disclaimer, and 

removal of products from the Schedule. 

(a) General Product Information 

The Agency is proposing to 

consolidate the general submission 

requirements applicable to all types of 

agents that may be listed on the 

Schedule in paragraph (a) of § 300.915. 

Subsequent regulatory paragraphs in 

this section are proposed to include 

requirements specific to each product 

category. Additionally, the Agency is 

proposing to require some additional 

information, as applicable, regarding 

products that are submitted for 

Schedule listing consideration. The 

proposed general information 

requirements for all products are 

proposed to be revised as follow: 

• Submitter: Name, physical address, 

email, telephone number, identity of 

submitter (i.e., manufacturer, vendor, 

importer, distributor, designated agent 

for the manufacturer), and 

documentation of such identity. 

• General Product: All name(s), 

brand(s), and/or trademark(s) under 

which the product is to be sold; Safety 

Data Sheet (SDS); sample product labels 

for all name(s), brand(s), and/or 

trademark(s); chemical or biological 

agent categories under which the 

product is submitted for listing, 

including information on the specific 

process(es) through which the product 

affects the oil, and the specific 

environment (waters and/or adjoining 

shorelines) on which it is intended to be 

used. 

• Supplier: Names, physical 

addresses, emails and telephone 

numbers of the primary distributors, 

vendors, importers, and/or designated 

agent acting on behalf of the 

manufacturer. 

• Product Storage: Maximum, 

minimum and optimum temperature, 

humidity and other relevant conditions 

for product storage; impact on product 

performance if the product is not stored 

within recommended limits; and 

anticipated shelf life at the 

recommended storage conditions. 

• Product Use: Recommended 

procedures, including product 

concentrations, application ratios, types 

of application equipment, conditions for 

use, and any application restrictions. 

The procedures must address variables 

such as weather, water salinity, water 

temperature, types and weathering 

states of oils or other pollutants, and 

product and oil containment, collection, 

recovery and disposal, and include 

supporting documentation and standard 

methods used to determine them. 

• Environmental Fate: Known 

measured data and supporting 

documentation on the persistence, 

bioconcentration factor, 

bioaccumulation factor, and 

biodegradability of the product and all 

of its components. 

• Physical/Chemical Properties and 

Formulation: Physical state and 

appearance; vapor pressure; flash point; 

pour point; viscosity; specific gravity; 

particle size for solid components; pH; 

citation of standard methods used to 

determine the physical/chemical 

properties; identity of all components in 

the product, including each specific 

component name; corresponding 

Chemical Abstract Service (CAS) 

Registry Number; the maximum, 

minimum, and average weight percent 

of each product component; and the 

intended function of each component 

(e.g., solvent, surfactant). 

• For products that contain 

microorganisms, enzymes and/or 

nutrients: All microorganisms and 

weight percent by current genus and 

species, including any reclassifications; 

all enzymes and their International 

Union of Biochemistry (I.U.B.) 

number(s); Enzyme Classification (EC) 

code numbers; the source of each 

enzyme, units, and specific oildegrading activity; name(s) and 

maximum, minimum, and average 

weight percent of the nutrients 

contained in the product; citation or 

description of the methodology used to 

determine product components; 

certification, including data, 

methodology, and supporting 

documentation, indicating that the 

product does not contain levels that 

exceed the National Ambient Water 

Quality Criteria lowest density value for 

the following: Bacterial, fungal, or viral 

pathogens or opportunistic pathogens, 

including, but not limited to, enteric 

bacteria such as Salmonella, fecal 

coliforms, Shigella, Coagulase positive 


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Staphylococci, and Beta Hemolytic 

Streptococci or enterococci. 

• National Water Quality Standard 

Contaminants: Certification, including 

data, methodology, and supporting 

documentation, indicating that the 

product does not contain levels that 

exceed the National Water Quality 

Standards lowest aquatic life acute 

value for the following contaminants: 

Metals reasonably expected to be in the 

product including arsenic, cadmium, 

chromium, copper, lead, mercury, 

nickel, vanadium, zinc; cyanide; 

chlorinated hydrocarbons; pesticides; 

polychlorinated biphenyls (PCBs); and 

polynuclear aromatic hydrocarbons 

(PAHs). 

• Certification, including data, 

methodology, and supporting 

documentation, indicating that the 

product does not contain prohibited 

agents (sinking agents, nonylphenol, or 

nonylphenol ethoxylates). 

• Testing Laboratory Information: 

Name, address, contact name, email, 

phone number; national or international 

accreditations. 

• Laboratory Testing Data and 

Reports: All applicable information, 

data and analysis specified in the testing 

protocols, including raw test data and 

replicates, notes and observations, 

calculated mean values and standard 

deviations, summary of stock solution 

preparation, source and preparation of 

test organisms, test conditions, and 

chain of custody forms. 

• Production capacity: Estimated 

annual production volume; average and 

maximum volume per day; time needed 

to reach that maximum production rate 

(days). 

• Performance Capabilities/Benefits: 

Recognition received from, if applicable; 

national and/or international product 

testing or use data, recognitions (e.g., 

EPA’s Design for the Environment), and/ 

or certifications, informing the 

performance capabilities or 

environmental benefits of the product. 

The proposed revisions group 

together and simplify the general 

submission requirements applicable to 

all product types. EPA believes 

reorganizing the general requirements in 

a central location will clarify which 

requirements are applicable to all 

submissions, and which are specific to 

each product type by including them in 

separate sections. While most of the 

information listed above is currently 

required to be submitted under Subpart 

J, the Agency is proposing revisions to 

several of the existing general 

requirements and several new data and 

information requirements. The Agency 

believes the proposed revisions and 

added new requirements will better 

characterize the nature of the product 

and will assist EPA in product listing 

decisions. The information will also 

assist the RRTs in their area planning 

activities, and the OSCs in authorizing 

the appropriate use of chemical and 

biological agents. Details on the 

proposed additions and revisions are as 

follow: 

(1) Identification and documentation 

by the submitter of its status in 

relationship to the product as the 

manufacturer, vendor, importer, 

distributor, or other designated agent of 

the manufacturer. This proposed 

requirement is intended to clearly 

establish the point of contact 

responsible for the submission, and to 

avoid any conflicts or claims from 

unauthorized entities on products listed 

or submitted for consideration. 

(2) Chemical or biological agent 

categories under which the product is 

submitted for listing, including 

information on the specific process(es) 

through which the product affects the 

oil, and the specific environment(s) 

(water and/or adjoining shorelines) on 

which it is intended to be used. 

Currently, when a product meets the 

definitions of two or more product 

categories, a submitter must provide 

technical product data for each of those 

product categories. After review of the 

submitted technical product data, EPA 

makes a determination on whether and 

under which category the ‘‘mixed 

product’’ should be listed on the 

Schedule. It has been Agency policy to 

list products only under one category to 

avoid confusion in the field during a 

response, and because the process(es) 

through which the products affect the 

oil for different product categories do 

not generally overlap or allow for 

multiple uses of one product. However, 

EPA has received comments from 

responders, vendors, and manufacturers 

who believe that it is appropriate for 

certain products to be listed under more 

than one category. The Agency is 

proposing to revise the current 

limitations for mixed products. The 

proposal allows for products to be 

considered under multiple categories 

provided they meet all of the listing 

requirements for each. To this end, the 

Agency is also requiring that 

information be provided identifying 

which environments the product is 

intended to be used for, in the water 

and/or on the shoreline. EPA is 

soliciting comments on the issue of 

multiple category product listing. 

(3) Copy of the Safety Data Sheet 

(SDS) required by the Occupational 

Safety and Health Administration 

(OSHA) under their Hazard 

Communication Standard (HAZCOM) 

for the product. EPA recognizes that 

chemical and biological agents may 

contain substances that could cause 

harm to oil spill responders who, if 

unaware of the product’s formula, may 

not wear the proper personal protective 

equipment. SDSs describe the hazards 

that may be involved with the product 

and recommend safety measures that 

would minimize or avoid adverse 

consequences that may result from 

exposures. The Agency believes SDS 

information will be useful to both OSCs 

and responders when authorizing and 

using the product respectively, and that 

adding this new requirement for a 

product SDS is appropriate. While the 

Agency believes that the relevant SDS 

information should be that of the 

product, we request comment on the 

value for responders of requiring an SDS 

for each individual component. The 

Agency requests comments on this new 

requirement, as well as whether the 

submitter should provide any additional 

information on potential adverse human 

health effects based on the product’s 

formula and application methods not 

captured in the SDS, and how to best 

communicate this information to 

product end users. 

(4) Sample product label for all 

names, brands, or trademarked versions 

of the product that include the 

manufacture and expiration dates of the 

product, as well as the conditions for 

storage. The Agency would be allowing 

flexibility in complying with this 

requirement by specifying that the 

submitter does not need to affix new 

labels to comply with this section if 

existing labels already convey the 

required information. This proposed 

requirement is not intended in any way 

to supersede any other federal labeling 

requirement in place (e.g., OSHA’s 

HAZCOM). The proposed requirement 

is intended to assist the OSC in ensuring 

that the product used to respond to an 

incident is still viable and effective, and 

the oil spill response organizations 

(OSROs) or any other responder that is 

storing the product to ensure that their 

stockpile is viable and available to be 

authorized for use. 

(5) Recommended product use 

procedures. The Agency is proposing to 

revise the requirement for providing 

information on the recommended 

application procedures. While the 

proposal is maintaining the specific 

elements included in the current 

requirement, the supporting 

documentation and information on the 

standard methods the product 

manufacturer used to establish the 

procedures is requested. EPA believes 

that providing detailed information on 

the recommended product use 


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procedures is necessary to inform the 

OSC when authorizing these products. 

This supporting documentation and 

specific information on the methods and 

standards used to establish them will 

inform OSCs and other response 

personnel in selecting products that can 

be effectively used under the operating 

conditions encountered for any given 

incident. The Agency requests comment 

on the revised data requirement, and 

whether there are other elements that 

should also be included to ensure the 

proper use and application of the 

products. 

(6) Environmental fate information. 

The Agency is proposing to request any 

known and available measured data and 

supporting documentation on the 

persistence, bioconcentration factor, 

bioaccumulation factor, and 

biodegradability of the product and all 

of its components. The Agency 

currently has no restriction on use of 

persistent bio-accumulative products. 

The Agency considered requirements 

using existing testing protocols and 

modeling approaches to establish 

thresholds for listing based on 

bioconcentration factors (BCF) or 

bioaccumulation factors (BAF). These 

factors offer ratios of the concentration 

of a particular chemical in a biological 

tissue per concentration of that 

chemical in water surrounding that 

tissue, or in the environment 

respectively. The Agency considered a 

tiered testing approach, where the 

submitter would provide known BCF/

BAF information for listing purposes, 

but would also be required to provide 

testing based on application rates 

authorized for use. That is, the lower 

application rates would only require 

existing information or the use of 

existing EPA models, while higher rates 

would require additional testing of fish, 

bivalves, and earthworms, as needed. 

Similarly, there are no restrictions on 

the use of environmentally persistent 

products. The Agency considered 

requiring the submitter to use 

estimation techniques/models, such as 

the EPA model EPI SuiteTM, which 

estimates environmental fate properties 

(breakdown in water or air, etc.) that can 

indicate where a chemical will go in the 

environment and how long it will stay 

there. A tiered testing approach for 

larger quantity/duration spills as 

discussed above for bioconcentration 

and bioaccumulation was also 

considered. 

EPA believes environmental fate 

information is necessary to inform the 

OSCs when authorizing these products 

for use, given the potential for their 

extended use in significant quantities. 

However, given that the Agency can 

estimate these factors, it is only 

proposing to require that available 

information or data be submitted on the 

product rather than specific product 

testing, as specific product testing for 

these factors can add significantly to the 

testing cost for each product. The 

Agency requests comment on whether 

testing for products’ bioconcentration, 

bioaccumulation and biodegradation 

should be required for listing purposes. 

Additionally, the Agency requests 

comment on whether thresholds for BCF 

and BAF should be established for 

listing a product on the Schedule. 

(7) New physical/chemical properties 

and removal of the incorporation by 

reference of the measurement 

standards. The Agency is proposing to 

add three new elements to the physical/ 

chemical property requirements: 

Physical state and appearance; vapor 

pressure; and particle size for solid 

components. The Agency believes these 

basic data requirements will provide 

added context when evaluating the 

products for listing determinations. 

These, in combination with the other 

general product information 

requirements, will assist the Agency in 

evaluating the expected product 

behavior, and the process through 

which it would affect the oil when used 

in the intended water and/or shoreline 

environment. Additionally, the Agency 

is proposing to remove the current 

incorporation by reference of specific 

standards to determine physical/

chemical properties, and replacing this 

with a requirement for a citation of the 

standard methodology used to 

determine these values. EPA believes 

that citing the standard methodology 

used to determine the required values is 

sufficient in lieu of specifying 

commonly recognized standard 

methodologies. The Agency believes it 

is appropriate to make this change given 

the new requirements for accredited 

laboratories to conduct testing. 

(8) Chemical Abstract Service (CAS) 

Registry Numbers for each component 

in a product. The CAS Registry is a 

collection of information covering a 

wide variety of substances identified 

from the scientific literature since 1957. 

CAS Numbers serve as an international 

resource for substance identifiers and 

are used by scientists, industry, and 

regulatory bodies because it can be 

validated quickly and reliably. This will 

assist the Agency in better 

characterizing a product’s components 

and assessing its specific process for 

affecting the oil prior to listing on the 

Schedule. 

(9) Certification that bioremediation 

agents do not contain, at levels that 

exceed the National Ambient Water 

Quality Criteria lowest density value, 

bacterial, fungal, viral or opportunistic 

pathogens. While providing information 

on these product contaminants is 

currently required for bioremediation 

agents, there are no threshold levels for 

product listing; a positive result for any 

of the above pathogens may raise 

concern, but would not prevent the 

product from being listed on the 

Schedule. The proposed requirement 

that these contaminants not exceed the 

National Ambient Water Quality Criteria 

lowest density value is intended to 

provide information for listing decisions 

that ensure the use of bioremediation 

agents that will not result in exceeding 

established water safety levels. The 

Agency believes that this information is 

necessary to determine if a product is 

suitable for listing, particularly for 

bioremediation agents, which could 

potentially be used at recreational 

beaches. The Agency requests 

comments on whether it should 

establish listing thresholds for products 

based on this criteria, and whether the 

levels selected for certification are 

appropriate for this application. 

(10) Certification that the product 

does not contain levels that exceed the 

National Water Quality Standards 

lowest acute value for aquatic life of the 

following contaminants: Arsenic, 

cadmium, chromium, copper, lead, 

mercury, nickel, zinc, or any other 

heavy metal reasonably expected to be 

in the product; cyanide; chlorinated 

hydrocarbons; pesticides; 

polychlorinated biphenyls (PCBs); and 

polynuclear aromatic hydrocarbons 

(PAHs). Providing information (i.e., 

upper limit/concentration, detailed 

analytical methods, and sample 

preparation) on most of these 

contaminants is currently required for 

all products, with no established 

threshold levels for product listing. The 

Agency will continue to require 

information on the methodology and the 

data and supporting documentation 

used to determine the levels of these 

contaminants in a product. The Agency, 

however, will not specify what 

analytical testing method the submitter 

should use to make these 

determinations, as it currently does for 

chlorinated hydrocarbons, allowing the 

submitter flexibility in testing their 

product. Additionally, the Agency is 

proposing to require data on several 

new contaminants: Pesticides, PCBs, 

and PAHs. The Agency’s concern with 

pesticides as contaminants is mostly 

due to their potential use on organic 

sorbents (e.g., peat moss, corn cobs, and 

cellulose fibers). The concern for PCBs 

is for their toxicity and classification as 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
3402 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

33http://www.epa.gov/dfe/. 

34http://www.epa.gov/oem/docs/oil/ncp/

notebook.pdf. 

persistent organic pollutants, having 

toxic effects such as endocrine 

disruption. PAHs are potent 

atmospheric pollutants, of concern 

because some compounds have been 

identified as carcinogenic, mutagenic, 

and teratogenic. The proposed threshold 

requirements for all of these 

contaminants is intended to provide 

information for listing decisions that 

ensure the use of any product will not 

result in exceeding established water 

safety levels. The Agency requests 

comments on whether it should 

establish a listing threshold for products 

based on these criteria, and whether the 

levels selected for certification are the 

appropriate levels for this application. 

The Agency also requests comments on 

whether there are any other 

contaminants that should be included 

for evaluation of a product prior to 

listing. 

(11) Removal of the requirement for 

laboratories performing the efficacy and 

toxicity testing for products to have 

prior experience specific to the required 

methodology in lieu of recognized 

national or international accreditations. 

Currently, laboratories performing 

testing for products to be submitted for 

listing consideration are required to 

document previous experience with the 

specific testing methodologies in 

Appendix C to part 300. The Agency 

believes it is more appropriate to require 

that laboratories be nationally or 

internationally accredited. Accredited 

laboratories are expected to be capable 

of following a prescribed testing 

protocol and good general practices, 

providing assurance that the test results 

will be reliable. Therefore, the Agency 

is proposing to remove the requirement 

for laboratories to have previous 

experience specific to the 

methodologies in Appendix C, and 

instead require that the laboratories 

hold accreditations from recognized 

national or international organizations. 

National and international accreditation 

organizations include, for example, the 

International Organization for 

Standardization (ISO), and the 

Laboratory Accreditation Bureau 

(recognized in the US through the 

National Cooperation for Laboratory 

Accreditation (NACLA) and the 

International Laboratory Accreditation 

Cooperation (ILAC)). The ISO 17025, 

Laboratory Competence standard, 

identifies high technical competence 

and management system requirements 

to guarantee laboratory test results and 

calibrations are consistently accurate. 

NACLA is a national voluntary 

organization of regulators, accreditation 

bodies and laboratories cooperatively 

working towards standardization of 

laboratory accreditations throughout the 

industry; ILAC is the international 

counterpart collaboration of laboratory 

and inspection accreditation bodies. 

Established to ensure that laboratories 

are subject to oversight by an 

authoritative body, accreditation 

organizations have been evaluated by 

peers as competent and have signed 

arrangements to enhance the acceptance 

of products and services. Because 

interested parties can have confidence 

in the test results and certifications 

provided by accredited laboratories, the 

Agency is proposing to amend the 

laboratory requirement and believes that 

having no prior experience with a 

specific methodology should not 

disqualify a laboratory that has been 

accredited by an appropriate 

authoritative body. However, the 

Agency reserves the right to not accept 

particular lab data should EPA find 

cause to doubt the quality and integrity 

of the work. EPA also reserves the right 

to conduct its own testing of any 

product. 

(12) Estimated annual product 

production volume, average and 

maximum amounts that could be 

produced per day, and time frame 

needed to reach maximum production 

rate (days). While there is currently no 

requirement for production capability 

information, the Agency believes it is 

important for the OSCs and responders 

to have this information. The 

availability of a product may impact 

decisions of authorization of use, 

depending on inventory or production 

capabilities. This would prove to be of 

key importance, for example, in the 

event of a major environmental disaster 

(e.g., a SONS event). 

(13) Recognition received from EPA’s 

Design for the Environment (DfE). EPA’s 

Design for the Environment (DfE) 33

works in partnership with industry, 

environmental groups, and academia to 

reduce risk to people and the 

environment by finding ways to prevent 

pollution. DfE evaluates human health 

and environmental concerns associated 

with traditional and alternative 

chemicals and processes in a range of 

industries in order to select safer 

chemicals and technologies. DfE focuses 

its review of formulation ingredients on 

key environmental and human health 

characteristics of concern within 

functional classes. This allows 

formulators to use those ingredients 

with the lowest hazard in their 

functional class, while still formulating 

high-performing products. The DfE label 

means that EPA scientists have 

evaluated every ingredient in the 

product to ensure it meets DfE’s 

stringent criteria. Products that meet the 

DfE criteria are safer chemical choices. 

In an effort to encourage the 

development and use of safer 

technologies, the Agency is proposing a 

requirement for the submitter to identify 

products that have met and can be 

labeled DfE certified as part of the 

general information, and would include 

this information in the NCP Product 

Schedule Technical Notebook.34 This 

Technical Notebook presents 

manufacturer’s summary information on 

the conditions under which each 

product is recommended to be used, 

and is a source of information for the 

OSC in the event of a response. 

(14) International product 

certifications, testing or use data 

informing the performance capabilities 

or environmental benefits of the 

product. The Agency believes that any 

additional data available from other 

countries may help identify the benefits 

or concerns for the listing and/or the 

authorization of use of a product. The 

Agency, however, is not proposing any 

specific listing criterion or threshold 

associated with this broad information 

request, as some products (particularly 

new formulations) may not have any of 

this additional data available. 

(b) Dispersant Testing and Listing 

Requirements 

The Agency is proposing revisions to 

the efficacy and toxicity testing 

protocols, as well as establishing new 

thresholds for listing dispersants on the 

Schedule in § 300.915(b). The Agency 

proposes to define dispersants as 

typically mixtures of solvents, 

surfactants, and additives that promote 

the formation of small droplets of oil in 

the water column by reducing the oilwater interfacial tension. These droplets 

are driven into the water column by 

wave action. Emergency response 

personnel need to know whether a 

dispersant or any other type of chemical 

or biological agent on the Schedule 

could have negative environmental 

impacts relative to the oil before 

decisions are made about its use in a 

particular oil discharge situation. 

Consequently, it is essential to consider 

comparative information about the 

efficacy and the toxicity of these 

products. The proposed revisions are in 

response to concerns not only for an 

increase in the frequency of planning for 

the use of these agents, but also for their 

potential use in large quantities, such as 

when responding to oil discharges from 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 3403 

35 Venosa, Albert D., National Risk Management 

Research Laboratory, US EPA; Sorial, George A., 

Department of Civil & Environmental Engineering, 

University of Cincinnati; King, Dennis W., Statking 

Consulting; Round-Robin Testing of a New EPA 

Dispersant Effectiveness Protocol, International Oil 

Spill Conference, 2001. 

oil tanker accidents and offshore well 

blowouts, as evidenced during the 

Deepwater Horizon incident in 2010. 

(1) Dispersant Efficacy 

Current Requirements: The current 

NCP Subpart J requires dispersants to be 

tested for saltwater efficacy in order to 

determine listing eligibility on the 

Schedule. Dispersant efficacy is tested 

following the Swirling Flask Test (SFT) 

listed in Appendix C to part 300 of the 

NCP. This protocol was developed by 

Environment Canada to provide a 

relatively rapid and simple testing 

procedure for evaluating dispersant 

efficacy (i.e., the percentage of oil that 

is dispersed). The procedure places 

seawater, oil, and a dispersant into an 

Erlenmeyer flask, which is then placed 

on a shaker table for a specified period 

of time. The flask is modified by the 

addition of a side spout attached to the 

bottom of the flask, which allows the 

analyst to pour off dispersed oil from 

the bottom into a collection vessel for 

extraction and measurement. After 20 

minutes, a sample of water is poured off 

and chemically analyzed for dispersed 

oil. For products to be listed, they must 

attain an efficacy value of 45 percent or 

greater average dispersion efficacy of 

two different crude oils (South 

Louisiana Crude (SLC) and Prudhoe Bay 

Crude (PBC)) at room temperature (20– 

23 degrees Celsius (°C)). 

Proposed Revisions: The Agency 

proposes to change the testing protocol 

for measuring efficacy and adopt the 

Baffled Flask Test (BFT) as the testing 

protocol for dispersant efficacy. The 

new BFT procedure incorporates a 

redesign of the testing flask by 

eliminating the side arm, incorporating 

baffles in the wall of the flask, and 

adding a stopcock at the bottom, which 

improves reproducibility in the hands of 

different operators. This protocol has 

undergone extensive peer review 35 and 

has been tested in several laboratories, 

providing reproducible and repeatable 

results. The Agency also proposes 

revisions to the efficacy listing criteria 

for dispersants to be listed. Specifically, 

the dispersant must demonstrate that 

the lower 95% confidence level (LCL95) 

of six replicate flasks meets the new 

proposed efficacy listing criteria at two 

test temperatures. New test oils 

representing a wider range of 

characteristics are also proposed for this 

protocol: Alaska North Slope (ANS) and 

Intermediate Fuel Oil (IFO–120) were 

tested for this proposal. Both oils are to 

be tested at two temperatures: 5 °C and 

25 °C. Finally, based on the ANS and 

IFO–120 testing, the Agency proposes 

that dispersants considered for listing 

must demonstrate that they attain all of 

the following dispersant effectiveness 

(DE) values: 

• ANS at 5 °C: DELCL95 ≥70%. 

• ANS at 25 °C: DELCL95 ≥75%. 

• IFO–120 at 5 °C: DELCL95 ≥55%. 

• IFO–120 at 25 °C: DELCL95 ≥65%. 

The Agency tested eight of the 

dispersants currently listed on the 

Schedule. Three of the eight dispersants 

clearly differentiated themselves from 

the other five dispersants for having the 

best DELCL95 efficacy results; they would 

meet all the proposed thresholds. For 

the next best dispersant tested, the 

results were substantially lower than 

those in the top group and would not 

meet all the thresholds proposed today. 

This natural break in the results 

provided the Agency with the basis for 

the proposed threshold criteria. The 

Agency is also proposing to replace the 

SLC and PBC test oils currently used for 

efficacy testing with two other oils that 

represent a wider range of 

characteristics. The proposal is based on 

the results of tests using ANS and IFO– 

120 oils with the new protocol. In 

proposing two new oils for efficacy 

testing, the Agency is seeking to ensure 

that the efficacy testing uses oils that 

represent a wider range of oil gravities 

throughout the different geographic 

locations in the country where 

dispersants might be used. The oils 

selected should exhibit sufficiently 

different characteristics to produce 

results that have statistically significant 

variation between them. The proposal is 

to replace the SLC and PBC oils, both 

of which were light oils, with a range of 

light-to-medium, and heavier oils. The 

light-to-medium gravity ANS pipeline 

blend and the heavier refined product, 

IFO–120 were selected for testing the 

protocol in this proposal. The current 

protocol, testing 4 replicates of both the 

SLC and the PBC oils and combining 

their results, provided one threshold 

criterion after determining that each of 

the oils produced statistically similar 

results. In contrast, the efficacy test 

results between the ANS and the IFO– 

120 showed statistically significant 

differences at each temperature. The 

Agency believes the use of ANS and 

IFO–120, or similar oils that represent a 

wider range of oil gravities, will provide 

better information on the efficacy of the 

products when used on different types 

of oils. 

Additionally, the Agency is proposing 

that efficacy testing be conducted at two 

different temperatures, 5 °C and 25 °C, 

rather than at an ambient temperature 

range of 20–23 °C as currently required. 

The Agency recognizes the current and 

future interest in arctic and deepwater 

drilling, and the continued oil 

production in the southern, more 

tropical areas of the country. Given the 

potential range of locations where 

dispersants may be used, the Agency 

believes it is appropriate to have 

products tested at temperatures that 

would reflect that range. These 

temperatures are intended to capture 

dispersant use scenarios in a wide range 

of geographic locations and under 

different temperatures that may occur in 

the same geographical location (such as, 

for example, the deep sea and surface 

water in the Gulf of Mexico, where the 

temperatures are typically 5 and 25 °C, 

respectively). 

The Agency is also proposing to 

replace the current SFT with the BFT, 

which is designed to be more 

representative of moderately turbulent 

sea conditions where dispersants are 

more likely to be successful when used. 

The revised testing protocol improves 

test repeatability and reproducibility 

within and between laboratories, as well 

as greatly reduces both the inherent 

error of the method and the human error 

associated with the current SFT, as 

discussed below. In addition, reporting 

the test results in terms of the product’s 

LCL95 accounts for between- and withinlaboratory error variability and the 

inherent error of the method. Only one 

number is reported compared to a mean 

and standard deviation, as the variation 

has already been subtracted in the 

reported number. Specifically: 

• The new baffled trypsinizing flask 

design, fitted with a glass stopcock 

positioned at the bottom side, promotes 

less manipulation that could result in 

erroneous re-suspension of nondispersed oil, as in the SFT. The resuspension of oil when using the SFT 

test protocol was a major source of error. 

In the SFT, the flask has a side arm 

spout, requiring the analyst to pick up 

the flask and pour the contents out 

manually. Through that action, resuspension of the dispersed oil can 

easily take place, leading to potentially 

erroneous results. In contrast, in the 

BFT, the flask contains a stopcock at the 

bottom, so the analyst need only open 

the stopcock to drain the contents from 

the flask without the potential of 

remixing or re-suspending the dispersed 

oil. 

• The BFT provides more turbulent 

mixing and better enables more 

reproducible and repeatable dispersant 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
3404 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

36 Venosa, A. D., D. W. King, and G. A. Sorial. 

2002. The Baffled Flask Test for Dispersant 

Effectiveness: A Round Robin Evaluation of 

Reproducibility and Repeatability. Spill Sci. & 

Technol. Bulletin 7(5–6):299–308. 

37Sorial, G. A., A. D. Venosa, K. M. Miller, E. 

Holder, and D. W. King. 2004a. Oil Spill Dispersant 

Effectiveness Protocol—Part I Impact of Operational 

Variables. ASCE. J. Env. Eng. Div., 130(10):1073– 

1084. 

38Sorial, G. A., A. D. Venosa, K. M. Miller, E. 

Holder, and D. W. King. 2004b. Oil Spill Dispersant 

Effectiveness Protocol—Part II Performance of the 

Revised Protocol. ASCE ASCE. J. Env. Eng. Div., 

130(10):1085–1093. 

39USEPA 2002a Methods for Measuring the 

Acute Toxicity of Effluents and Receiving Waters to 

Freshwater and Marine Organisms, Fifth edition. 

(Acute Methods Manual), Office of Water, 

Cincinnati, OH. EPA–821–R–02–012. 

40USEPA 2002b. Short-term Methods for 

Estimating the Chronic toxicity of Effluents and 

Receiving Waters to Marine and Estuarine 

Organisms, Third Edition. (Saltwater Chronic 

Methods manual). Office of Water, Cincinnati, OH. 

EPA–821–R–02–014. 

action than the SFT. The mixing energy 

within the flask is higher and, as a result 

of this increased mixing energy, better 

dispersion is possible. Turbulence is 

needed for the proper mixing of 

dispersant and oil and for producing the 

sheer forces needed to create the small 

droplet sizes with high surface area-tovolume ratio that promote the effective 

dispersion of the oil into the water 

column. The BFT provides such mixing 

and better enables more repeatable and 

reproducible dispersant effectiveness 

than the SFT. The BFT was tested 

extensively in a nine-participant roundrobin inter-laboratory calibration test on 

six commercial dispersant products.36

In addition, based on the mixing energy 

that can be achieved using the new 

baffled flask, the Agency believes a 

higher efficacy threshold is warranted. 

As a result of this increased mixing 

energy, better dispersion is realized 

under conditions more realistic of wave 

action in the sea. 

• The variability both between 

analysts and within analysts is 

substantially lower for the BFT 

compared to the SFT, as measured by 

the coefficient of variation (CV). The CV 

is defined as the standard deviation 

divided by the mean and is expressed in 

terms of percent; the higher the CV, the 

greater the variability.37 38

The Agency considered establishing 

listing thresholds for efficacy based on 

the types of oil. The Schedule could list 

sub-categories of dispersants based on 

gravities of the oil (i.e., light-medium or 

heavy), so that a dispersant would only 

be authorized for use on oils that fall 

within the range for which it tested 

effective. Similarly, the Schedule could 

list dispersants based on temperature, 

allowing a dispersant to be authorized 

for use only at the temperature for 

which it tested effective. However, 

determining ranges or definitions for 

when oil changes from light to medium 

or heavy, is challenging because they 

may be affected by a number of external 

factors, including temperature. 

Likewise, listing dispersants based on 

temperature would require an 

additional degree of complexity to the 

authorization for use, as the 

temperatures may change drastically in 

some geographical regions affected by 

the same oil discharge. Even within 

more stable geographical regions, there 

may be variations at the time of an oil 

discharge that could affect the decision 

to use a dispersant stockpiled for a 

different temperature range. While these 

more specific listing approaches would 

provide more information on effective 

product choices, the Agency is 

concerned about how such specific 

listing approaches may contribute to 

OSC confusion in an emergency, the 

cost of stockpiling multiple types of 

dispersants, or the immediate 

availability of the appropriate 

dispersant in an emergency. 

Furthermore, the Agency is proposing 

revisions to Subpart J to authorize RRTs 

to request supplementary testing and 

information to provide greater flexibility 

in tailoring testing conditions to address 

area- and site-specific concerns. Given 

these factors, the Agency believes that it 

is appropriate that only those 

dispersants that achieve efficacy for 

both types of oils and at both 

temperatures be listed. Listing only the 

products that achieve efficacy for both 

types of oils at both temperatures would 

demonstrate a wide range of efficacy for 

the product, and a single listing would 

facilitate authorizing their use during a 

response action. The Agency requests 

comments on this approach. 

(2) Dispersant Toxicity 

Current Requirements: The current 

NCP Subpart J requires dispersants to be 

tested for toxicity to saltwater species. 

This information is available to the OSC 

for their consideration in authorizing 

dispersant use. Dispersant toxicity is 

tested following the protocols in 

Appendix C to part 300 of the NCP. The 

standard toxicity test for dispersants 

involves exposing two saltwater species, 

the inland silverside fish (Menidia 

beryllina or M. beryllina) and the mysid 

shrimp (Americamysis bahia or A. 

bahia), to five concentrations of the test 

product and No. 2 fuel oil, alone and in 

a 1:10 mixture of product to oil. 

Reference toxicity tests are conducted 

using dodecyl sodium sulfate (DSS) as 

a reference toxicant. The test length is 

96 hours for M. beryllina and 48 hours 

for A. bahia. The concentration of test 

product causing 50% lethality to the test 

organisms (LC50) is calculated at the end 

of the exposure period. 

Proposed Revisions: The Agency 

proposes to revise the toxicity testing 

requirements for dispersants, including 

the testing protocol and the use of the 

test results. The proposal would require 

acute toxicity testing for the dispersant 

alone, and the dispersant mixed with 

both oils used for efficacy testing; the 

proposal is based on the ANS and IFO– 

120 oils. While the Agency currently 

provides the toxicity testing results to 

the OSC to assist in authorization of use 

determinations, it is proposing to use 

these testing results to determine 

eligibility for listing on the Schedule. 

Specifically, the Agency is proposing 

to require evaluations of dispersant 

toxicity using acute toxicity tests 

following existing USEPA effluent 

testing guidelines,39 40 modified for use 

with dispersant product or dispersant 

product/oil mixtures, as detailed in 

Appendix C to part 300. Measured 

toxicity values for dispersant product 

and dispersant product/oil mixtures are 

proposed to include static acute toxicity 

tests using A. bahia and M. beryllina. 

Developmental toxicity using a sea 

urchin assay, and sub-chronic effects 

using A. bahia and M. beryllina are also 

proposed to be conducted, but with 

dispersant product only. The Agency is 

proposing the following toxicity 

thresholds for listing dispersants on the 

Schedule: 

• Lethal concentration for 50% of the 

test species (LC50) at the lower 95% 

confidence interval for all acute toxicity 

tests greater than 10 ppm; 

• Inhibition concentration for 50% of 

the test species (IC50) at the lower 95% 

confidence interval greater than 10 ppm; 

• No Observed Effect Concentration 

(NOEC) equal to or greater than 1 ppm 

for sub-chronic toxicity. 

Test Oils and Oil Acute Toxicity 

Values. The Agency proposes to replace 

the No. 2 fuel oil currently used for 

toxicity testing with two test oils that 

better represent a wider range of 

characteristics and that may be 

encountered during an incident. The 

proposal is based on ANS and IFO–120, 

as previously discussed. In addition to 

making the test oils consistent with the 

dispersant efficacy tests, testing oils of 

different gravities also provides a better 

estimation of dispersant/oil toxicity 

associated with differing oil 

constituencies, and ultimately a better 

representation of the potential overall 

toxicity of a product. 

The Agency proposes to conduct the 

oil-only acute toxicity tests for the two 

reference oils, with both A. bahia and 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 3405 

41http://www.epa.gov/oppefed1/ecorisk_ders/

toera_analysis_eco.htm#Ecotox. 

42The modified protocol is based on a variable 

dilution modification of the Chemical Response to 

Oil Spills: Ecological Research Forum (CROSERF) 

testing protocol; Aurand, D. and G. Coelho 

(Editors). 2005. Cooperative Aquatic Toxicity 

Testing of Dispersed Oil and the ‘‘Chemical 

Response to Oil Spills: Ecological Effects Research 

Forum (CROSERF).’’ Ecosystem Management & 

Associates, Inc. Lusby, MD. Technical Report 07– 

03. 

43Barron, MG, Ka’aihue L. 2003. Critical 

evaluation of CROSERF test methods for oil 

dispersant toxicity testing under subarctic 

conditions. Mar Pollut Bull 46:1191–1199. 

44Hemmer, MJ, Barron, MG, Greene, R. 2011. 

Comparative toxicity of eight oil dispersants, 

Louisiana sweet crude oil (LSC) and chemically 

dispersed LSC to two aquatic species. Environ 

Toxicol Chem, 30: 2244–2252. 

45USEPA 2002a Methods for Measuring the 

Acute Toxicity of Effluents and Receiving Waters to 

Freshwater and Marine Organisms, Fifth edition. 

(Acute Methods Manual), Office of Water, 

Cincinnati, OH. EPA–821–R–02–012. 

46USEPA 2002b. Short-term Methods for 

Estimating the Chronic toxicity of Effluents and 

Receiving Waters to Marine and Estuarine 

Organisms, Third Edition. (Saltwater Chronic 

Methods manual). Office of Water, Cincinnati, OH. 

EPA–821–R–02–014. 

47CROSERF was established as a working group 

of industry, government, and university scientists to 

coordinate and disseminate research on chemical 

oil spill dispersants. CROSERF participants 

developed aquatic toxicity testing protocols during 

1994 to 2000 with the foremost objective of 

standardizing test methods and reducing interlaboratory variability. 

48USEPA 1996. Short-term Methods for 

Estimating the Chronic Toxicity of Effluents and 

Receiving Waters to West Coast Marine and 

Estuarine Organisms. EPA/600/R–95/136. 

49USEPA 2002b. Short-term Methods for 

Estimating the Chronic Toxicity of Effluents and 

Receiving Waters to Marine and Estuarine 

Organisms, Third Edition. (Saltwater Chronic 

Methods manual). Office of Water, Cincinnati, OH. 

EPA–821–R–02–014. 

M. beryllina, and provide this data for 

comparisons to dispersant and 

dispersant-oil mixture acute toxicity 

tests. EPA will make all of the reference 

oil toxicity test results available to the 

public on its Web site, including raw 

data and calculated median LC50 values. 

By providing this information, the 

Agency is reducing the number of 

required toxicity tests the submitter 

would need to conduct. Alternatively, 

the Agency considered requiring 

submitters to conduct the oil acute 

toxicity testing as it would provide an 

opportunity to detect anomalies in the 

submitted data. The Agency is 

requesting comments on whether the 

submitter should be required to conduct 

the oil-only acute toxicity testing for the 

two test oils. 

Dispersant and Dispersant-Oil Acute 

Toxicity Threshold. Using the EPA 

toxicity classification scheme,41 LC50

values ranging from 10 ppm to 100 ppm 

are classified as slightly toxic and above 

100 ppm substances are considered 

acutely nontoxic to aquatic organisms. 

For both M. beryllina and A. bahia, the 

Agency is proposing as the threshold 

value the lower bound of the LC50 95% 

confidence interval (CI) greater than or 

equal to 10 ppm for all toxicity tests to 

qualify a dispersant to be listed on the 

Schedule. The rationale for using the 

lower bound of the CI is that the CI 

should not contain any values less than 

or equal to 10 ppm since theoretically, 

the LC50 can fall anywhere within the 

CI. By using the lower CI, the Agency 

is providing a conservative decision 

criterion for acute toxicity, and by 

proposing a greater than or equal to 10 

ppm threshold level, it is establishing 

an adequate safety margin without being 

overly restrictive. 

Dispersant-Oil Mixture Acute Toxicity 

Protocol. The Agency is proposing to 

substitute the existing preparation 

procedure for the dispersant-oil mixture 

(DOM) in Appendix C to Part 300, 

Section 3 method for the preparation 

procedure for dispersant-oil mixture 

using a modified protocol 42 first 

described by Baron and Ka’aihue 43 and 

fully described by Hemmer et al.44

These new modified procedures for 

preparation of the chemically enhanced 

water accommodated fractions 

(CEWAFs) of dispersant-oil mixtures are 

used to make exposure solutions. 

Evaluations of the dispersant-oil 

mixture toxicity using acute toxicity 

tests follow existing EPA effluent testing 

guidelines,45 46 modified for use with 

these exposure solutions and are 

detailed in Appendix C to part 300. EPA 

proposes to modify the variable loading 

preparation procedure described in 

Chemical Response to Oil Spills: 

Ecological Research Forum 

(CROSERF) 47 to a variable dilution 

procedure to standardize the oil-towater ratio and provide a consistent 

chemical concentration in a test series. 

Additionally, the modified preparation 

procedure provides economies in 

analytical costs by reducing the need to 

analyze the composition of every tested 

concentration. Chemical analysis for the 

total petroleum hydrocarbon (TPH) 

concentration of the CEWAF stock 

solution is required. 

Sea Urchin Developmental Assay. The 

Agency is proposing to require a sea 

urchin developmental assay (also 

referred to as an embryogenesis assay) to 

assess the potential for a dispersant 

product to cause adverse effects on the 

developmental process. During the Deep 

Water Horizon spill event, the possible 

adverse effects of oil dispersants on the 

developmental processes of fish and 

invertebrate species were identified as 

critical issues of concern. By 

incorporating the sea urchin 

developmental assay, the Agency is 

using it as a sensitive surrogate test for 

pelagic early life stages. This assay 

would employ an existing EPA test 

protocol 48 routinely used in effluent 

testing. As suggested for the dispersant 

acute toxicity test criteria with A. bahia 

and M. beryllina, the Agency is 

proposing as the threshold value the 

lower bound of the developmental IC50

95% confidence interval greater than or 

equal to 10 ppm. For this test, the IC50

is defined as the concentration of 

dispersant that inhibits the development 

of 50% of exposed embryos. As 

described above for acute toxicity levels, 

the Agency is adopting a similar 

rationale for IC such that IC50 values 

ranging from 10 ppm to 100 ppm are 

considered to cause slight adverse 

effects on the developmental process, 

and above 100 ppm substances are 

considered to cause no adverse effects. 

By using the lower CI the Agency is 

providing a conservative decision 

criterion for developmental toxicity, and 

by proposing a greater than or equal to 

10 ppm threshold level it is establishing 

an adequate safety margin without being 

overly restrictive. 

Sublethal/Subchronic Studies. The 

Agency has limited information 

concerning the possible sublethal effects 

of dispersants currently listed on the 

Product Schedule. The Agency is 

proposing requirements for subchronic 

assays (duration approximately 7 days) 

to be performed with A. bahia and M. 

beryllina following established EPA 

short-term methods for estimating 

chronic toxicity of effluents.49 While the 

Agency considered requiring longerterm tests, it believes the 7-day 

subchronic tests are reasonable 

alternatives for estimating chronic 

toxicity. This information would also be 

of value as guidance to regional 

responders and OSC’s on possible 

adverse effects on survival and growth 

of larval fish and invertebrates caused 

by longer-term exposure to dispersants. 

The Agency is proposing a NOEC equal 

to or greater than 1 ppm listing 

threshold level for sub-chronic effects. 

This threshold level provides a tenfold 

safety factor from the proposed acute 

toxicity threshold values. The tenfold 

safety factor is a common practice in 

ecological risk assessment and thus the 

Agency believes it provides an adequate 

safety margin without being overly 

restrictive. The Agency is requesting 

comment on whether it should consider 

longer-term tests (e.g., early life stage 

tests), which may be more relevant to 

sublethal effects caused by longer 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
3406 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

50Fingas, M., (Ed.), 2011, Oil Spill Science and 

Technology, Gulf Professional Publishing, pp. 513– 

518. 

51 Koran, K.M., Venosa, A.D., Luedeker, C.C., 

Dunnigan, K., Sorial, G.A., 2009. Development and 

Testing of a New Protocol for Evaluating the 

Effectiveness of Oil Spill Surface Washing Agents. 

Mar. Pollut. Bull., 58: 1903–1908. 

duration exposure to low concentrations 

of a dispersant product. 

Alternative Options 

In addition to the criteria discussed 

above, the Agency considered 

calculating a toxicity threshold based on 

the ratio of the LC50 of oil-alone to the 

LC50 of the dispersant-oil mixture for M. 

beryllina and A. bahia to assist in 

comparing the relative toxicity of crude 

oil to chemically dispersed oil. A ratio 

of less than or equal to 1 would indicate 

the toxicity of the dispersant-oil mixture 

is less than or equal to the toxicity of the 

oil-alone. The Agency considered 

whether this ratio should be used as a 

criterion for inclusion of dispersants on 

the Schedule or as guidance to 

emergency responders. Using a less than 

or equal to 1 ratio as a guideline would 

afford an adequate safety margin 

without being overly restrictive. While 

the ratio would provide a simple, 

interpretable, and easily justifiable 

value for determining acceptable 

toxicity levels of dispersant-oil 

mixtures, it would not be specific to oils 

in particular discharge situations. The 

Agency is requesting comment as to 

whether such a value should be 

calculated, and if so, whether it should 

be an additional listing criterion, or 

provided as information for the 

responders to consider in authorizing 

dispersant use. 

The Agency also considered including 

geographically or ecologically 

representative species in the testing 

protocol. The Agency believes, however, 

that this issue is addressed by the 

proposed revisions to the supplemental 

testing and information requirements in 

section 300.910(g), with the decisions of 

testing geographically and ecologically 

representative species left to the 

discretion of the RRTs. While inclusion 

of species from different phyla and 

habitats would provide useful and 

important information on possible 

adverse effects of dispersant products 

and dispersed oil, the proposed testing 

protocols would need to be modified 

and validated. Further, the Agency is 

concerned about balancing the time and 

cost associated with the development of 

these tests on the part of the submitter 

rather than on the end users. 

The Schedule currently requires no 

specific toxicity or efficacy tests for 

subsea dispersant listing or 

authorization of use. While the 

differences in toxicity values and 

efficacy may be affected by application 

in subsea environments, the Agency 

believes that the proposed requirements 

establish an adequate baseline for listing 

dispersants on the Schedule and for 

authorizing their use by responders in 

case of an incident. The Agency is 

addressing these concerns by proposing 

new provisions for dispersant 

monitoring for all subsea use, and 

requests comments on alternative 

testing and listing approaches to 

specifically address subsea concerns. 

(3) Limitations of Use 

The Agency is proposing a 

conditional use listing for dispersants. 

The proposal specifies that dispersants 

may only be used in saltwater 

environments. Dispersants are typically 

designed and traditionally used for 

responding to oil discharges in 

saltwater. In general, the effectiveness of 

dispersants decreases as the salinity of 

the water decreases, given the same 

hydrophilic-lipophilic balance, and the 

effectiveness is minimal in freshwater 

environments. Surfactants, the main 

active ingredient in dispersants, sustain 

oil droplets in water by orienting the 

lipophilic side of its molecule in the oil 

and the hydrophilic side in the water. 

The hydrophilic side of the surfactant is 

generally more soluble in waters with 

higher salinity values, causing the oil 

droplets to be more stable in saline 

water environments. In waters with no 

salinity, many dispersants have shown 

a very low effectiveness or are 

sometimes completely ineffective.50

The Agency is also concerned with 

using dispersants in freshwater 

environments because of the limited 

dilution typically available as compared 

with the open sea and because of the 

existence of water intakes in rivers, 

streams, and lakes for use in drinking 

water supplies. Using dispersants in 

freshwater has the potential for 

compounding the impacts caused by 

already discharged petroleum products, 

particularly near potable and nonpotable subsurface water intakes. The 

Agency does recognize, however, that as 

a last resort, dispersants may have some 

limited applicability in freshwater. The 

provision for authorization of use under 

§ 300.910(d) would allow for exceptions 

to the prohibition on the use of 

dispersants in freshwater in cases where 

there is an immediate threat to human 

life. The Agency is requesting comment 

on this proposed listing limitation. 

(c) Surface Washing Agent Testing and 

Listing Requirements 

The Agency is proposing to define 

Surface washing agents (SWA) as 

substances that separate oil from solid 

surfaces, such as beaches, rocks, or 

concrete, through a detergency 

mechanism that lifts and floats oil for 

collection and recovery from the 

environment with minimal dissolution, 

dispersion, or transfer of oil into the 

water column. For this agent category, 

the Agency is proposing to revise the 

toxicity testing protocols, to establish 

efficacy testing protocols, and to 

establish both toxicity and efficacy 

listing thresholds in § 300.915(c). The 

proposed revisions respond to concerns 

regarding their frequent use and the 

potential for residual impacts after their 

use. 

(1) Surface Washing Agent Efficacy 

Current Requirements: There are 

currently no efficacy testing 

requirements in the NCP Subpart J for 

surface washing agents to determine 

listing eligibility on the Schedule. 

Proposed Revisions: The Agency is 

developing a laboratory testing protocol 

to evaluate the efficacy of SWAs in 

removing crude oil from a solid 

substrate.51 Currently available efficacy 

testing protocols for these agents are 

concerned with assessing the 

detergency, or cleaning power, of the 

agents by quantifying the physical 

removal of oil from non-vegetative 

substrates as a result of their use. The 

protocols typically involve the 

application of oil to a solid substrate (or 

the use of pre-oiled substrate), 

weathering of the oil on the substrate, 

application of the agent to the oiled 

substrate, a contact period for SWA 

penetration, and washing of the 

substrate with water. The fractions of oil 

removed in the wash water and/or 

remaining on the substrate are 

quantified. Oil removal efficiencies for 

surface washing treatments are typically 

compared to the washing efficiency of 

water without surface washing agents 

(untreated controls). Disadvantages or 

potential sources of error have been 

identified in the existing protocols that 

may not reflect field performance. Of 

concern are, for example, the use of 

substrates (e.g., stainless steel, 

porcelain) with different wetting and 

adhesion properties than natural 

substrates such as sand or gravel; short 

weathering times insufficient for oil 

attachment; and the absence of mixing 

energy during the washing step, which 

may lead to incomplete detachment of 

partially released oil. 

The Agency’s goal is to develop and 

evaluate a new bench-scale testing 

protocol that would provide a standard 

for EPA to use in SWA product 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 3407 

52ASTM Standard Test Method for Evaluating the 

Effectiveness of Cleaning Agents. Designation: 

G122—96 (Reapproved 2008). ASTM International, 

100 Barr Harbour Dr., P.O. Box C–700 West 

Conshohocken, Pennsylvania 19428–2959, United 

States 53Fingas, Merv and Fieldhouse, Ben; ‘‘Surfacewashing Agents or Beach Cleaners’’ (2010). Chapter 

21 Surface-Washing Agents or Beach Cleaners. In 

Oil Spill Science and Technology (p716). London: 

Gulf Professional Publishing. 

54http://water.epa.gov/scitech/methods/cwa/wet/

upload/2007_07_10_methods_wet_disk2_atx1- 

6.pdf. 

55USEPA 2010. http://www.epa.gov/oppefed1/

ecorisk_ders/toera_analysiseco.htm#Ecotox. 

evaluation prior to listing on the 

Schedule. Changes over established 

protocols the Agency considered 

include: Using natural substrates to 

reflect the most commonly impacted 

shoreline material; establishing 

sufficient weathering time to permit 

strong attachment of the oil to the 

substrate surface; fully quantifiable 

approaches with known volumes and 

precise measurements to allow mass 

balance; and a standardized and 

reproducible methodology to minimize 

operator error. PBC oil was used as the 

representative standard reference oil in 

developing the protocol since it had 

previously been selected as one of two 

standard oils for the Agency’s published 

protocols for dispersant and 

bioremediation agent testing. However, 

the Agency is proposing revisions to the 

dispersant and bioremediation testing 

protocols, including replacing the PBC 

reference oil. The protocol being 

developed has not been tested: With the 

IFO–120 or the ANS oils that are 

proposed to be used in the revised 

dispersant efficacy testing protocol; at 

multiple temperatures; or to include 

freshwater systems. The Agency expects 

to develop final recommendations for 

the testing protocol following round 

robin testing after adjusting for the new 

variables. The Agency would propose 

this protocol in the Federal Register 

through notice and comment before 

adopting it as part of Subpart J 

requirements. 

Consequently, because of the 

additional work needed to finalize its 

protocol, the Agency is proposing to 

allow the use of standard recognized 

efficacy testing methodologies for 

surface washing agents. An example of 

such a standard recognized 

methodology is the American Society 

for Testing and Materials (ASTM) 

Standard Test Method for Evaluating the 

Effectiveness of Cleaning Agents.52

Another methodology is Environment 

Canada’s Test Method.53 The capability 

of a particular surface washing agent 

depends upon the application 

procedures and the characteristics of the 

surface being cleaned, such as size, 

shape, and material. The ASTM test 

method in particular covers a procedure 

for evaluating the capability of the 

agents, providing a relatively rough 

surface to which the oil can adhere. The 

Environment Canada method uses a 

stainless-steel ‘trough’ which is placed 

at a specified angle. The target oil is 

placed on an area on the trough. The 

treating agent is then applied in droplets 

to the surface of the oil and after 10 

minutes at 5-minute intervals, rinses of 

water are applied to the trough. After 

drying, the trough is weighed and the 

removal calculated from the weight loss. 

Repeatability is within 5%. The Agency 

is requesting comment on available 

methodologies and its published 

protocol to incorporate as the testing 

protocol for these agents. The Agency 

also requests comment on whether the 

rule should identify the specific 

methodologies to be used until EPA 

develops and adopts a new testing 

protocol for SWA efficacy testing. 

The Agency is also proposing an 

efficacy threshold of 30% in either fresh 

or salt water or both depending on the 

intended product use. This is based on 

the efficacy data published in ‘‘Surfacewashing Agents or Beach Cleaners.’’ 48

Numerous surface washing agent 

products, including several from the 

Schedule were tested using the 

Environment Canada methodology. The 

average efficacy of the surface washing 

agents tested is approximately 30%. The 

Agency requests comments on this 

approach and other efficacy test data 

available. 

(2) Surface Washing Agent Toxicity 

Current Requirements: The current 

NCP Subpart J requires surface washing 

agents to be tested for saltwater species 

toxicity. Surface washing agent toxicity 

is tested following the dispersant 

toxicity testing protocols in Appendix C 

to part 300 of the NCP. 

Proposed Revisions: The Agency is 

proposing revisions to the toxicity 

testing requirements for surface washing 

agents, including the testing protocol. 

While the Agency currently provides 

the toxicity testing results to the OSC to 

assist in authorization of use 

determinations, it is proposing to use 

these toxicity testing results to 

determine listing eligibility on the 

Schedule. 

The proposed revisions to the testing 

protocols for surface washing agents are 

detailed in Appendix C to part 300. The 

proposed acute toxicity test protocol for 

surface washing agents is based on 

EPA’s protocol, Methods for Measuring 

the Acute Toxicity of Effluents and 

Receiving Waters for Freshwater and 

Marine Organisms.54 The Agency 

proposes to require surface washing 

agents be tested for acute toxicity using 

fresh water species Ceriodaphnia dubia 

and Pimephales promelas, or saltwater 

species Americamysis bahia and 

Menidia beryllina, or both, depending 

on the intended product use. The 

concentration of test product causing 

50% lethality to the test organisms 

(LC50) and lower and upper 95% 

confidence intervals (LCI95 and ULCI95) 

are calculated at the end of the exposure 

period. To be listed on the Schedule, 

surface washing agents must 

demonstrate an acute lethal 

concentration for 50% of the test species 

(LC50) at the lower 95% confidence 

interval greater than 10 ppm in either 

fresh or salt water, consistent with the 

acute toxicity thresholds proposed for 

dispersants. EPA’s toxicity classification 

scheme 55 classifies LC50 values ranging 

from 10 ppm to 100 ppm as slightly 

toxic and values above 100 ppm 

substances are considered practically 

nontoxic to aquatic organisms. By 

proposing this threshold level, the 

Agency is establishing an adequate 

safety margin without being overly 

restrictive. The Agency requests 

comments on the proposed acute 

toxicity methods (or any others 

available) and thresholds for surface 

washing agents. 

The Agency is proposing provisions 

for conducting acute toxicity tests with 

dispersant-oil mixtures, but not for any 

other agent, including SWAs. EPA 

believes that non-dispersant products 

are not likely to be used in the same 

quantities or durations as dispersants 

and some may be recovered making a 

requirement to conduct toxicity tests of 

product/oil mixtures unnecessary. 

There may be concerns, however, for 

increased product toxicity because of 

their interaction with the oil. Thus, the 

Agency is requesting comment on the 

need for acute toxicity tests conducted 

with surface washing agents-reference 

oil mixtures. A protocol for preparation 

of product/oil mixtures for toxicity 

testing is available for review in the 

docket. 

(3) Limitations 

The Agency is proposing a 

conditional use listing for SWAs. The 

proposal specifies that these products 

may only be used in those water 

environments for which the product 

was tested and for which it met the 

listing threshold criteria. The Agency 

recognizes that products may yield 

effective results in certain environments 

and not in others. Products that may be 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
3408 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

56Artificially distilled Alaska North Slope crude 

oil at 521 °F (272°C) to remove the low molecular 

weight hydrocarbons to approximate natural 

weathering processes that occur after a spill. 

effective in freshwater environments 

may not necessarily be so in saltwater 

environments, and vice versa. The 

Agency is proposing this limitation to 

allow product manufacturers the 

flexibility to select which environment 

the product is to be tested and 

authorized for use, either saltwater, 

fresh water, or both environments. 

Therefore, the product would be listed 

and could only be authorized for use in 

those water environments for which it 

was tested and for which it met both the 

efficacy and toxicity listing criteria. 

(d) Bioremediation Testing and Listing 

Requirements 

The Agency is proposing to define 

bioremediation agents as biological 

agents and/or nutrient additives 

deliberately introduced into a 

contaminated environment to increase 

the rate of biodegradation and mitigate 

any deleterious effects caused by the 

contaminant constituents. 

Bioremediation agents include 

microorganisms, enzymes, and nutrient 

additives such as fertilizers containing 

bioavailable forms of nitrogen, 

phosphorus and potassium. For this 

agent category, the Agency is proposing 

to revise the efficacy testing protocols, 

to establish toxicity testing protocols, 

and to establish both efficacy and 

toxicity listing thresholds in 

§ 300.915(d). 

(1) Bioremediation Agent Efficacy 

Current Requirements: 

Bioremediation agent efficacy is 

currently tested following the protocols 

in Appendix C to part 300 of the NCP. 

The current bioremediation agent 

efficacy testing protocol is designed to 

determine a product’s ability to 

biodegrade oil by quantifying changes in 

the oil composition resulting from 

biodegradation using natural seawater 

as the test water. The protocol tests the 

bioremediation agent for microbial 

activity and quantifies the 

disappearance of saturated 

hydrocarbons and PAHs in weathered 

oil; for purposes of the proposal the 

Agency tested the protocol using ANS 

521.56 The sample preparation 

procedure extracts the oil phase into 

dichloromethane (DCM), with a 

subsequent solvent exchange into 

hexane. The analytical technique uses a 

high-resolution gas chromatograph/mass 

spectrometer (GC/MS); GC/MS provides 

for a high degree of chemical separation 

and spectral resolution. Concurrently 

with the chemical analysis, a 

microbiological analysis is also 

performed to determine and monitor the 

viability and growth of the microbial 

cultures being studied. For commercial 

products that are strictly microbial 

agents not containing their own 

nutrients, a mineral nutrient solution is 

provided if requested by the submitter; 

no further nutrients are added to 

commercial products containing their 

own nutrients. To be listed on the 

Schedule, bioremediation agents must 

demonstrate a statistically significant 

difference between the average 

degradation of both total alkanes and 

total aromatics in the oil achieved by 

the product after 28 days and the 

average degradation for the same 

compounds achieved by the nonnutrient control in the same time 

period. 

Proposed Revisions: The proposal 

reflects a series of changes to the current 

efficacy testing protocol for 

bioremediation agents. The protocol 

includes freshwater testing in addition 

to the current saltwater-based test, and 

uses artificial water for both fresh and 

saltwater testing, replacing the natural 

seawater currently used. The proposed 

protocol also eliminates several 

gravimetric and microbiological 

analyses and testing endpoints not used 

in the proposed listing determinations. 

Additionally, the proposed protocol 

limits the levels at which external 

nutrients may be added, which allows 

the addition for product formulations 

without nutrients, or for product 

formulations that have nutrient 

concentrations at insufficient levels for 

the experimental setup. Finally, the 

methodology streamlines the statistical 

analysis. The proposed revisions 

address concerns with the existing 

methodology as discussed below, 

expanding its application to include 

freshwater environments, improving the 

consistency and comparability of the 

test results, and generally streamlining 

the protocol. 

Protocol. The proposed efficacy 

testing protocol is designed to 

determine a bioremediation agent’s 

ability to biodegrade weathered crude 

oil in the exposure water (saltwater or 

freshwater) by quantifying changes in 

the oil composition resulting from 

biodegradation. It consists of a series of 

six product and control flasks 

containing artificial seawater or 

artificial freshwater and weathered 

crude oil in which biodegradation of the 

crude oil hydrocarbons is monitored for 

28 days. Product flasks at day 28 are 

compared to product flasks at day 0 to 

determine if a specified reduction both 

in total resolved alkanes and total 

resolved aromatics was achieved in that 

time period. Product flasks contain 

exposure water, weathered oil, and 

product in concentrations specified by 

the manufacturer. Positive control flasks 

must contain exposure water, oil, 

nutrients, and the standard culture 

supplied by the Agency. A negative 

control, consisting of artificial exposure 

water, product, weathered crude oil, 

nutrients, and a sterilant is also used to 

ensure that the observed degradation of 

hydrocarbons was not caused by abiotic 

losses or interaction with the product. 

The Agency is requesting comment on 

whether an additional protocol specific 

to products containing enzymes only 

would be appropriate; this would 

consist only of exposure water, 

weathered oil and the enzymatic 

product in the concentrations specified 

by the manufacturer. The proposed 

protocol quantifies the degradation (or 

disappearance) of alkane hydrocarbons 

and aromatic hydrocarbons. The sample 

preparation procedure extracts the oil 

phase into the solvent dichloromethane 

(DCM; also known as methylene 

chloride) with a subsequent solvent 

exchange into hexane. The test method 

targets the relatively easy to degrade 

normal alkanes and the more resistant 

and toxic aromatics. The analytical 

technique uses a high resolution GC/MS 

because of its high degree of chemical 

separation and spectral resolution. GC/ 

MS has long been used to study the 

weathering and fate of oil spilled into 

the environment. It gives unambiguous 

results for determining biodegradation 

efficacy. For quantitative analyses, the 

instrument is operated in the selected 

ion monitoring mode (SIM) of detection 

at a scan rate of > 5 scans per second 

to maximize the linear quantitative 

range and precision of the instrument. 

Fresh and Saltwater Environments. 

The existing bioremediation test is 

exclusively for saline environments 

with no equivalent test for freshwater 

environments. Further, the existing test 

uses natural seawater and has been 

found to give variable results due to the 

compositional variability of seawater 

both chemically and microbiologically. 

The Agency proposes to replace the 

natural seawater with a standardized 

artificial saltwater formula called GP2, 

whose components and concentrations 

are generally recognized, and which is 

easily made. The use of artificial 

saltwater allows for better test 

reproducibility. Additionally, the 

Agency proposes to expand the 

requirement for efficacy testing to 

include freshwater, which allows for a 

better evaluation of the use of these 

agents in this environment. Similarly to 


emcdonald on DSK67QTVN1PROD with PROPOSALS3
Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 3409 

the artificial saltwater, artificial minimal 

salts freshwater would be used with 

known ingredients (Bushnell and Haas; 

Journal of Bacteriology, Vol. 41: 653, 

1941). Because the Agency is adding a 

freshwater test, it is also allowing the 

submitter to test a product for 

freshwater only, saltwater only, or both. 

The Schedule listing would specify in 

which environment the product was 

tested and authorized for use. Products 

could be listed for use on saltwater only, 

on freshwater only, or for use on both 

environments, giving the option to the 

submitter to market its products 

accordingly. 

GC/MS Testing Endpoints. GC/MS has 

long been used to study the weathering 

and fate of oil spilled into the 

environment. However, GC/MS being 

the primary tool used in the analysis 

makes this test expensive. The current 

protocol includes several measured 

variables in both the product flasks and 

the non-nutrient control flasks, 

including the gravimetric residual oil 

weight analysis, a Most Probable 

Number microbiological analysis, and 

the GC/MS analysis at 3 different time 

points, days 0, 7, and 28. The Agency 

is proposing to eliminate all of these 

analyses except the day 0 and 28 GC/MS 

analysis of both the non-nutrient control 

and the product flasks. The Agency 

believes this is appropriate because the 

other measurements are not used in 

determining whether a product meets 

the listing criterion. Additionally, the 

statistical analysis has been greatly 

simplified, and a new decision rule is 

proposed for listing determinations 

rather than relying on a statistical 

significance test. 

• Gravimetric Weight Analysis: 

Originally, the gravimetric weight 

analysis was used as a preliminary test 

to avoid having to perform a GC/MS 

analysis. Products that failed to 

significantly reduce the gravimetric 

weight of the oil within 28 days were 

considered not effective, thereby 

eliminating the need to conduct the 

more expensive GC/MS analysis. 

However, numerous compounds can 

give rise to positive interferences with 

the gravimetric weight analysis, such as 

biomass lipids and other biogenic 

materials, thereby rendering the 

gravimetric analysis suspect. 

Furthermore, numerous factors can 

confound the interpretation of 

gravimetric weight changes in oil over 

time. This has led to confusion as some 

manufacturers have mistakenly 

concluded their product passed the 

testing protocol simply by complying 

with the gravimetric weight loss 

measurement. By eliminating the 

gravimetric analysis altogether, EPA is 

streamlining the testing process, 

resulting in less confusion and a modest 

analytical cost savings for the 

manufacturer. 

• Most Probable Number 

Enumeration (Microbiological Analysis), 

Nutrient Control, and Day-Seven 

Sampling Event: Results of these test 

endpoints, while currently required, 

would not be used in determining 

whether a product meets the proposed 

listing requirements. Therefore, the 

Agency is proposing to eliminate these 

test requirements from the proposed 

protocol. 

• 28 day Sampling Event: Generally, 

results of biodegradation may occur in 

less than 28 days, particularly for 

alkanes for which biodegradation often 

takes place in a much shorter time 

period. However, 28 days are needed to 

make sure that the aromatic 

components, which biodegrade more 

slowly, have been reduced significantly; 

testing protocols that accommodate 

aromatics are of particular importance 

because of their potential ecological 

toxicity. While the Agency could 

propose different time frames in 

determining whether the product met 

the reduction criterion for alkanes and 

aromatics, it believes that such an 

approach would be confusing. 

Therefore, the 28 day time period is 

being proposed for both fractions for 

simplicity and to provide sufficient time 

for degradation of the aromatics. 

Protocol Verification. The Agency 

proposes to provide a standard culture 

for performing laboratories to use as a 

positive control benchmark. A positive 

control is needed as an indication that 

the test was performed properly. The 

Agency is proposing to use as the 

standard culture an oil-degrading 

bacteria isolated from Disk Island in 

Prince William Sound in 1990. This 

culture is an excellent degrader of 

alkanes and aromatics in saltwater and 

freshwater, although it performs better 

in saltwater, especially in degrading the 

aromatics. This culture has the ability to 

degrade ANS 521 oil, with known 

efficacy values for both fresh and 

saltwater. The proposed positive control 

consists of triplicate flasks containing 

sterile artificial seawater or freshwater, 

nutrients (salts of nitrogen and 

phosphorus), the weathered ANS 521 

oil, and the standard culture. The 

performing laboratory must achieve the 

known reduction in alkane and aromatic 

fractions in these positive control flasks 

in order to certify they successfully 

conducted the test procedure. 

Additionally, data from the positive 

control are required to be submitted 

with the product test results. The 

Agency is not proposing, however, that 

the positive control be repeated every 

time a product test is performed. Rather, 

the certifying laboratory would be 

required to report the results of the 

positive control tests conducted within 

a year prior to the product testing, as 

part of the product submission package. 

Additionally, this positive control 

culture would be used as a standard 

microbial inoculum to test abiotic 

products, such as nutrients and 

enzymes. 

Added Nutrients. The current 

protocol allows the manufacturer to 

request the addition of nutrients to 

support a culture’s ability to degrade the 

crude oil hydrocarbons. This addition is 

currently allowed for commercial 

products that are strictly microbial 

agents and do not contain any nutrients; 

the addition of nutrients is not allowed 

for commercial products containing its 

own nutrients. A modified salt solution 

of nitrogen and phosphorus is used as 

the mineral nutrient. All microbial 

cultures need nutrients to survive and 

grow. In the natural environment, 

biodegradation is not completely 

limited by nutrient availability given 

that a low level flow of nutrients is 

continuous. To maximize 

biodegradation rates, the addition of 

nutrients is typically recommended in 

the field with a bioremediation product 

unless nutrients are already high (i.e., 

>5 mg/L). However, in a closed 

laboratory flask, the amount of nitrogen 

and phosphorus supplied by a typical 

product might easily become limiting 

quickly as biodegradation takes place 

because they are supplied only once at 

the beginning of the test. If nutrient 

limitation occurs, further reduction of 

hydrocarbons would likely be inhibited, 

and this may cause the product to fail 

the listing criteria. To address this 

problem, the Agency proposes 

modifying the protocol by allowing the 

addition of nutrients to any product 

containing living microbes that does not 

contain said nutrients in sufficient 

quantities to allow a fair evaluation. 

However, the additional quantities 

allowed are limited to total 

concentrations of nitrogen and 

phosphorus that do not to exceed the 

equivalent amounts used in the positive 

control. Capping the amount of 

nutrients that can be added to all 

products will yield more consistent 

results and more effective comparisons 

among products. 

Efficacy Thresholds. The Agency is 

proposing to revise the listing criteria by 

replacing the current ‘‘statistically 

significant difference’’ test with defined 

values for the percent reduction of total 

alkane and aromatic concentrations. For 

a bioremediation agent to be listed on 


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57Haines, J.R., E.J. Kleiner, K.A. McClellan, K.M. 

Koran, E.L. Holder, D.W. King, and A.D. Venosa. 

2005. ‘‘Laboratory evaluation of oil spill 

bioremediation products in salt and freshwater 

systems.’’ J. Ind. Micorbiol. Biotechnol. 32:171–185. 

58Blenkinsopp, S, G Sergy, Z Wang, MF Fingas, 

J Foght and DWS Westlake. 1995. Oil spill 

bioremediation agents-Canadian efficacy test 

protocols. Proceedings of the 1995 International Oil 

Spill Conference, Feb 27–March 2, Long Beach, CA. 

American Petroleum Institute, Washington, DC. pp. 

91–96. 

59USEPA 2010. http://www.epa.gov/oppefed1/

ecorisk_ders/toera_analysiseco.htm#Ecotox. 

the Schedule, the Agency proposes the 

percent reduction of the total alkane 

fraction (sum of all alkane 

concentrations determined by GC/MS) 

to be greater than 95% at day 28, and 

that the percent reduction of the total 

aromatic fraction (sum of all aromatic 

concentrations determined by GC/MS) 

must be greater than 70% at day 28, 

both based on the one-tailed Upper 95% 

Confidence Limit (UCL95) for salt water. 

For freshwater, the Agency proposes the 

percent reduction of the total alkane 

fraction (sum of all alkane 

concentrations determined by GC/MS) 

to be greater than 95% at day 28, and 

that the percent reduction of the total 

aromatic fraction (sum of all aromatic 

concentrations determined by GC/MS) 

must be greater than 40% at day 28, 

both based on the one-tailed Upper 95% 

Confidence Limit (UCL95). 

Basis of Efficacy Thresholds. 

According to Haines et al. (2005),57 the 

positive control culture was able to 

biodegrade total alkanes in saltwater by 

98.9% and total aromatics by 79.8% in 

28 days, based on the UCL90. In 

freshwater, the percent reduction values 

were 97.9% and 37.8%, respectively, 

again based on the UCL90. Thus, the 

proposed listing thresholds for the 

percent reduction of total alkanes and 

total aromatics from the GC/MS analysis 

are based on the findings of Haines et 

al. (95% for alkanes vs. 98.9% in 

saltwater and 97.9% in freshwater, and 

70% for aromatics in saltwater and 40% 

in freshwater vs. 79.8% in saltwater and 

37.8% in freshwater). As for the positive 

control, the Agency believes a 

reasonable target in saltwater would be 

95% for total alkanes in both types of 

exposure waters. For aromatics 

reduction, 70% is considered reasonable 

in saltwater and 40% in freshwater, 

based on Haines et al. EPA is using 

UCL95 values rather than the UCL90

values from Haines because EPA’s latest 

research uses 6 replicates for the test 

protocol which increases precision. The 

proposed criteria demonstrate that the 

product can cause a substantial 

degradation of the alkane and aromatic 

fractions of weathered crude oil 

compared to a control, as determined 

solely by GC/MS analysis. 

Of note, these proposed thresholds for 

listing bioremediation products on the 

Schedule are similar to those 

established for Canadian efficacy 

testing, which are reductions of 30% for 

total aliphatics and 10% for total 

aromatics. The 30% reduction in total 

aliphatics (including all resolvable and 

non-resolvable but GC-detectable 

aliphatics) is approximately equivalent 

to an 80% reduction in total GC/MSresolvable target n-alkanes, based on 

Canadian data. The 10% reduction in 

total aromatics is approximately 

equivalent to a 50% reduction of the 5- 

aromatic homologue group consisting of 

naphthalene, fluorene, 

dibenzothiophene, phenanthrene, and 

chrysene and their alkylated homologs. 

The U.S. aromatic series includes 2 

other 4-ring aromatics in addition to 

those 5 aromatic series considered by 

Blenkinsopp et al.58 Thus, the U.S. and 

Canadian protocols are similar in terms 

of decision criteria. The Agency 

requests comments on all the proposed 

changes and listing thresholds. 

(2) Bioremediation Agent Toxicity 

Current Requirements: The Agency 

currently has no bioremediation agent 

toxicity testing requirements for 

purposes of listing these agents on the 

Schedule. Section 5 of Appendix C is 

reserved for this purpose. The Agency 

has, however, on a case-by-case basis, 

requested manufacturers to test 

bioremediation agents for toxicity if the 

product contains surfactants or other 

ingredients that may be harmful to the 

environment. 

Proposed Revisions: The Agency is 

proposing an acute toxicity testing 

protocol for bioremediation agents to 

include both fresh and saltwater. The 

Agency will use these testing results to 

determine listing eligibility on the 

Schedule. The proposed testing 

protocols for bioremediation agents are 

detailed in Appendix C. The proposed 

acute toxicity test protocol for 

bioremediation agents is based on EPA’s 

protocol, Methods for Measuring the 

Acute Toxicity of Effluents and 

Receiving Waters for Freshwater and 

Marine Organisms. The Agency 

proposes to require bioremediation 

agents be tested for acute toxicity for the 

product alone using fresh water species 

Ceriodaphnia dubia and Pimephales 

promelas, and saltwater species 

Americamysis bahia and Menidia 

beryllina. The concentration of test 

product causing 50% lethality to the test 

organisms (LC50) lower and upper 95% 

confidence intervals (LCI95 and ULCI95) 

are calculated at the end of the exposure 

period. To be listed on the Schedule, 

bioremediation agents must demonstrate 

an acute lethal concentration for 50% of 

the test species (LC50) at the lower 95% 

confidence interval greater than 10 ppm 

in either fresh or salt water, consistent 

with the acute toxicity thresholds 

proposed for dispersants. EPA’s toxicity 

classification scheme 59 classifies LC50

values ranging from 10 ppm to 100 ppm 

as slightly toxic, and values above 100 

ppm substances are considered 

practically nontoxic to aquatic 

organisms. By proposing this threshold 

level the Agency is establishing an 

adequate safety margin without being 

overly restrictive. The Agency requests 

comments on the proposed acute 

toxicity methods (or any others 

available) and thresholds for 

bioremediation agents. 

Similarly to surface washing agents, 

the Agency is not proposing provisions 

for conducting acute toxicity tests with 

bioremediation agent-oil mixtures. The 

Agency is requesting comment on the 

need for acute toxicity tests conducted 

with bioremediation agents-reference oil 

mixtures. A protocol for preparation of 

product/oil mixtures for toxicity testing 

is available for review in the docket. 

(3) Listing of Non-Proprietary Nutrients 

The Agency recognizes there may be 

oil discharge situations where it is 

determined that the addition of 

nutrients in the form of salts of nitrogen, 

phosphorus and potassium (i.e., 

fertilizers) to stimulate or enhance 

bioremediation may be the most 

effective and environmentally favorable 

mitigation method. However, nonproprietary commercially available 

formulations of nutrients are not 

specifically listed on the Schedule, even 

though as nutrient additives they are 

subject to Subpart J requirements. 

Currently, an OSC may only authorize 

the use of an agent not listed on the 

Schedule when its use is necessary to 

prevent or substantially reduce a hazard 

to human life. Further, RRTs are not 

currently able to preauthorize the use of 

nutrients unless they are listed on the 

Schedule. To address these concerns, 

the Agency proposes to include on the 

Schedule a specific list of the following 

generic non-proprietary nutrients: 

Ammonium nitrate, ammonium 

phosphate, sodium nitrate, potassium 

nitrate, urea, sodium triphosphate (or 

tripolyphosphate), sodium phosphate, 

potassium phosphate (mono- or 

dibasic), triple super phosphate, or any 

combination thereof. For these nonproprietary commercial nutrients, the 

Agency believes there is no need for 

submission of readily available 


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60USEPA 2010. http://www.epa.gov/oppefed1/

ecorisk_ders/toera_analysis_eco.htm#Ecotox. 

information. Thus, the proposal requires 

no technical product data or further 

action on the part of a manufacturer 

prior to authorizing their use in 

response to a discharge event. However, 

this listing will be limited to products 

commonly formulated entirely of those 

mineral nutrients and syntheticallyderived urea listed. For products that 

may contain additional proprietary 

components or have unique proprietary 

formulations, the requirement for the 

submitter to provide the toxicity and 

efficacy data under the bioremediation 

agent category will apply. 

The Agency considered proposing a 

definition of ‘‘fertilizer’’ to specifically 

capture the listed bioremediation agents 

proposed to be exempted. However, 

fertilizer is a term commonly used to 

describe organic nutrients, which may 

contain substances that do not play a 

role in mitigating oil discharges, and 

that may have deleterious effects on the 

environment. Some non-proprietary 

fertilizers, for example, comprised of 

activated sewage sludge or manure, 

could contain unwanted pathogens and 

trace metals that could further stress the 

environment if used in response to an 

oil discharge. Thus, instead of an 

exemption based on a fertilizer 

definition, EPA proposes to restrict the 

exemption under the bioremediation 

category only to those nutrients listed 

above in order to avoid any confusion. 

The Agency requests comments on this 

approach. 

(e) Solidifier Testing and Listing 

Requirements 

The proposal defines solidifiers as 

substances that cause oil to become a 

coherent mass, preventing oil from 

dissolving or dispersing into the water 

column, and which are collected and 

recovered from the environment. For 

this agent category, the Agency proposes 

to revise the toxicity testing protocol 

and to establish a listing threshold for 

toxicity in § 300.915(e). Although 

solidifiers are intended to be removed 

from the environment, the proposed 

revisions and new toxicity listing 

threshold respond to concerns regarding 

the general increase in the use of 

chemical and biological agents as tools 

available for oil discharge responses. 

(1) Solidifier Efficacy 

There are currently no efficacy testing 

requirements in the NCP Subpart J for 

solidifiers to determine listing eligibility 

on the Schedule. These agents would 

have been captured by the current 

MOSCA agent category, which currently 

has no efficacy testing requirements, 

and which the Agency is proposing to 

eliminate. While the Agency is aware of 

existing protocols to determine the 

effectiveness of solidifiers, its focus has 

been on reviewing the protocols for 

dispersants and bioremediation agents, 

given that their specific process for 

affecting the oil allows them to be left 

in the environment, whereas solidifiers 

are intended for removal from the 

environment. Therefore, the Agency is 

not proposing an efficacy testing 

methodology for solidifiers, but is 

requesting comment on available 

methodologies and/or performance 

criteria (e.g., buoyancy) it can consider. 

(2) Solidifier Toxicity 

Current Requirements: The current 

NCP Subpart J requires solidifiers to be 

tested for saltwater species toxicity. 

Solidifier toxicity is tested following the 

dispersant toxicity testing protocols in 

Appendix C to part 300 of the NCP. 

Proposed Revisions: The proposal 

revises the toxicity testing requirements 

for solidifiers, including the testing 

protocol. While the Agency currently 

provides the toxicity testing results to 

the OSC to assist in authorization of use 

determinations, it is proposing to use 

these results to determine listing 

eligibility on the Schedule. 

The proposed revisions to the testing 

protocols for solidifiers are detailed in 

Appendix C to part 300. The proposed 

acute toxicity test protocol for solidifiers 

is based on EPA’s protocol, Methods for 

Measuring the Acute Toxicity of 

Effluents and Receiving Waters for 

Freshwater and Marine Organisms. The 

Agency proposes to require solidifiers 

be tested for acute toxicity for the 

product alone using fresh water species 

Ceriodaphnia dubia and Pimephales 

promelas, or saltwater species 

Americamysis bahia and Menidia 

beryllina, or both, depending on the 

intended product use. The 

concentration of test product causing 

50% lethality to the test organisms 

(LC50) and lower and upper 95% 

confidence intervals (LCI95 and ULCI95) 

are calculated at the end of the exposure 

period. To be listed on the Schedule, 

solidifiers must demonstrate an acute 

lethal concentration for 50% of the test 

species (LC50) at the lower 95% 

confidence interval greater than 10 ppm 

in either fresh or salt water, consistent 

with the acute toxicity thresholds 

proposed for dispersants. EPA’s toxicity 

classification scheme 60 considers LC50

values ranging from 10 ppm to 100 ppm 

as slightly toxic and values above 100 

ppm substances practically nontoxic to 

aquatic organisms. By proposing this 

threshold level, the Agency is 

establishing an adequate safety margin 

without being overly restrictive. The 

Agency requests comments on the 

proposed acute toxicity methods (or any 

others available) and thresholds for 

solidifiers. 

Similarly to surface washing agents, 

the Agency is not proposing provisions 

for conducting acute toxicity tests with 

solidifiers-oil mixtures. The Agency is 

requesting comment on the need for 

acute toxicity tests conducted with 

solidifiers-reference oil mixtures. A 

protocol for preparation of product/oil 

mixtures for toxicity testing is available 

for review in the docket. 

(3) Limitations 

The Agency is proposing a 

conditional use listing for solidifiers. 

The proposal specifies that the listing of 

these products is limited to use only in 

those water environments for which the 

product was tested and for which it met 

the listing threshold criteria. The 

Agency recognizes that products may 

yield effective results in certain 

environments and not in others. 

Products that may be effective in 

freshwater may not necessarily be so in 

saltwater, and vice versa. The Agency is 

proposing this limitation to allow 

product manufacturers the flexibility to 

select which environment the product is 

to be tested and could be authorized for 

use, either saltwater, fresh water, or 

both. Therefore, the product would be 

listed and may only be authorized for 

use in those water environments for 

which it was tested and for which it met 

the listing criteria. 

(f) Herding Agent Testing and Listing 

Requirements 

The proposal defines herding agents 

as substances that are used to control 

the spreading of oil across the water 

surface. For this agent category, the 

Agency proposes to revise the toxicity 

testing protocol and to establish a listing 

threshold for toxicity in § 300.915(f). 

While these agents are intended to be 

removed from the environment, the 

proposed revisions and new toxicity 

listing threshold respond to concerns 

regarding the general increase in the use 

of chemical and biological agents as 

tools available for oil discharge 

responses. 

Currently, there is a test requirement 

for distinguishing surface collecting 

agents from other chemical agents 

(§ 300.915(c)(9), Test to Distinguish 

Between Surface Collecting Agents and 

Other Chemical Agents). Because the 

proposal eliminates surface collecting 

agents as a category and redefines 

herding agents to better reflect its 

specific process for affecting the oil, and 


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61USEPA 2010. http://www.epa.gov/oppefed1/

ecorisk_ders/toera_analysis_eco.htm#Ecotox. 

62Buist, I., Potter, S., Nedwed, T., (2011) Herding 

Agents to Thicken Oil Spills in Drift Ice for In Situ 

Burning: New Developments, IOSC, http:// 

ioscproceedings.org/doi/abs/10.7901/2169-3358- 

2011-1-230. 

63Buist, I., Nedwed, T., (2011) Using Herders for 

Rapid In Situ Burning Of Oil Spills on Open Water, 

IOSC, http://ioscproceedings.org/doi/abs/10.7901/

2169-3358-2011-1-231. 

given that the agents will need to be 

identified in order for the required 

testing to be submitted, the Agency is 

eliminating this requirement. 

(1) Herding Agent Efficacy 

There are currently no efficacy testing 

requirements in the NCP Subpart J for 

herding agents to determine listing 

eligibility on the Schedule. These agents 

would have been captured by the 

current surface collecting agent 

category, which currently has no 

efficacy testing requirements, and which 

the proposal eliminates. The Agency is 

not proposing an efficacy testing 

methodology for herding agents, but is 

requesting comment on available 

methodologies and/or performance 

criteria it can consider. 

(2) Herding Agent Toxicity 

Current Requirements: The current 

NCP Subpart J requires herding agents 

to be tested for saltwater species 

toxicity. Herding agent toxicity is tested 

following the dispersant toxicity testing 

protocols in Appendix C to part 300 of 

the NCP. 

Proposed Revisions: The proposal 

revises the toxicity testing requirements 

for herding agents, including the testing 

protocol. While the Agency currently 

provides the toxicity testing results to 

the OSC to assist in authorization of use 

determinations, we are proposing to use 

these results to determine listing 

eligibility on the Schedule. 

The proposed revisions to the testing 

protocols for herding agents follow the 

same procedures as described for 

surface washing agents and are detailed 

in Appendix C to part 300. The acute 

toxicity test protocol for herding agents 

is based on EPA’s protocol, Methods for 

Measuring the Acute Toxicity of 

Effluents and Receiving Waters for 

Freshwater and Marine Organisms. The 

Agency proposes to require herding 

agents to be tested for acute toxicity for 

the product alone using fresh water 

species Ceriodaphnia dubia and 

Pimephales promelas, or saltwater 

species Americamysis bahia and 

Menidia beryllina, or both, depending 

on the intended product use. The 

concentration of test product causing 

50% lethality to the test organisms 

(LC50) and lower and upper 95% 

confidence intervals (LCI95 and 

ULCI95) are calculated at the end of the 

exposure period. To be listed on the 

Schedule, herding agents must 

demonstrate an acute lethal 

concentration for 50% of the test species 

(LC50) at the lower 95% confidence 

interval greater than 10 ppm in either 

fresh or salt water, consistent with the 

acute toxicity thresholds proposed for 

dispersants. EPA’s toxicity classification 

scheme 61 considers LC50 values ranging 

from 10 ppm to 100 ppm as slightly 

toxic and values above 100 ppm 

substances practically nontoxic to 

aquatic organisms. By proposing this 

threshold level, the Agency is 

establishing an adequate safety margin 

without being overly restrictive. The 

Agency requests comments on the 

proposed acute toxicity methods (or any 

others available) and thresholds for 

herding agents. 

Herding agents form a monolayer of 

surfactants on the water surface that 

result in the contraction of the oil 

slick.62 63 Herding agent composition 

may include hydrocarbons, 

fluorosurfactants and/or silicone-based 

surfactants, which suggests that a stock 

solution prepared using a WAF 

procedure similar to solidifiers may be 

appropriate. The Agency is requesting 

comment on the procedure for preparing 

the stock solution for herding agents for 

the acute toxicity tests proposed in 

Appendix C. Any alternative procedure 

for preparing the stock solution must 

include an appropriate rationale in 

order for the Agency to be able to 

consider it for final action. 

Similarly to surface washing agents, 

the Agency is not proposing provisions 

for conducting acute toxicity tests with 

herding agents-oil mixtures. The Agency 

is requesting comment on the need for 

acute toxicity tests conducted with 

herding agents-reference oil mixtures. A 

protocol for preparation of product/oil 

mixtures for toxicity testing is available 

for review in the docket. 

(3) Limitations 

The Agency is proposing a 

conditional use listing for herding 

agents. The proposal specifies that these 

products may only be used in those 

water environments for which the 

product was tested and for which it met 

the listing threshold criteria. The 

Agency recognizes that products may 

yield effective results in certain 

environments and not in others. 

Products that may be effective in 

freshwater may not necessarily be so in 

saltwater, and vice versa. The Agency is 

proposing this limitation to allow 

product manufacturers the flexibility to 

select which environment the product is 

to be tested and could be authorized for 

use, either saltwater, fresh water, or 

both. Therefore, the product would be 

listed and may only be authorized for 

use in those water environments for 

which it was tested and for which it met 

the listing criteria. 

(g) Sorbent Requirements 

The proposal defines sorbents as 

inert, insoluble substances that readily 

absorb and/or adsorb oil or hazardous 

substances. Sorbents would exclude 

those contaminated with substances that 

would interact with the environment 

beyond their absorption/adsorption 

capabilities (e.g., an invasive species). 

The proposed definition states that 

sorbents are generally collected and 

removed from the environment and may 

be used in their natural bulk form, or as 

manufactured products in particulate 

form, sheets, rolls, pillows, or booms. 

The list of sorbent materials in the 

proposed definition includes: Natural 

organic substances (e.g., feathers, cork, 

peat moss, and cellulose fibers such as 

bagasse, corncobs, and straw); (2) 

inorganic/mineral compounds (e.g., 

volcanic ash, perlite, vermiculite, 

zeolite, clay); and (3) synthetic 

compounds (e.g., polypropylene, 

polyethylene, polyurethane, polyester). 

The Agency proposes to identify a list 

of known sorbent materials, and make it 

publicly available so that emergency 

responders can be aware and make use 

of such sorbents on oil discharges. The 

Agency is also proposing a process for 

submitters to request to include other 

products as sorbents if they can certify 

they meet the inert, insoluble criteria. 

Current Requirements: Sorbents are 

currently not listed on the Schedule, but 

rather a list characterizing these 

materials is included in section 

300.915(g). The current rule allows the 

OSC to request written certification 

from the manufacturers that their 

particular sorbent product is comprised 

solely of those materials identified in 

the rule. When a sorbent consists of 

materials that are not specifically listed 

in the current rule, the Agency issues 

written certifications, and sometimes 

requires testing and evaluation for 

possible listing on the Schedule. 

Proposed Revisions: The Agency 

proposes to provide a Sorbent Product 

List that includes certain publicly 

available non-proprietary sorbent 

materials. The Agency also proposes to 

allow submitters to request that other 

products be included in this list as 

sorbents if they provide the technical 

information required, including data to 

support the claim that their product 

meets the sorbent definition. The 

Agency recognizes that a sorbent 


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material may consist of one or more 

substances not specifically identified in 

the proposed non-proprietary listing. 

For products consisting of one or more 

substances not specifically identified in 

the proposed listing, the Agency 

proposes submission requirements that 

include general and product 

characterization information required 

under paragraphs (a)(1) through (8), and 

paragraph (a)(13) of proposed § 300.915. 

These include name and contact 

information, identification as 

manufacturer or designated agent, 

product name/brand/trademark(s), 

contact information for primary 

distributors or importers, product SDS, 

conditions for product storage, product 

shelf life, and product label samples. 

The proposal would additionally 

require the certification statements 

required under paragraphs (a)(14)(iv), 

(a)(15), and (a)(16) of proposed 

§ 300.915. The submitter would be 

required to certify that the product does 

not contain specified bacterial, fungal, 

or viral pathogens or opportunistic 

pathogens above National Ambient 

Water Quality Criteria lowest density 

values; that the product does not 

contain specified contaminants above 

National Water Quality Standards 

levels; and that the product does not 

contain any of the prohibited agents. 

Finally, the submitter would be required 

to include information to support the 

claim that the product meets the sorbent 

definition, including data such as its 

relative solubility and non-reactivity in 

fresh and/or salt water. The Agency will 

review the submission and make a 

determination to include the product as 

a sorbent on the Sorbent Product List. 

The Agency requests comments on this 

approach. 

Testing Options 

The current Subpart J has no toxicity 

or efficacy testing requirements for 

sorbents. There are two ASTM 

standards for performance testing that 

could be applicable to sorbents: The 

ASTM F716–09 Standard Test Methods 

for Sorbent Performance of Absorbents, 

and the ASTM F726–12 Standard Test 

Method for Sorbent Performance of 

Adsorbents. These methods include 

laboratory tests that describe the 

performance of these products in 

removing oils that are not emulsified 

and other floating, immiscible liquids 

from the surface of water. While these 

methods are to be individually used as 

a basis for comparison of either 

absorbents or adsorbents in a consistent 

manner, they are not useful for a cross 

comparison of absorbents with 

adsorbents, even though according to 

ASTM F716–09 all absorbents exhibit 

adsorbent properties. Further, these 

agents are comprised of inert and 

insoluble materials that are generally 

removed from the environment after 

use, minimizing their potential harm. 

Thus, the Agency is not proposing to 

include efficacy or toxicity testing 

requirements for these agents, but is 

requesting comments on whether testing 

information should be included as part 

of the submission requirements for other 

materials or products to be included as 

part of the Sorbent Product List. 

5. Submission of Confidential Business 

Information (CBI) 

Currently, manufacturers may assert a 

claim of confidential business 

information (CBI) for any information in 

their product package submissions to 

EPA. Typically, manufacturers claim as 

CBI the chemical identity (e.g., chemical 

name and chemical abstracts number 

[CAS]) and concentration (weight 

percent) of each chemical component in 

the product along with information 

about the concentrations of those 

components in the product. The 

manufacturer may also claim certain 

other information in the technical 

product data, including technical data 

for sorbents, as CBI. EPA safeguards CBI 

information under the requirements in 

40 CFR part 2, subpart B. The proposal 

addresses the CBI provisions for product 

submission under Subpart J in 

§ 300.950. 

Due to the amount of dispersant used 

during the Deepwater Horizon incident, 

and the need for the public’s right-toknow about chemicals intentionally 

discharged into the environment, EPA 

wanted to make public information 

about the chemicals in the dispersant 

used, the results of air and water 

monitoring for these chemicals, and the 

concerns for human and environmental 

impact. A number of stakeholders 

wanted to know the chemical makeup of 

not only the dispersant used during the 

incident, but also of all other 

dispersants on the Schedule. This 

resulted in both a number of Freedom 

of Information Act (FOIA) requests and 

a Notice of Intent to Sue for Failure to 

Perform Nondiscretionary Duties under 

the CWA, requesting that the Agency 

release CBI for all dispersants on the 

Schedule. 

EPA worked with the manufacturer 

for the dispersant used on the Gulf in 

response to the Deepwater Horizon 

incident to make the product chemical 

information publicly available (see 

http://www.epa.gov/bpspill/). The 

Agency also compiled a comprehensive 

aggregate list of the chemicals used in 

all listed dispersants. During this 

process, some manufacturers recognized 

the need to make information available 

to the public, but also argued the need 

to protect proprietary business 

information from competitors. 

Companies provided information on the 

magnitude of resources expended to 

develop a product and test it for listing 

on the Schedule; however, they argued 

that disclosing the chemical 

components, CAS numbers, and/or 

concentrations for their product would 

allow domestic and international 

competitors to freely duplicate or 

reverse engineer their product and 

potentially drive them out of the market. 

EPA is aware that over 90% of 

businesses on the current Schedule are 

small, and that for some companies the 

product they developed for the 

Schedule is their only business. While 

companies could protect their product 

via the U.S. patent process, they would 

be required to release components and 

concentrations information, which 

would be made public. Manufacturers 

voiced concern that not only others may 

use that information to tailor 

competitive products, but that the U.S. 

patent process would offer no protection 

against international competitors. 

EPA believes that when chemical 

agents are used on oil discharges, it is 

critically important for the public and 

all other stakeholders to have 

information regarding the chemicals 

being added to the environment, along 

with information about their toxicity 

and fate. This is particularly true for 

major discharge events where larger 

quantities of chemical or biological 

agents may be authorized for use. 

Prompt and accurate information will 

allow the public to evaluate and 

understand the potential human and 

environmental effects of these chemical 

agents. While EPA understands it is 

essential for companies to protect their 

investment in developing unique 

products, it is proposing limitations to 

what submitters are allowed to claim as 

CBI in an effort to balance public access 

to information with proprietary business 

needs. The proposal provides that if a 

company submits a product for listing 

on the Schedule, then it will only be 

allowed to claim CBI for the 

concentrations of all chemical 

components, microbiological cultures, 

enzymes, or nutrients; all other 

information submitted to EPA for listing 

a product on the Schedule will not be 

considered CBI and will be made 

public. While providing confidential 

treatment for the concentrations of 

product components, the proposal 

allows public access to the identity of 

chemical components and relevant 

health and environmental effects 


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information. All other information 

required for a product submission (e.g., 

company data, distributors, general 

product properties, recommended use 

procedures, the product category, 

contaminants, production capacities, 

product testing data) would already be 

publicly available for commercial 

products, and would not constitute 

proprietary business information or 

provide a business advantage. The 

Agency requests comments on whether 

this approach safeguards against 

duplication or reverse engineering of 

products by competitors and whether 

other information in Subpart J should be 

considered as CBI. 

Alternatively, the Agency considered 

maintaining the current approach of 

allowing CBI claims for any information 

in their submission. When the incident 

arises where affected stakeholders or the 

public wants access to specific 

information, the Agency would request 

that the company substantiate its claims 

and make a determination whether to 

honor the claim or release the 

information to the public as provided in 

40 CFR part 2, subpart B. The Agency 

also considered modifying the current 

approach by making the component 

identity and concentration information 

public without further notice or action 

for major discharge events or SONS, or 

for events where a given amount of 

chemical or biological agent would be 

allowed for use. Finally, another option 

for modifying the current approach 

would be to allow manufacturers to 

waive CBI claims only for certain 

chemical components for monitoring 

purposes (e.g. manufacturer identifies a 

‘‘marker’’ component as a condition for 

listing) was also considered. The 

Agency is rejecting the current approach 

because it does not believe that, even 

with the modifications considered, it 

offers the appropriate balance between 

the public interest and business needs. 

EPA also considered developing an 

aggregate list of components used in 

categories of chemical and biological 

agents for public disclosure. For 

example, a list of all the chemicals used 

in listed dispersants, a separate list for 

those substances used in surface 

washing agents, etc. This would allow 

information to be disassociated with 

specific products and protected from 

reverse engineering or duplication of 

products by competitors, while 

providing public access. The concern 

with this approach is how to update the 

aggregate list for new products without 

potentially revealing the components 

added to the list for that new product. 

Further, in the event of a major 

discharge or SONS, the interest will be 

for information and monitoring data 

specific to the product being used. 

Consequently, EPA is not adopting this 

approach, but requests comments on 

these and other options to handle CBI 

while balancing all interests. 

6. Addition of a Product to the Schedule 

The proposal establishes the 

requirements for submitters to request a 

product be listed on the Schedule in 

§ 300.955. It provides administrative 

information, such as the address where 

to submit the package, as well as details 

of the requirements for a complete 

submission package. Additionally, it 

addresses how a submitter may request 

a listing determination review and the 

requirements when there are changes in 

a listed product. Finally, the proposal 

addresses the process the Agency will 

follow to review all new submissions, 

requests for review of decisions and 

product changes, as well as how it will 

transition from the current Schedule to 

a new one that reflects the new and 

amended testing and data requirement. 

Submission. The proposal updates the 

address where the package is to be 

submitted. 

Package contents. The proposal 

specifies a complete package must 

include, as follows: 

• A company letter certifying all 

testing was conducted on representative 

product samples at a nationally or 

internationally accredited laboratory, 

that it was conducted in accordance 

with all technical rule requirements, 

and that all test results and product 

technical data and information reported 

are true and accurate; 

• A numbered Table of Contents 

showing all required information and 

data submitted; 

• All required data and information 

(both general and product category 

specific) in the order the requirements 

appear in the rule; and 

• A separate inner envelope labeled: 

‘‘CONFIDENTIAL BUSINESS 

INFORMATION—TO BE OPENED BY 

THE PRODUCT SCHEDULE MANAGER 

ONLY’’, if applicable. 

Because of their intended function in 

responding to oil discharges, products 

listed on the Schedule will certainly 

impact the environment. It is important 

that the information provided by the 

submitter is true and accurate, as it 

serves as the basis for evaluating those 

potential environmental impacts. The 

Agency believes that it is appropriate for 

the submitter to be held accountable for 

the technical data and information 

provided to make these listing 

determinations. Thus, the proposal 

requires the submitter to certify the 

accuracy of the information submitted, 

and will reject any submission that is 

determined to be incomplete or noncompliant, misleading, or inaccurate. 

The requirements for a Table of 

Contents and for the information to be 

organized as it appears in the regulation 

are intended to make the Agency review 

process as efficient as possible. These 

requirements will assist the Agency in 

conducting a quick and accurate review, 

both during the transition period, as 

well as for future submissions, by 

generally simplifying the review 

process. 

While the Agency needs to process 

packages containing information 

claimed to be CBI with additional 

safeguards, it is the responsibility of the 

submitter to ensure that this information 

comes to the Agency clearly identified 

as such. Therefore, the proposal requires 

a separate and clearly marked envelope 

for CBI to ensure proper handling. 

EPA Review. The proposal maintains 

most of the existing Agency process for 

reviewing product submissions. A 

revision to the current process increases 

the number of days allowed for the 

Agency to complete its product review 

from the current 60 days to 90 days from 

the date of receipt. This proposed 

change considers the additional 

technical data and information 

proposed to be required, as well as the 

Agency’s past experience with 

submission packages based on the 

current requirements. 

EPA will first review the package for 

completeness and compliance with all 

data and information requirements and 

will contact the submitter to verify 

information, or to request clarification 

or additional information, including a 

product sample, as necessary. The 

Agency will make product listing 

determinations based on a technical 

evaluation of all data and information 

submitted, any relevant information on 

impacts or potential impacts of the 

product or any of its components on 

human health or the environment, and 

on the intended use of the product. The 

Agency reserves the right to make a 

determination on whether the product 

will be listed, and under which 

category. For products that may meet 

more than one category (e.g., a product 

that meets both the bioremediation and 

dispersant agent criteria), the Agency 

requests comments on whether there 

should be any product listing 

limitations beyond those identified for 

each individual product category. 

Within the 90-day timeframe, the 

Agency will notify the submitter, in 

writing, of its decision to either list the 

product on the Schedule and under 

which category or categories, or of its 

decision and supporting rationale to 

reject the submission. Submitters may 


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revise submission packages to address 

test results, data, or information 

deficiencies and resubmit them. 

Because the Agency will need a 

complete set of data and technical 

information to make a listing 

determination, the 90-day review time 

period will start anew once a complete 

package is resubmitted. 

Request for review of decision. The 

proposal is not substantively changing 

the process for a submitter to request 

that the Agency review its 

determination on a product. If the 

Agency rejects a product for listing on 

the Schedule, the proposal continues to 

allow for a submitter to appeal to the 

EPA Administrator to review its 

determination to reject the product 

listing. The proposal maintains the 

requirement that such a request be in 

writing, within 30 days of receipt of the 

written notification of EPA’s decision 

not to list the product on the Schedule. 

The request to review the Agency’s 

determination must include a clear and 

concise statement with supporting facts 

and technical analysis that demonstrates 

why the submitter believes the Agency’s 

assessment of the product was incorrect. 

The proposal allows the Administrator 

to request additional information or a 

meeting opportunity. Within 60 days of 

receipt of any such request, or within 60 

days of receipt of any requested 

additional information, the proposal 

requires the Administrator or her 

designee to notify the submitter in 

writing of the review decision, 

maintaining the current timeframe. 

Changes to a product listing. The 

Agency proposes to revise the 

provisions for notification of changes to 

a product listing. Submitters must notify 

EPA in writing within 30 days of any 

changes to the general product 

information submitted for listing on the 

Schedule so the OSCs have timely 

updated information. The proposal 

revises the notification requirement to 

include details of the specific changes to 

information submitted under 

§ 300.915(a)(1) through (8) and 

§ 300.915(a)(19) through (21) for a 

product on the Schedule, including the 

reasons for such changes and the 

supporting data and information, and 

maintains the provision allowing EPA to 

request additional information and 

clarification regarding these changes. 

For any changes to the chemical 

components and/or their 

concentrations, the proposed revisions 

would require retesting of the product 

according to the requirements for the 

product category, and the resubmission 

of a complete new package for a new 

review and consideration for a listing 

determination by the Agency of the 

reformulated product. While the Agency 

currently has and is retaining the option 

of requiring additional testing, it 

believes that when the chemical 

components or concentrations of a 

product change, an automatic retesting 

requirement is merited. The Agency 

believes this requirement is appropriate 

when the identity of the product itself 

changes; the only way of evaluating the 

potential effects of these changes on the 

efficacy and toxicity of a new product 

formulation is to retest it. The Agency 

considered whether it was necessary to 

explicitly provide the flexibility to 

waive this requirement under 

extraordinary circumstances (i.e., a 

SONS event). However, OSCs already 

have broad authority to use agents in 

areas impacted or threatened by a 

release or discharge, whether the agent 

is identified or not on the Schedule, to 

prevent or substantially reduce an 

immediate threat to human life. In 

addition, the Agency considered 

whether there is a chemical 

concentration threshold that could 

accommodate minor adjustments to a 

product. For example, a producer may 

make a slight variation in a product 

formula to account for a food grade or 

technical grade chemical component. 

Such a threshold might be that if 

concentration changes vary by no more 

than 1%, no retesting is necessary. 

However, the Agency has no basis for 

such a threshold and requests comment 

on this approach with appropriate 

technical details. Because of this, and 

the concern for the potential impact 

reformulated products may have on the 

environment, the Agency is proposing 

to require retesting whenever the 

chemical components or concentrations 

of a product change. However, the 

Agency is requesting comments on 

whether it should require the retesting 

of all products that have a change in 

composition, even if the only change is 

of chemical components that may 

considered inert. 

Transitioning Listed Products from 

the Current Schedule to the New 

Schedule. The Agency believes it 

important that products on the current 

Schedule continue to be available 

during the transition period to a new 

Schedule that reflects the amended 

requirements. During this transition 

period, all products on the current 

Schedule will remain conditionally 

listed and the Agency will rely on it for 

planning and response activities. 

Because of the proposed revisions to test 

protocols and listing criteria, and 

because of the additional test 

requirements, the Agency proposes that 

all products currently on the Schedule 

be retested, and that the new data and 

information be submitted to the Agency 

for reevaluation of the current listings 

within 24 months of the effective date 

of a final rule. The Agency believes this 

provides adequate time for submitters to 

prepare and submit new packages to 

EPA and for the Agency to review and 

make decisions on these products. For 

a product to be transitioned from the 

current Schedule to the new Schedule, 

manufacturers would be required to 

submit a new, complete package 

according to the amended test and 

listing criteria, and EPA would need to 

make a favorable finding to list the 

product on the new Schedule, either as 

currently listed or with modifications. 

Products on the current Schedule for 

which a new submission is not received, 

or that upon review of their submissions 

do not meet the revised listing criteria, 

would be removed from the Schedule at 

the end of the 24-month transition 

period. While the Agency is reviewing 

the new submission packages, planning 

and response authorities are encouraged 

to consider those products that based on 

existing data would meet the revised 

listing criteria. While the existing data 

may be limited and likely developed 

with different protocols, considering the 

new requirements in selecting products 

for planning and response activities 

would provide an increased level of 

environmental protection. The Agency 

notes, however, that this is not a 

requirement, and that the proposal 

would allow any product on the current 

Schedule to be authorized for use 

following the current protocols, until 

the 24-month transition period is over. 

The Agency is requesting comments on 

the practicability of this transition 

process, and whether the 24-month 

period allows sufficient time for 

retesting of products on the current 

Schedule, and for EPA to review and 

make listing determinations on the 

submissions for the new Schedule. The 

Agency also requests comments on 

potential R&D costs of modifying 

existing products to meet the new 

requirements that could be incurred 

during this transition. 

7. Mandatory Product Disclaimer 

The current requirements provide that 

the listing of a product on the Schedule 

does not constitute approval or 

endorsement of the product. To avoid 

possible misinterpretation or 

misrepresentation, the Agency currently 

requires that any label, advertisement, 

or technical literature that refers to the 

placement of the product on the 

Schedule must either reproduce in its 

entirety EPA’s written notification that 

it will add the product to the Schedule 


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currently in § 300.920(a)(2) or (b)(2), or 

include the disclaimer currently set 

forth in § 300.920(e). It remains the 

Agency’s position that listing a product 

on the Schedule does not constitute 

approval or endorsement of that 

product, nor a recommendation of its 

use. The Agency continues to believe 

that it is important to avoid any possible 

misinterpretation or misrepresentation 

of this policy. Thus, the requirement for 

a disclaimer to be included on any label, 

advertisement, or technical literature for 

the product is maintained. However, the 

proposal removes the alternative to 

reproduce in its entirety EPA’s written 

notification that it will add the product 

to the Schedule currently in 

§ 300.920(a)(2) or (b)(2). The Agency 

believes it will be able to update the 

Schedule list within a reasonable 

timeframe given the advances in 

information technology, and thus the 

option of producing the EPA letter of 

notification for a product listing should 

no longer be necessary. The Agency is 

proposing to modify the disclaimer 

language as follows: 

[PRODUCT NAME] is listed on the 

National Contingency Plan (NCP) Product 

Schedule. This listing does NOT mean that 

EPA approves, recommends, licenses, or 

certifies the use of [PRODUCT NAME] on an 

oil discharge. This listing means only that 

data have been submitted to EPA as required 

by Subpart J of the NCP. Only a Federal OnScene Coordinator (OSC) may authorize use 

of this product according to the NCP. 

The proposed revisions set forth in 

§ 300.965 are intended to clarify that the 

use of these products is conditional to 

OSC authorization following the 

requirements set forth under the NCP 

regulations. The disclaimer language 

must continue to be conspicuously 

displayed in its entirety, and must be 

fully reproduced on all product 

literatures, labels, and electronic media, 

including Web site pages. As discussed 

in the next section, a product can be 

removed from the Schedule if the 

submitter does not comply with the 

disclaimer requirements, or makes any 

improper attempt to demonstrate the 

approval or endorsement of a product. 

The Agency requests comments on the 

proposed revisions. 

8. Removal of a Product From the 

Schedule 

Products that are not properly used in 

the field may cause harm to human 

health and the environment, and may 

constitute violations of the CWA, and 

other federal, state, or local laws. 

Misleading, inaccurate, or incorrect 

statements within a product submittal 

package or within language that refers to 

the listing of a product on the Schedule 

may result in their improper or incorrect 

use. Falsification of federal documents, 

unsupported toxicity or efficacy claims, 

submission of incorrect product 

composition or use information, or 

withholding technical product data are 

some examples of these acts. To 

minimize potential misuse of listed 

products, the Agency believes it is 

appropriate to further clarify the criteria 

for the removal of a product from the 

Schedule. In § 300.970 the proposal 

specifically includes, but does not limit, 

as causes for removal from the 

Schedule: Any misleading, inaccurate, 

or incorrect statements within the 

product submission to EPA or to any 

person or private or public entity 

regarding the composition or use of the 

product to remove or control oil 

discharges, including on labels, 

advertisements, or technical literature; 

any alterations to the chemical 

components, concentrations, or use 

conditions of the product without 

proper notification to EPA as required 

by § 300.955(e); the failure to print the 

disclaimer provided in § 300.965 on all 

labels, advertisements, or technical 

literature; or any new or previously 

unknown relevant information 

concerning the impacts or potential 

impacts of the product to human health 

or the environment. It also establishes a 

process for removal if the Agency 

obtains evidence of cause for removal. 

EPA would notify the submitter in 

writing, at the address of record, of its 

reasons for removal of the product from 

the Schedule. The proposal would allow 

for an appeals process similar to the one 

set forth for listing determinations. 

Appeals must be received within 30 

days of receipt of EPA’s removal 

notification and must contain a clear 

and concise statement with supporting 

facts and technical analysis 

demonstrating why the submitter 

believes EPA’s decision was incorrect. 

Written notification from the 

Administrator will be sent to the 

submitter within 60 days of any appeal, 

or within 60 days of receipt of any 

requested additional information. 

However, if no appeal is received within 

the 30 days of receipt of EPA’s removal 

notification, the product would be 

delisted without further notice. The 

Agency requests comments on the 

proposed clarification of criteria for 

removal of products from the Schedule, 

and on the associated appeals process. 

9. Appendix C to Part 300 

The Agency is proposing to revise the 

current Appendix C—Swirling Flask 

Dispersant Efficacy Test, Revised 

Standard Dispersant Toxicity Test, and 

Bioremediation Agent Efficacy Test as 

Appendix C—Requirements for Product 

Testing Protocols and Summary Test 

Data: Dispersant Baffled Flask Efficacy 

and Toxicity Tests; Standard Acute 

Toxicity Test for Bioremediation Agents, 

Surface Washing Agents, Herding 

Agents, and Solidifiers; and 

Bioremediation Agent Efficacy Test. The 

proposed revisions reflect the proposed 

new and revised testing protocols for 

listing agents on the Schedule. The 

details of the technical changes and 

rationale are discussed for each agent in 

section V.C.4 of this preamble—Data 

and Information Requirements for 

Product Schedule Listing. The appendix 

reflects the proposed technical 

considerations and listing requirements. 

The Agency is requesting comment on 

the protocols and their technical 

rationale. The Agency is also requesting 

comment on its organization and ease of 

use. 

10. Appendix E to Part 300 

The 1994 revisions to the NCP 

established Appendix E, Oil Spill 

Response, which separates the oil spill 

response requirements of the NCP from 

the hazardous substance release 

requirements (59 FR 47414). The 

purpose of creating this appendix was to 

compile general oil discharge response 

requirements into one document to aid 

responsible parties and responders with 

their duties under the national response 

system. The Agency’s intent was to 

provide guidance, and not to alter in 

any way the meaning or policy stated in 

other sections or subparts of the NCP. 

However, some minor variations 

between the Appendix E provisions and 

the analogous provisions of the NCP 

rule language were necessary to ensure 

that the appendix addressed only oil 

discharges; hazardous substance 

releases continue to be addressed in the 

NCP rule but are not addressed in 

Appendix E. 

The Agency proposes to remove 

Appendix E. While having all of the 

information pertaining to oil discharges 

compiled in one location may offer 

useful guidance, it is not necessary that 

this guidance be codified as a regulatory 

appendix to the NCP. The provisions in 

the appendix do not alter any NCP 

requirement; however, they do contain 

variations from the main NCP 

requirements in order to have the 

appendix be relevant solely to oil 

discharges. While EPA carefully 

reviewed the appendix and the relevant 

sections of the NCP at the time it was 

established to ensure consistency in 

policy, instructions, guidance and 

requirements, there were intentional 

minor variations. These may result in 

having responses to oil discharges 


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subject to two sets of what appear to be 

potentially conflicting requirements, 

causing unnecessary confusion. 

Because all requirements in Appendix 

E are part of the NCP, any revisions to 

the NCP necessitate revisions to this 

appendix. This adds burden not only for 

the Agency in revising and ensuring 

consistency, but also for the regulated 

community in reviewing redundant and 

duplicative requirements. While it may 

be a useful tool to have all of the oil 

discharge specific requirements in one 

location, the Agency has reconsidered 

its position and believes that this is 

more appropriately achieved through a 

separate guidance document, one that 

does not codify duplicative regulatory 

requirements. The Agency requests 

comments on the proposal to remove 

Appendix E from the NCP regulation, 

and whether it should continue to offer 

similar guidance through other formats. 

VI. Summary of Proposed Rule 

Provisions 

This section summarizes the proposed 

changes to 40 CFR parts 110 and 300. 

Subpart J has been renumbered to 

include new, consolidated, and revised 

sections. Some of the rule sections have 

been retained, removed, or moved in 

their entirety. The Table below provides 

an overview of the existing rule and 

proposed rule citations for a quick 

reference of the proposed changes. 

Section 110.4, Dispersants, would be 

revised to link the rule with the new 

and amended regulatory definitions for 

Subpart J product categories. 

Section 300.5, Definitions, would be 

revised to include new, amended, and 

deleted definitions. 

Subpart J—Use of Dispersants, 

Chemicals, and Bioremediations Agents, 

heading would be revised to reflect new 

and amended regulatory definitions for 

product categories. 

Section 300.900, General, paragraphs 

(a) and (c) would be revised to reflect 

new and amended regulatory definitions 

for product categories. 

Section 300.905, NCP Product 

Schedule, would be removed. 

Section 300.910, Authorization of 

Use, would be revised and new 

paragraphs added to clarify planning 

and preauthorization responsibilities. 

• Paragraph (a) would be revised to 

clarify the requirements, including 

process, responsibilities, and factors to 

consider for preauthorization; and add 

new requirements for preauthorization 

plan review, concurrence, and 

withdrawal procedures. 

• Paragraph (b) would be revised to 

clarify the requirements for using a 

listed product not addressed by a 

preauthorization plan and add new 

parameters for use considerations. 

• Paragraph (c) would be revised to 

clarify the requirements for authorizing 

the use of burning agents by an OSC for 

authorized in-situ burns. 

• Paragraph (d) would be revised to 

clarify the exception requirements and 

add specific time frames for notification 

of continued agent use. 

• Paragraph (e) would be revised to 

expand the prohibition to include 

nonylphenol (NP) or nonylphenol 

ethoxylates (NPEs) as components of 

chemical or biological agents. 

• Paragraph (f) would be revised to 

add new regulatory requirements for 

agent storage and use. Existing 

paragraph (f) requirements would be 

moved to new paragraph (g), 

Supplemental Testing, Monitoring, and 

Information. 

• New paragraph (g), Supplemental 

Testing, Monitoring, and Information, 

would revise the regulatory text to 

clarify the requirements for 

supplemental testing, monitoring and 

information. 

• New paragraph (h), Recovery of Oil 

and Agents from the Environment, 

would add regulatory requirements for 

recovery of oil and agents from the 

environment. 

• New paragraph (i), Reporting of 

Agent Use, would add regulatory 

requirements for notification of agent 

use on an oil discharge. 

New section 300.913, Monitoring the 

Use of Dispersants, would add 

regulatory requirements for monitoring 

certain prolonged surface and 

subsurface use of dispersants. 

Section 300.915, Data Requirements, 

would be revised to consolidate general 

submission requirements applicable to 

all product categories. The section 

would be restructured to include new 

testing and listing requirements for 

specific product categories. 

• Paragraph (a), Dispersants, would 

be revised to consolidate general testing 

and listing requirements from existing 

paragraphs (a), (b), (d), and (f). The 

paragraph would include revisions and 

new requirements for the identification 

of and testing for all product categories 

designated for listing. Existing 

paragraph (a) requirements specific to 

dispersants would be moved to new 

section 300.915(b), Dispersant Testing 

and Listing Requirements. The 

paragraph would also be revised to add 

new toxicity and efficacy testing 

requirements, limitations for use, and 

new criteria for listing a dispersant to 

the Schedule. Existing paragraph (b) 

would be moved to new paragraph (c), 

Surface Washing Agent Testing and 

Listing Requirements. 

• Paragraph (b), Surface Washing 

Agents, would be moved to new 

paragraph (c), Surface Washing Agent 

Testing and Listing Requirements. The 

paragraph would be revised to add new 

toxicity and efficacy testing 

requirements, limitations for use, and 

new criteria for listing a surface washing 

agent to the Schedule. Existing 

paragraph (c), Surface Collecting 

Agents, would be deleted. 

• Paragraph (d), Bioremediation 

Agents, would be revised to add new 

toxicity and efficacy testing 

requirements, limitations for use, and 

new criteria for listing a bioremediation 

agent to the Schedule. Existing 

paragraphs (d)(9) and (10) were moved 

to new paragraph (a), General Product 

Information. 

• Paragraph (e) would be revised to 

add new regulatory requirements for 

submission and listing of a solidifier. 

Existing paragraph (e), Burning Agents, 

would be deleted. 

• Paragraph (f) would be revised to 

add new toxicity testing requirements, 

limitations of use, and criteria for listing 

a herding agent on the Schedule. 

Existing paragraph (f), Miscellaneous 

Oil Spill Control Agents, would be 

deleted. 

• Paragraph (g), Sorbents, would be 

revised to add new exceptions for listing 

a sorbent to the Schedule. 

Section 300.920, Addition of Products 

to Schedule, would be moved to new 

section 300.955, Addition of a Product 

to the Schedule. 

• Paragraph (a) would be revised to 

include submission instructions for all 

product categories. Existing paragraphs 

(a)(1) through (3) regulatory text specific 

to dispersant applications would be 

moved to new §§ 300.915(b) and 

300.955(c) and (d). 

• Paragraph (b) would be revised to 

add new regulatory text for preparation 

of complete submission packages. 

Existing paragraph (b) regulatory text 

would be moved to new § 300.955(c) 

and (d). 

• Paragraph (c) would be revised to 

add regulatory text for EPA’s review of 

submission packages and decision 

criteria for listing. Existing paragraph (c) 

would be moved to new § 300.950, 

Submission of Confidential Business 

Information (CBI). 

• Paragraph (d) would be revised to 

add regulatory text for requesting a 

listing decision review. Existing 

paragraph (d) would be moved to new 

§ 300.955(e), Changes to a Listed 

Product. 

• Paragraph (e) would be revised to 

add new regulatory text for notification 

of changes to a listed product. Existing 

paragraph (e) would be moved to new 


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3418 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

§ 300.965, Mandatory Product 

Disclaimer. 

• New paragraph (f) would add new 

regulatory requirements for 

transitioning products on the current 

Schedule to the new Schedule. 

New § 300.950, Confidential Business 

Information (CBI), would revise and 

clarify the allowable CBI claims in a 

submission package. 

New § 300.965, Mandatory Product 

Disclaimer, would clarify the regulatory 

text for including a disclaimer statement 

on all product labels and literature. 

New § 300.970, Removal of a Product 

from the Schedule, would add basis for 

removal of products from the Schedule, 

EPA notification of decision, and 

appeals process. 

Revised Appendix C to Part 300— 

Requirements for Product Testing 

Protocols and Summary Test Data: 

Dispersant Baffled Flask Efficacy and 

Toxicity Tests; Standard Acute Toxicity 

Test for Bioremediation Agents, Surface 

Washing Agents, Herding Agents, and 

Solidifiers; and Bioremediation Agent 

Efficacy Test. 

Removed Appendix E to Part 300— 

Oil Spill Response. 

40 CFR PART 100 DISCHARGE OF OIL—DISTRIBUTION TABLE

Current citation Proposed rule citation 

110.4 Dispersants .................................................................................. 110.4 Chemical and Biological Agents. 

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

Current citations Proposed rule citations 

§ 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 Discharges Addressed by a Preauthorization Plan. 

§ 300.910(b) .............................................................................................. § 300.910(b) Use of Agents Identified on the Schedule on Oil Discharges 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 Requirements. 

§ 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, 

Bioremediation Agents, and Miscellaneous Oil Spill Control Agents.

§ 300.955(a) Submission. 


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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 

Reviews 

A. Executive Order 12866: Regulatory 

Planning and Review and Executive 

Order 13563: Improving Regulation and 

Regulatory Review 

Under Executive Order 12866 (58 FR 

51735, October 4, 1993), this action is a 

‘‘significant regulatory action.’’ This 

action raises novel legal or policy issues 

arising out of legal mandates, the 

President’s priorities, or the principles 

set forth in the Executive Order. 

Accordingly, EPA submitted this action 

to the Office of Management and Budget 

(OMB) for review under Executive 

Orders 12866 and 13563 (76 FR 3821, 

January 21, 2011) and any changes made 

in response to OMB recommendations 

have been documented in the docket for 

this action. 

In addition, EPA prepared an analysis 

of the potential costs and benefits 

associated with this action. This 

analysis is contained in the Regulatory 

Impact Analysis for Proposed Revisions 

to the National Oil and Hazardous 

Substances Pollution Contingency Plan 

Regulations. A copy of the analysis is 

available in the docket for this action 

and the analysis is briefly summarized 

here. 

The Agency expects the proposed rule 

would not cause a significant economic 

impact on a substantial number of small 

businesses. The total incremental costs 

are estimated as $667,610 to $694,343 

annually at 3% and 7% ($2011) 

annualization rates, respectively. The 

benefits of this action are assessed 

qualitatively and include, for example, 

greater clarity of regulatory 

requirements, as well as less toxic 

products. The resulting ratio of 

compliance cost to annual sales revenue 

for the proposed rule for existing and 

new product manufacturers would be 

less than one percent in most instances. 

B. Paperwork Reduction Act 

The information collection 

requirements in this proposed rule have 

been submitted for approval to the 

Office of Management and Budget 

(OMB) under the Paperwork Reduction 

Act, 44 U.S.C. 3501 et seq. The 

Information Collection Request (ICR) 

document prepared by EPA has been 

assigned EPA ICR number 1664.10. You 

can find a copy of the ICR in the docket 

for this rule, and it is briefly 

summarized here. The ICR supporting 

this proposed rule is largely selfimplementing. The information 

collection is to ensure that: (1) The 

Agency has the necessary information to 

make Schedule listing determinations 

specific to the different product 

categories; (2) product use by owners or 

operators of facilities or vessels, or 

response personnel, in response to oil 

discharges is performed in accordance 

with all applicable requirements; and 

(3) the Agency can verify compliance as 

needed. Section 300.950 of the NCP 

contains provisions for confidentiality. 

EPA has carefully considered the 

burden imposed upon the regulated 

community by the proposed regulations. 

EPA believes that the activities required 

are necessary and, to the extent 

possible, has attempted to minimize the 

burden imposed. The minimum 

requirements specified in the proposed 

rule are intended to ensure that, when 

needed, products are used properly in 

the field to respond to an oil discharge 

in a manner protective of human health 

and the environment. 

Respondents/affected entities: 

Manufacturers of oil spill mitigating 

agents (products)/Oil spill responsible 

parties. 

Respondent’s obligation to respond: 

Mandatory (40 CFR Part 300, Subpart J). 

Estimated number of respondents: 65. 

Frequency of response: Initially. 

Total estimated burden: 721 hours 

(per year). Burden is defined at 5 CFR 

1320.3(b). 

Total estimated cost: $584,504 (per 

year), includes $575,400 operation & 

maintenance costs. 

An agency may not conduct or 

sponsor, and a person is not required to 

respond to, a collection of information 

unless it displays a currently valid OMB 

control number. The OMB control 

numbers for EPA’s regulations in 40 

CFR are listed in 40 CFR part 9. 

Submit your comments on the 

Agency’s need for this information, the 

accuracy of the provided burden 

estimates, and any suggested methods 

for minimizing respondent burden to 

the EPA using the docket identified at 

the beginning of this rule. You may also 

send your ICR-related comments to 

OMB’s Office of Information and 

Regulatory Affairs via email to oria_

submisssions@omb.eop.gov, Attention: 

Desk Officer for EPA. Since OMB is 

required to make a decision concerning 

the ICR between 30 and 60 days after 

receipt, OMB must receive comments no 

later than February 23, 2015. The EPA 

will respond to any ICR-related 

comments in the final rule. 

C. Regulatory Flexibility Act (RFA) 

The Regulatory Flexibility Act (RFA) 

generally requires an agency to prepare 

a regulatory flexibility analysis of any 

rule subject to notice and comment 

rulemaking requirements under the 

Administrative Procedure Act or any 

other statute unless the agency certifies 

that the rule will not have a significant 

economic impact on a substantial 

number of small entities. Small entities 

include small businesses, small 

organizations, and small governmental 

jurisdictions. 

For purposes of assessing the impacts 

of the proposed rule on small entities, 

small entity is defined as: (1) As defined 

by the Small Business Administration’s 

(SBA) regulations at 13 CFR 121.201; (2) 

a small governmental jurisdiction that is 

a government of a city, county, town, 

school district or special district with a 

population of less than 50,000; or (3) a 

small organization that is any not-forprofit enterprise that is independently 

owned and operated and is not 

dominant in its field. 

After considering the economic 

impacts of this proposed rule on small 

entities, I certify that this action will not 

have a significant economic impact on 

a substantial number of small entities. 

The small entities directly regulated by 

this proposed rule are product 


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manufacturers and laboratories and state 

and local governments that are involved 

in product development, testing and use 

for oil discharge response. EPA 

conducted a small business analysis 

consistent with the Agency’s 2006 small 

business guidance. The Agency’s 

analysis indicates that about 95 percent 

of manufacturers are small businesses. 

In conducting the small business 

analysis, the agency compared the 

incremental annualized compliance 

costs to the annual sales revenue for the 

smallest entities. The results indicate 

that 90 percent of the smallest 

manufacturers have annualized 

compliance costs that are less than 1 

percent of their annual sales revenue, 

and that no manufacturers are expected 

to have incremental costs that exceed 3 

percent of annual sales. The small 

business analysis is available for review 

in the Regulatory Impact Analysis (RIA). 

Therefore, we have determined that this 

proposed rule does not have a 

significant impact on a substantial 

number of small entities. 

Nonetheless, EPA has tried to reduce 

the impact of this rule on small entities 

in developing the regulatory 

requirements that balance the costs and 

burden, while addressing the 

environmental protection concerns. We 

continue to be interested in the 

potential impacts of this proposed rule 

on small business entities and welcome 

comments on the issues related to such 

impacts. 

D. Unfunded Mandates Reform Act 

This action contains no Federal 

mandates under the provisions of Title 

II of the Unfunded Mandates Reform 

Act of 1995 (UMRA), 2 U.S.C. 1531– 

1538 for State, local, or tribal 

governments or the private sector. This 

proposed rule imposes no new 

enforceable duty on any state, local or 

tribal governments or the private sector. 

UMRA excludes from the definition of 

‘‘Federal intergovernmental mandate’’ 

and ‘‘Federal private sector mandate’’ 

duties that arise from conditions of 

Federal assistance. UMRA generally 

excludes from the definition of ‘‘Federal 

intergovernmental mandate’’ duties that 

arise from participation in a voluntary 

Federal program. UMRA also excludes 

from the definition of ‘‘Federal private 

sector mandate’’ duties that arise from 

participation in a voluntary Federal 

program. Since the decision on whether 

to request that a product be included on 

the Schedule is voluntary, the Agency 

has determined that this proposed rule 

is not subject to the requirements of 

sections 202 or 205 of UMRA. This 

action is also not subject to the 

requirements of section 203 of UMRA 

because it contains no regulatory 

requirements that might significantly or 

uniquely affect small governments. 

E. Executive Order 13132: Federalism 

This action does not have federalism 

implications. It will not have substantial 

direct effects on the States, on the 

relationship between the national 

government and the States, or on the 

distribution of power and 

responsibilities among the various 

levels of government, as specified in 

Executive Order 13132. This proposal 

does not alter the general procedures 

already defined in the NCP of how state, 

local, and federal agencies cooperate in 

responding to oil spills and how to 

consult with the OSC and RRT when 

considering the use of products on the 

Schedule. Thus, Executive Order 13132 

does not apply to this action. In the 

spirit of Executive Order 13132, and 

consistent with EPA policy to promote 

communications between EPA and State 

and local governments, EPA specifically 

solicits comment on this proposed 

action from State and local officials. 

F. Executive Order 13175: Consultation 

and Coordination With Indian Tribal 

Governments 

Subject to Executive Order 13175 (65 

FR 67249, November 9, 2000), EPA may 

not issue a regulation that has tribal 

implications, that imposes substantial 

direct compliance costs, and that is not 

required by statute, unless the Federal 

government provides the funds 

necessary to pay the direct compliance 

costs incurred by tribal governments, or 

EPA consults with tribal officials early 

in the process of developing the 

proposed regulation and develops a 

tribal summary impact statement. 

EPA has concluded that this action 

may have tribal implications. However, 

it will neither impose substantial direct 

compliance costs on tribal governments, 

nor preempt Tribal law, similarly to the 

effect on states. EPA will be consulting 

with tribal officials as it develops this 

regulation to permit them to have 

meaningful and timely input into its 

development. Consultation will include 

conference calls, webinars, and 

meetings with interested tribal 

representatives to ensure that their 

concerns are addressed before the rule 

is finalized. In the spirit of Executive 

Order 13175 and consistent with EPA 

policy to promote communications 

between EPA and tribal governments, 

EPA specifically solicits comment on 

this proposed rule from tribal officials. 

G. Executive Order 13045: Protection of 

Children From Environmental Health 

Risks and Safety Risks 

EPA interprets EO 13045 (62 FR 

19885, April 23, 1997) as applying only 

to those regulatory actions that concern 

health or safety risks, such that the 

analysis required under section 5–501 of 

the EO has the potential to influence the 

regulation. This action is not subject to 

EO 13045 because it does not establish 

environmental standards, such as limits 

on levels of pollutants in the water, that 

are intended to directly mitigate health 

or safety risks. 

H. Executive Order 13211: Actions That 

Significantly Affect Energy Supply, 

Distribution or Use 

This proposed rule is not a 

‘‘significant energy action’’ as defined in 

Executive Order 13211, ‘‘Actions 

Concerning Regulations that 

Significantly Affect Energy Supply, 

Distribution, or Use’’ (66 FR 28355, May 

22, 2001) because it is not likely to have 

a significant adverse effect on the 

supply, distribution, or use of energy. 

The proposal focuses on maintaining 

the availability of certain response tools 

that can be considered when responding 

to oil discharges, minimizing any 

potential adverse impacts from their 

use, and resulting in greater overall 

environmental protection. Thus, the 

proposed rule would not cause 

reductions in the supply or production 

of oil, fuel, coal, or electricity; nor 

would it result in increased energy 

prices, increased cost of energy 

distribution, or an increased 

dependence on foreign supplies of 

energy. 

I. National Technology Transfer and 

Advancement Act 

Section 12(d) of the National 

Technology Transfer and Advancement 

Act of 1995 (‘‘NTTAA’’), Public Law 

104–113, 12(d) (15 U.S.C. 272 note) 

directs EPA to use voluntary consensus 

standards in its regulatory activities 

unless to do so would be inconsistent 

with applicable law or otherwise 

impractical. Voluntary consensus 

standards are technical standards (e.g., 

materials specifications, test methods, 

sampling procedures, and business 

practices) that are developed or adopted 

by voluntary consensus standards 

bodies. NTTAA directs EPA to provide 

Congress, through OMB, explanations 

when the Agency decides not to use 

available and applicable voluntary 

consensus standards. 

This rulemaking involves technical 

standards. The Agency conducted a 

search to identify potentially applicable 


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voluntary consensus standards for 

efficacy testing. However, we identified 

no such standards. Therefore, EPA 

developed the Baffled Flask Efficacy 

Test and the Bioremediation Efficacy 

Test required in Appendix C of this 

proposed rule. Voluntary consensus 

standards developed by ASTM are 

recommended for several product 

property data points, such as pH, flash 

point and pour point. The product 

toxicity testing relies on existing 

protocols that are universally accepted. 

EPA welcomes comments on this aspect 

of the proposed rulemaking and, 

specifically, invites the public to 

identify potentially-applicable 

voluntary consensus standards for 

product efficacy and to explain why 

such standards should be used in this 

regulation. 

J. Executive Order 12898: 

Environmental Justice 

Executive Order 12898, ‘‘Federal 

Actions to Address Environmental 

Justice in Minority Populations and 

Low-Income Populations’’ (59 FR 7629 

(February 11, 1994)) establishes federal 

executive policy on environmental 

justice. Its main provision directs 

federal agencies, to the greatest extent 

practicable and permitted by law, to 

make environmental justice part of their 

mission by identifying and addressing, 

as appropriate, disproportionately high 

and adverse human health or 

environmental effects of their programs, 

policies, and activities on minority 

populations and low-income 

populations in the United States. 

EPA is committed to addressing 

environmental justice concerns and has 

assumed a leadership role in 

environmental justice initiatives to 

enhance environmental quality for all 

citizens of the United States. The 

Agency’s goals are to ensure that no 

segment of the population, regardless of 

race, color, national origin, income, or 

net worth bears disproportionately high 

and adverse human health and 

environmental impacts as a result of 

EPA’s policies, programs, and activities. 

In response to Executive Order 12898, 

EPA’s Office of Solid Waste and 

Emergency Response (OSWER) formed 

an Environmental Justice Task Force to 

analyze the array of environmental 

justice issues specific to waste programs 

and to develop an overall strategy to 

identify and address these issues 

(OSWER Directive No. 9200.3–17). To 

address this goal, EPA conducted a 

qualitative analysis of the 

environmental justice issues under this 

proposed rule. 

Under the NCP, RRTs and ACs are 

required to address, as part of their 

planning activities, the desirability of 

using appropriate chemical or biological 

agents, or other spill mitigating devices. 

In addition, the OSC, under authority 

granted by the NCP, must respond to an 

oil spill in a diligent and effective 

manner to protect human health and the 

environment. If chemical or biological 

agents are needed, the OSC must 

coordinate with the RRT and ACs before 

their use is authorized. In all cases, the 

RRT, ACs and OSC will address a broad 

array of oil spill response and mitigation 

issues, including the potential for 

environmental justice concerns. 

Historically, EPA has not found any 

evidence that the use of chemical or 

biological agents on the Schedule on oil 

spills in the U.S. has had any 

disproportionate effect on any 

environmental justice communities. 

However, EPA will continue to monitor 

the implementation of the rule to ensure 

the planned or actual use of chemical or 

biological agents has no 

disproportionate effect on any EJ 

communities. 

EPA has determined that this 

proposed rule will not have 

disproportionately high and adverse 

human health or environmental effects 

on minority or low-income populations 

because it increases the level of 

environmental protection for all affected 

populations without having any 

disproportionately high and adverse 

human health or environmental effects 

on any population, including any 

minority or low-income population. 

Specifically, the proposed rule provides 

additional safeguards before any 

product can be listed on the Schedule, 

as well as allows OSCs and RRTs to 

request additional information to ensure 

that the use of any chemical or 

biological agent, or any other spill 

mitigating substance, in responding to 

oil discharges is protective of human 

health and the environment. This 

proposed rule is consistent with EPA’s 

Environmental Justice Strategy and the 

OSWER Environmental Justice Action 

Agenda. 

List of Subjects 

40 CFR Part 110 

Environmental protection, Oil 

pollution, and Reporting and 

recordkeeping requirements. 

40 CFR Part 300 

Air pollution control, Area 

contingency planning, Bioremediation, 

Chemicals, Dispersants, Environmental 

protection, Hazardous materials, 

Hazardous substances, 

Intergovernmental relations, Natural 

resources, Oil spills, Oil spill mitigating 

devices, Regional response teams, 

Sorbents, and Surface washing agents. 

Dated: January 9, 2015. 

Gina McCarthy, 

Administrator. 

For the reasons set out in the 

preamble, the Environmental Protection 

Agency proposes to amend 40 CFR parts 

110 and 300 to read as follows: 

PART 110—DISCHARGE OF OIL 

■ 1. The authority citation for part 110 

continues to read as follows: 

Authority: 33 U.S.C. 1321(b)(3) and (b)(4) 

and 1361(a); E.O. 11735, 38 FR 21243, 3 CFR 

parts 1971–1975 Comp., p. 793. 

■ 2. Revise § 110.4 and its section 

heading to read as follows: 

§ 110.4 Chemical or biological agents. 

Addition of any chemical or 

biological agent, as defined in § 300.5, to 

oil to be discharged that would 

circumvent the provisions of this part is 

prohibited. 

PART 300—NATIONAL OIL AND 

HAZARDOUS SUBSTANCES 

POLLUTION CONTINGENCY PLAN 

■ 3. The authority citation for part 300 

continues to read as follows: 

Authority: 33 U.S.C. 1321(c)(2); 42 U.S.C. 

9601–9657; E.O. 13626, 77 FR 56749, 3 CFR, 

2013 Comp., p. 306; E.O. 12777, 56 FR 54757, 

3 CFR, 1991 Comp., p. 351; E.O. 12580, 52 

FR 2923, 3 CFR, 1987 Comp., p. 193. 

Subpart A—Introduction 

■ 4. Amend § 300.5 by: 

■ a. Adding in alphabetical order the 

definitions of ‘‘Bioaccumulation’’, 

‘‘Bioconcentration’’, ‘‘Biodegradation’’, 

‘‘Biological agents’’, and 

‘‘Bioremediation’’; 

■ b. Revising the definitions of 

‘‘Bioremediation agents’’, ‘‘Burning 

agents’’, ‘‘Chemical agents’’, and 

‘‘Dispersants’’; 

■ c. Adding in alphabetical order the 

definition of ‘‘Herding agents’’; 

■ d. Removing the definitions for 

‘‘Miscellaneous oil spill control agent’’; 

■ e. Adding in alphabetical order the 

definition of ‘‘Products’’; 

■ f. Revising the definition of ‘‘Sinking 

agents’’; 

■ g. Adding in alphabetical order the 

definition of ‘‘Solidifiers’’; and 

■ h. Revising the definition of 

‘‘Sorbents’’ 

■ i. Removing the definition for 

‘‘Surface collecting agents’’. 

■ j. Revising the definition title ‘‘Surface 

washing agent’’ and its definition; 

The revisions and additions read as 

follows: 


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§ 300.5 Definitions. 

* * * * * 

Bioaccumulation is the process of 

accumulation of chemicals in the tissue 

of organisms through any route, 

including respiration, ingestion, or 

direct contact with the ambient or 

contaminated medium. 

Bioconcentration is the accumulation 

of chemicals in the tissues of organisms 

from water alone. 

Biodegradation is a process by which 

microorganisms metabolically 

decompose contaminants into biomass 

and simpler compounds such as carbon 

dioxide, water, and innocuous end 

products. 

Biological agents are microorganisms 

(typically bacteria, fungi, or algae) or 

biological catalysts, such as enzymes, 

able to enhance the biodegradation of a 

contaminated environment. 

Bioremediation is the process of 

enhancing the ability of microorganisms 

to convert contaminants into biomass 

and innocuous end products by the 

addition of materials into a 

contaminated environment to accelerate 

the natural biodegradation process. 

Bioremediation agents are biological 

agents and/or nutrient additives 

deliberately introduced into a 

contaminated environment to increase 

the rate of biodegradation and mitigate 

any deleterious effects caused by the 

contaminant constituents. 

Bioremediation agents include 

microorganisms, enzymes, and nutrient 

additives such as fertilizers containing 

bioavailable forms of nitrogen, 

phosphorus and potassium. 

Burning agents are additives that 

improve the combustibility of the 

materials to which they are applied 

through physical or chemical means. 

* * * * * 

Chemical agents are elements, 

compounds, or mixtures designed to 

facilitate the removal of oil from a 

contaminated environment and mitigate 

any deleterious effects. Chemical agent 

categories include burning agents, 

dispersants, herding agents, sinking 

agents, solidifiers, surface washing 

agents, and bioremediation agents that 

consist of nutrient additives. 

* * * * * 

Dispersants are typically mixtures of 

solvents, surfactants, and additives that 

promote the formation of small droplets 

of oil in the water column by reducing 

the oil-water interfacial tension. 

* * * * * 

Herding agents are substances that are 

used to control the spreading of the oil 

across the water surface. 

* * * * * 

Products are chemical or biological 

agents manufactured using a unique 

composition or formulation. 

* * * * * 

Sinking agents are substances 

deliberately introduced into an oil 

discharge for the purpose of submerging 

the oil to the bottom of a water body. 

* * * * * 

Solidifiers are substances that through 

a chemical reaction cause oil to become 

a cohesive mass, preventing oil from 

dissolving or dispersing into the water 

column, and which are collected and 

recovered from the environment. 

Sorbents are inert, insoluble 

substances that readily absorb and/or 

adsorb oil or hazardous substances, and 

that are not combined with or act as a 

chemical or biological agent. Sorbents 

are generally collected and recovered 

from the environment. Sorbents may be 

used in their natural bulk form, or as 

manufactured products in particulate 

form, sheets, rolls, pillows, or booms. 

Sorbents consist of: 

(1) Natural organic substances (e.g., 

feathers, cork, peat moss, and cellulose 

fibers such as bagasse, corncobs, and 

straw); 

(2) Inorganic/mineral compounds 

(e.g., volcanic ash, perlite, vermiculite, 

zeolite, clay); and 

(3) Synthetic compounds (e.g., 

polypropylene, polyethylene, 

polyurethane, polyester). 

* * * * * 

Surface washing agents are substances 

that separate oil from solid surfaces, 

such as beaches, rocks, metals, or 

concrete, through a detergency 

mechanism that lifts and floats oil for 

collection and recovery from the 

environment with minimal dissolution, 

dispersion, or transfer of oil into the 

water column. 

* * * * * 

Subpart J—Use of Dispersants, and 

Other Chemical and Biological Agents 

■ 5. Revise the heading of Subpart J as 

set out above. 

■ 6. Amend § 300.900 by revising 

paragraphs (a) and (c), and by adding 

paragraph (d) to read as follows: 

§ 300.900 General. 

(a) Section 311(d)(2)(G) of the Clean 

Water Act (CWA) requires EPA to 

prepare a schedule identifying 

dispersants, other chemicals, other spill 

mitigating devices and substances if 

any, that may be used in carrying out 

the NCP; and the waters and quantities 

in which they may be used. This 

subpart establishes a schedule 

identifying chemical and biological 

agents, and procedures that, when taken 

together, identify the waters and 

quantities in which such dispersants, 

other chemicals, or other spill 

mitigating devices and substances may 

be used. 

* * * * * 

(c) This subpart applies to the use of 

chemical and biological agents as 

defined in Subpart A of this part, or 

other substances that may be used to 

remove, control, or otherwise mitigate 

oil discharges. 

(d) [Reserved] 

§ 300.905 [Removed] 

■ 7. Remove § 300.905. 

■ 8. Revise § 300.910 and the section 

heading to read as follows: 

§ 300.910 Authorization for agent use. 

Use of chemical or biological agents 

in response to oil discharges to waters 

of the U.S. or adjoining shorelines must 

be authorized by the OSC in accordance 

with the provisions of this section: 

(a) Use of Agents Identified on the 

Schedule on Oil Discharges Addressed 

by a Preauthorization Plan. RRTs and 

Area Committees shall address in a 

preauthorization plan, as part of their 

planning activities, whether the use of 

chemical and biological agents listed on 

the Schedule on certain oil discharges is 

appropriate. RRTs and Area Committees 

shall, as appropriate, include applicable 

approved preauthorization plans in 

RCPs and ACPs. When a 

preauthorization plan is approved in 

advance for the use of certain agents 

under specified discharge situations, 

then the OSC may authorize the use of 

agents on the Schedule for their 

intended purpose without obtaining the 

incident specific concurrences 

described in paragraph (b) of this 

section. 

(1) Preauthorization Plan 

Development. For discharge situations 

identified where such agents may be 

used, the preauthorization plan must 

specify limits for the quantities and the 

duration of use, and use parameters for 

water depth, distance to shoreline, and 

proximity to populated areas. In 

meeting the provisions of this 

paragraph, preauthorization plans 

should document how regional factors 

are addressed including likely sources 

and types of oil that might be 

discharged, various discharge scenarios, 

the existence and location of 

environmentally sensitive resources or 

restricted areas that might be impacted 

by discharged oil, and logistical factors 

including inventory, storage locations 

and manufacturing capability of 

available agents, availability of 

equipment needed for agent use, 

availability of adequately trained 


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operators, and means to monitor agent 

use in the environment. 

(2) Preauthorization Plan Approval. 

The EPA representative to the RRT, the 

Department of Commerce and the 

Department of the Interior natural 

resource trustees and, as appropriate the 

RRT representative from the state(s) 

with jurisdiction over waters and 

adjoining shorelines within the 

preauthorization plan area shall review 

and either approve, approve with 

modification, or disapprove the 

preauthorization plans developed by the 

RRT and/or the Area Committees. 

Withdrawal of concurrence means the 

preauthorization plan becomes invalid 

and the authorization of use for 

chemical or biological agents must be 

performed according to paragraph (b) of 

this section. The RRTs and Area 

Committees shall address the 

withdrawal and the RRT shall notify the 

NRT of the final status of the 

preauthorization plan within 30 days 

from withdrawal. 

(3) Preauthorization Plans Reviews. 

The RRT and/or the Area Committees 

must review, and revise as needed, 

preauthorization plans at least every 5 

years; after a major discharge or after a 

Spill of National Significance (SONS); 

to address revisions of the Schedule; to 

reflect new listings of threatened and/or 

endangered species; and to address any 

other change that may impact the 

conditions under which the use of 

chemical and biological agents is 

preauthorized. The designated EPA RRT 

representative, the Department of 

Commerce and the Department of the 

Interior natural resource trustees, and 

the RRT representative from the state(s) 

with jurisdiction over the waters of the 

area to which a preauthorization plan 

applies shall review and either approve, 

approve with modification, or 

disapprove any revisions to the 

preauthorization plans. 

(b) Use of Agents Identified on the 

Schedule on Oil Discharges Not 

Addressed by a Preauthorization Plan. 

For discharge situations that are not 

addressed by the preauthorization plan 

developed pursuant to paragraph (a) of 

this section, the OSC may authorize the 

use of appropriate chemical or 

biological agents identified on the 

Schedule for their intended purpose on 

an oil discharge with the concurrence of 

the designated EPA RRT representative 

and, as appropriate, the concurrence of 

the RRT representatives from the state(s) 

with jurisdiction over the waters and 

adjoining shorelines threatened by the 

release or discharge, and in consultation 

with the Department of Commerce and 

the Department of the Interior natural 

resource trustees. In meeting the 

provisions of this paragraph, the OSC 

must consider and document the 

parameters for the use of agents 

including the quantities to be used, the 

duration of use, the depth of water, the 

distance to shoreline and proximity to 

populated areas, and should address 

factors such as environmentally 

sensitive resources or restricted areas 

that might be impacted, agent inventory 

and storage locations, agent 

manufacturing capability, availability of 

equipment needed for agent use, 

availability of adequately trained 

operators and appropriate means to 

monitor agent use in the environment. 

(c) Burning Agents. For authorized insitu burns, the OSC may authorize the 

use of burning agents. 

(d) Exception. The OSC may authorize 

the use of any chemical or biological 

agent, whether it is identified or not on 

the Schedule, without obtaining the 

immediate concurrence of the 

designated EPA RRT representative and, 

as appropriate, the RRT representatives 

from the state(s) with jurisdiction over 

the waters and adjoining shorelines 

threatened by the release or discharge, 

when, in the judgment of the OSC, the 

use of the agent is necessary to prevent 

or substantially reduce a threat to 

human life. If an OSC authorizes the use 

of an agent pursuant to this paragraph, 

he or she shall immediately notify, and 

document the circumstances requiring 

and the reasons for use of the agent to 

the EPA RRT representative and, as 

appropriate, the RRT representatives 

from the affected state(s) and, the 

Department of Commerce/Department of 

the Interior natural resources trustees. 

Use of any agent beyond 48 hours under 

this exception shall be in accordance 

with paragraphs (a) or (b) of this section. 

(e) Prohibited Agents. 

Notwithstanding paragraph (d) of this 

section, the OSC may not authorize the 

use of the following: 

(1) Sinking agents, or any other 

chemical agent, biological agent, or any 

substance that acts as a sinking agent 

when mixed with oil; and 

(2) Chemical or biological agents that 

have either nonylphenol (NP) or 

nonylphenol ethoxylates (NPEs) as 

components. 

(f) Storage and Use of Agents. The 

OSC may authorize for use only 

products that are certified by the 

responsible party to have been stored 

under the conditions provided by the 

submitter under § 300.915(a)(6) and 

whose date of use does not exceed the 

expiration date listed on the container’s 

label at the time of the incident. The 

responsible party must provide the OSC 

product documentation, developed in 

consultation with the submitter of the 

product to the Schedule, prior to OSC 

authorization of product use affirming it 

has maintained its integrity, including 

no changes in its composition, efficacy, 

and toxicity. The owner or operator of 

a facility or vessel must ensure samples 

of the expired product lot are tested 

following the applicable testing 

protocols in Appendix C, and that they 

are representative of all storage 

conditions at any end user location. If 

testing demonstrates the expired 

product has maintained its integrity, the 

product may be used for an additional 

5 years from the date of the testing 

described above. The responsible party, 

or its representative, must re-label the 

tested product lots and maintain test 

results and document all of the 

information under § 300.915(a)(17) and 

(a)(18) until used. The owner or 

operator of a facility or vessel must 

ensure the testing of re-labeled products 

every 5 years. 

(g) Supplemental Testing, Monitoring 

and Information. The RRT may require 

supplementary toxicity and efficacy 

testing, or available data or information 

that addresses site, area, or ecosystem 

specific concerns relative to the use of 

a product for both planning and 

authorization of use. During a discharge 

incident, the RRT may request that the 

OSC require a responsible party to 

conduct additional monitoring 

associated with the use of a product. 

Such additional monitoring data may 

include supplemental toxicity and 

efficacy testing or submission of 

available data or information that 

addresses the discharge area or 

ecosystem specific concerns relative to 

the use of a product or that aids the OSC 

and/or the RRT in operational decisions. 

(h) Recovery of Agents from the 

Environment. Depending on factors 

such as the safety of response personnel 

and harm to the environment, and as 

directed by the OSC, the responsible 

party shall ensure that any removal 

action adequately contains, collects, 

stores and disposes of agents that are 

intended to be recovered from the 

environment. 

(i) Reporting of Agent Use. Unless 

already included in the OSC report 

required under § 300.165 of this part, 

within 30 days of completion of agent 

operations, the authorizing OSC shall 

provide the RRT the following 

information on chemical and biological 

agents used in response to an oil 

discharge: product name, quantity and 

concentration used, duration of use, 

locations, and any data collected and 

analysis of efficacy or environmental 

effects. 

■ 9. Add § 300.913 to read as follows: 


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§ 300.913 Monitoring the use of 

dispersants. 

As directed by the OSC, the 

responsible party must monitor any 

subsurface use of dispersant in response 

to an oil discharge, surface use of 

dispersant in response to oil discharges 

of more than 100,000 U.S. gallons 

occurring within 24 hours, and surface 

use of dispersant for more than 96 hours 

in response to an oil discharge, and 

submit a Quality Assurance Project Plan 

for approval to the OSC covering the 

collection of all environmental data. 

When these dispersant use conditions 

are met, and for the duration of 

dispersant operations, the responsible 

party shall: 

(a) Document the characteristics of the 

source oil; best estimate of the oil 

discharge flow rate, periodically 

reevaluated as conditions dictate, 

including a description of the method, 

associated uncertainties, and materials; 

dispersant(s) product used, rationale for 

dispersant product choice(s) including 

the results of any efficacy and toxicity 

tests specific to area or site conditions, 

recommended dispersant-to-oil ratio 

(DOR); and the application method and 

procedures, including a description of 

the equipment to be used, hourly 

application rates, capacities, and total 

amount of dispersant needed. For 

subsurface discharges also document 

the best estimate of the discharge flow 

rate of any associated volatile petroleum 

hydrocarbons, periodically reevaluated 

as conditions dictate, including a 

description of the method, associated 

uncertainties, and materials. 

(b) In areas not affected by the 

discharge of oil, collect a representative 

set of background water column 

samples following standard operating 

and quality assurance procedures, at the 

closest safe distance from the discharge 

as determined by the OSC and in any 

direction of likely transport considering 

surface and subsurface currents and oil 

properties for the variables listed below. 

In the dispersed oil plume, collect daily 

water column samples following 

standard operating and quality 

assurance procedures, at such depths 

and locations where dispersed oil is 

likely to be present and analyze for: 

(1) In-situ oil droplet size distribution, 

including mass or volume mean 

diameter for droplet sizes ranging from 

2.5 to 2,000 mm, with the majority of 

data collected between the 2.5 and 100 

mm size; 

(2) In-situ fluorometry and 

fluorescence signatures targeted to the 

type of oil discharged and referenced 

against the source oil; 

(3) Dissolved oxygen (DO); 

(4) Total petroleum hydrocarbons, 

individual resolvable constituents 

including volatile organic compounds, 

aliphatic hydrocarbons, monocyclic, 

polycyclic, and other aromatic 

hydrocarbons including alkylated 

homologs, and hopane and sterane 

biomarker compounds; 

(5) Carbon dioxide (CO2) (subsurface 

only); 

(6) Methane, if present (subsurface 

only); 

(7) Heavy metals, including nickel 

and vanadium; 

(8) Turbidity; 

(9) Water temperature; 

(10) pH; and 

(11) Conductivity. 

(c) In consultation with the OSC, and 

using best available technologies, 

characterize the dispersant effectiveness 

and oil distribution, considering the 

condition of oil, dispersant, and 

dispersed oil components from the 

discharge location; 

(d) In consultation with the OSC, 

characterize the ecological receptors 

(e.g. aquatic species, wildlife, and/or 

other biological resources) and their 

habitats that may be present in the 

discharge area and their exposure 

pathways. Include those species that 

may be in sensitive life stages, transient 

or migratory species, breeding or 

breeding-related activities (e.g., embryo 

and larvae development), and 

threatened and/or endangered species 

that may be exposed to the oil that is not 

dispersed, the dispersed oil, and the 

dispersant alone. Estimate an acute 

toxicity level of concern for the 

dispersed oil using available dose/

response information relevant to 

potentially exposed species. 

(e) Immediately report to the OSC 

any: 

(1) Deviation of more than 10 percent 

from the mean hourly dispersant use 

rate for subsurface application, based on 

the dispersant volume authorized for 24 

hours use, and the reason for the 

deviation; and 

(2) Ecological receptors, including any 

threatened or endangered species that 

may be exposed based on dispersed 

plume trajectory modeling and level of 

concern information. 

(f) Report daily to the OSC water 

sampling and data analyses collected in 

§ 300.913(b) and include: 

(1) Specific hourly dispersant 

application rate and the total amount of 

dispersant used for the previous 

reporting period established by the OSC 

with concurrence from the EPA 

representative to the RRT; 

(2) All collected data and analyses of 

those data within a timeframe necessary 

to make operational decisions (e.g., 

within 24 hours of collection), including 

documented observations, photographs, 

video, and any other information related 

to dispersant use, unless an alternate 

timeframe is authorized by the OSC; 

(3) For analyses that take more than 

24 hours due to analytical methods, 

provide such data and results within 5 

days, unless an alternate timeframe is 

authorized by the OSC; and 

(4) Estimates of the daily transport of 

dispersed and non-dispersed oil and 

associated volatile petroleum 

hydrocarbons, and dispersants, using 

the best available trajectory modeling. 

■ 10. Revise § 300.915 and the section 

heading to read as follows: 

§ 300.915 Data and information 

requirements for Product Schedule listing. 

If you are submitting an application 

for listing a product to the Schedule, 

you must provide EPA the information 

required under § 300.955. Your 

submission must contain: 

(a) General Information for any 

Product Category. (1) Your name, 

physical address, email, and telephone 

number; 

(2) Your identity as the manufacturer 

of the product, a vendor, importer, or 

distributor of the product, and/or a 

designated agent acting on behalf of the 

manufacturer. Provide documentation of 

such identity; 

(3) All name(s), brand(s), and/or 

trademark(s) under which the product is 

to be sold; 

(4) Names, physical addresses, emails 

and telephone numbers of the primary 

distributors, vendors, importers, and/or 

designated agent acting on behalf of the 

manufacturer; 

(5) A Safety Data Sheet (SDS) for the 

product; 

(6) The maximum, minimum and 

optimum temperature, humidity and 

other relevant conditions for product 

storage and a brief description of the 

consequences to performance if the 

product is not stored within these 

limits; 

(7) The anticipated shelf life of the 

product at the storage conditions noted 

in paragraph (a)(6) of this section and 

documentation for this determination; 

(8) A sample product label for all 

name(s), brand(s), and/or trademark(s) 

under which the product is to be sold 

that includes manufacture and 

expiration dates, and conditions for 

storage. You may use an existing label 

provided it already contains the 

required dates and storage information; 

(9) The chemical or biological agent 

category under which you want the 

product to be considered for listing on 

the Schedule, including detailed 

information on the specific process(es) 


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through which the product affects the 

oil, and the specific environment(s) 

(waters and/or adjoining shorelines) on 

which it is intended to be used. If your 

product meets the definition of more 

than one chemical or biological agent 

category and you want it considered for 

listing on the Schedule in more than 

one category, you must identify all 

applicable categories and provide the 

test data to meet the listing criteria 

appropriate to each category; 

(10) Recommended product use 

procedures, including product 

concentrations, use ratios, types of 

application equipment, conditions for 

use, and any application restrictions. 

These procedures must address, as 

appropriate, variables such as weather, 

water salinity, water temperature, types 

and weathering states of oils or other 

pollutants, and product and oil 

containment, collection, recovery and 

disposal, and include supporting 

documentation and standard methods 

used to determine them; 

(11) Environmental fate information, 

including any known measured data 

and supporting documentation, on the 

persistence, bioconcentration factor, 

bioaccumulation factor, and 

biodegradability of the product and all 

of its components in the environment; 

(12) The physical/chemical properties 

of the product, as appropriate, and a 

citation for the standard methods used 

to determine them, including: 

(i) Physical state and appearance; 

(ii) Vapor pressure; 

(iii) Flash point; 

(iv) Pour point; 

(v) Viscosity; 

(vi) Specific gravity; 

(vii) Particle size for solid 

components; and 

(viii) pH. 

(13) The identity and concentration of 

all components in the product, 

including each specific component 

name; corresponding Chemical Abstract 

Service (CAS) Registry Number; the 

maximum, minimum, and average 

weight percent of each component in 

the product; and the intended function 

of each component (e.g., solvent, 

surfactant); 

(14) For products that contain 

microorganisms, enzymes and/or 

nutrients, provide the following along 

with a citation or a description of the 

methodology used to determine: 

(i) The name of all microorganisms by 

current genus and species, including 

any reclassifications, and any physical, 

chemical, or biological technique used 

to manipulate the genetic composition 

and the weight percent of each genus in 

the product; 

(ii) The name of all enzymes and their 

International Union of Biochemistry 

(I.U.B.) number(s); Enzyme 

Classification (EC) code numbers; the 

source of each enzyme; units; and 

specific oil-degrading activity; 

(iii) The name(s), maximum, 

minimum, and average weight percent 

of the nutrients contained in the 

product; and 

(iv) Certification, including data, 

methodology, and supporting 

documentation, indicating that the 

product does not contain, at levels that 

exceed the National Ambient Water 

Quality Criteria lowest density value, 

bacterial, fungal, or viral pathogens or 

opportunistic pathogens including, but 

not limited to: enteric bacteria such as 

Salmonella, fecal coliforms, Shigella, or 

Coagulase positive Staphylococci, and 

Beta Hemolytic Streptococci and 

enterococci. 

(15) Certification, including data, 

methodology, and supporting 

documentation, indicating that the 

product does not contain, at levels 

above National Water Quality Standards 

lowest acute value for aquatic life: 

(i) Arsenic, cadmium, chromium, 

copper, lead, mercury, nickel, 

vanadium, zinc, and any other heavy 

metal reasonably expected to be in the 

product; 

(ii) Cyanide; 

(iii) Chlorinated hydrocarbons; 

(iv) Pesticides; 

(v) Polychlorinated Biphenyls (PCBs); 

and 

(vi) Polynuclear aromatic 

hydrocarbons (PAHs). 

(16) Certification, including data, 

methodology, and supporting 

documentation, indicating that the 

product does not contain any of the 

prohibited agents identified in 

§ 300.910(e); 

(17) Information about the laboratory 

that conducted the required tests, 

including: 

(i) Name of the laboratory, address, 

contact name, email, and phone 

number; and 

(ii) The national and/or international 

accreditations held by the laboratory. 

(18) All test data and calculations, 

including: 

(i) Raw data and replicates, including 

positive controls; 

(ii) Notes and observations collected 

during tests; 

(iii) Calculated mean values and 

standard deviations; 

(iv) Reports, including a summary of 

stock solution preparation; 

(v) Source and preparation of test 

organisms; 

(vi) Test conditions; and 

(vii) Chain of custody forms. 

(19) An estimate of the annual 

product production volume, the average 

and maximum amount that could be 

produced per day, and the time frame 

needed to reach that maximum 

production rate (days); 

(20) Recognition received from EPA’s 

Design for the Environment (DfE) if 

applicable; and 

(21) International product testing or 

use data or certifications, if available, 

informing the performance capabilities 

or environmental benefits of the 

product. 

(b) Dispersant Testing and Listing 

Requirements—(1) Dispersant Efficacy 

test and listing criteria. Test the 

dispersant product for efficacy using the 

Baffled Flask Test (BFT) method in 

Appendix C to part 300. To be listed on 

the Schedule, the dispersant must 

demonstrate for each oil and 

temperature a Dispersant Effectiveness 

(DE) at the 95% lower confidence level 

(LCL95) greater than or equal to: 

(i) 55% for Intermediate Fuel Oil 120 

(IFO–120) at 5 °C; 

(ii) 65% for IFO–120 at 25 °C; 

(iii) 70% for Alaska North Slope 

(ANS) crude oil at 5 °C; and 

(iv) 75% for ANS at 25 °C. 

(2) Dispersant Toxicity tests and 

listing criteria. Use the methods 

specified in Appendix C to part 300 to 

test the dispersant alone, the dispersant 

mixed with ANS, and the dispersant 

mixed with IFO–120 for acute toxicity, 

using Americamysis bahia and Menidia 

beryllina. Use the methods specified in 

Appendix C to part 300 to test the 

dispersant alone for developmental 

toxicity using a sea urchin assay and for 

sub-chronic effects using Americamysis 

bahia and Menidia beryllina. To be 

listed on the Schedule, the lethal 

concentration for 50% of the test species 

(LC50) at the lower 95% confidence 

interval for all acute toxicity tests must 

be greater than 10 ppm; the inhibition 

concentration for 50% of the test species 

(IC50) at the lower 95% confidence 

interval must be greater than 10 ppm; 

and the sub-chronic No Observed Effect 

Concentration (NOEC) must be equal to 

or greater than 1 ppm. 

(3) Limitations. Product listing would 

be for use only in saltwater 

environments. 

(c) Surface Washing Agent Testing 

and Listing Requirements— 

(1) Surface Washing Agent Efficacy 

test and listing criteria. To be listed on 

the Schedule, using a recognized 

standard methodology, the surface 

washing agent must meet an efficacy of 

greater than or equal to 30% in either 

fresh or saltwater or both depending on 

the intended product use. 


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3426 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

(2) Surface Washing Agent Toxicity 

test and listing criteria. Using the 

toxicity test methodology in Appendix 

C to part 300, test the surface washing 

agent for acute toxicity against fresh 

water species Ceriodaphnia dubia and 

Pimephales promelas, or saltwater 

species Americamysis bahia and 

Menidia beryllina, or both, depending 

on the intended product use. To be 

listed on the Schedule, the surface 

washing agent must demonstrate an 

LC50 at the lower 95% confidence 

interval of greater than 10 ppm in either 

fresh or saltwater for all tested species. 

(3) Limitations. Based on testing, 

product listing would be for use only in 

the fresh and/or saltwater environments 

for which it was tested and for which it 

met the efficacy and toxicity listing 

criteria. 

(d) Bioremediation Agent Testing and 

Listing Requirements—(1) 

Bioremediation Agent Efficacy test and 

listing criteria. To be listed on the 

Schedule, a bioremediation agent must 

successfully degrade both alkanes and 

aromatics as determined by gas 

chromatography/mass spectrometry 

(GC/MS) in salt or fresh water or both, 

depending on the intended product use, 

following the test method specified in 

Appendix C to part 300. The percentage 

reduction of total alkanes (aliphatic 

fraction) from the GC/MS analysis must 

be greater than or equal to 95% at day 

28, based on the ninety-fifth percentile 

Upper Confidence Limit (UCL95) for 

both salt and freshwater. The percentage 

reduction of total aromatics (aromatic 

fraction) must be greater than or equal 

to 70% at day 28 for saltwater and 

greater than or equal to 40% for 

freshwater based on the UCL95. 

(2) Bioremediation Agent Toxicity test 

and listing criteria. The bioremediation 

agent must be tested for acute toxicity 

in saltwater, freshwater or both, 

depending on the intended product use, 

following the method specified in 

Appendix C to part 300. To be listed on 

the Schedule, the bioremediation agent 

must demonstrate an LC50 at the lower 

95% confidence interval of greater than 

10 ppm in either fresh or saltwater for 

all tested species. 

(3) Limitations. Based on testing, 

product listing would be for use only in 

the fresh and/or saltwater environments 

for which it was tested and for which it 

met the efficacy and toxicity listing 

criteria. 

(4) Exceptions. If the product consists 

solely of: ammonium nitrate, 

ammonium phosphate, ammonium 

sulfate, calcium ammonium nitrate, 

sodium nitrate, potassium nitrate, 

synthetically-derived urea, sodium 

triphosphate (or tripolyphosphate), 

sodium phosphate, potassium 

phosphate (mono- or dibasic), triple 

super phosphate, potassium sulphate, or 

any combination thereof, no technical 

product data are required, are 

generically listed as non-proprietary 

nutrients on the Schedule, and no 

further action is necessary. 

(e) Solidifier Testing and Listing 

Requirements. (1) Solidifiers must be 

tested for acute toxicity in saltwater, 

freshwater or both, depending on the 

intended product use, following the 

method specified in Appendix C to part 

300. To be listed on the Schedule, the 

solidifier must demonstrate an LC50 at 

the lower 95% confidence interval of 

greater than 10 ppm in either fresh or 

saltwater for all tested species. 

(2) Limitations. Based on testing, 

product listing would be for use only in 

the fresh and/or saltwater environments 

for which it was tested and for which it 

met the toxicity listing criteria. 

(f) Herding Agent Testing and Listing 

Requirements. (1) Herding agents must 

be tested for acute toxicity in saltwater, 

freshwater, or both, depending on the 

intended product use, following the 

method specified in Appendix C to part 

300. The herding agent must 

demonstrate an LC50 at the lower 95% 

confidence interval of greater than 10 

ppm in either fresh or saltwater for all 

tested species. 

(2) Limitations. Based on testing, 

product listing would be for use only in 

fresh and/or saltwater environments for 

which it was tested and for which it met 

the toxicity listing criteria. 

(g) Sorbent Requirements. Known 

sorbent materials and products will be 

identified on a publicly available 

Sorbent Product List for the use of such 

products when responding to an oil 

discharge as follows: 

(1) For sorbent products that consist 

solely of the following materials, or any 

combination thereof, no technical data 

are required and no further action is 

necessary for use as a sorbent: 

(i) Feathers, cork, peat moss, and 

cellulose fibers such as bagasse, 

corncobs, and straw; 

(ii) Volcanic ash, perlite, vermiculite, 

zeolite, and clay; and 

(iii) Polypropylene, polyethylene, 

polyurethane, and polyester. 

(2) If the product consists of one or 

more natural organic substances, 

inorganic/mineral compounds, and/or 

synthetic compounds not specifically 

identified in paragraph (g)(1) of this 

section but you believe the product 

meets the definition of a sorbent then, 

as applicable under § 300.955(a) and (b), 

you must submit the following 

information for consideration for listing 

it as a sorbent on the Sorbent Product 

List: 

(i) The information required under 

paragraphs (a)(1) through (8), and 

paragraph (a)(13) of this section; 

(ii) The certifications required under 

paragraphs (a)(14)(iv), (a)(15), and 

(a)(16) of this section; and 

(iii) Information, including data, to 

support the claim your product meets 

the sorbent definition under § 300.5. 

§ 300.920 [Removed] 

■ 11. Remove § 300.920. 

■ 12. Add § 300.950 to subpart J to read 

as follows: 

§ 300.950 Submission of Confidential 

Business Information (CBI). 

(a) Except as provided in paragraph 

(b) of this section, all product 

information submitted to EPA as 

required under § 300.915 will be 

disclosed to the public. 

(b) You may only claim the 

concentration and the maximum, 

minimum, and average weight percent 

of each chemical component or 

microorganism in your product, as 

identified in § 300.915(a)(13) or (14), to 

be CBI. EPA will handle such claims in 

accordance with 40 CFR part 2, subpart 

B. 

(1) You must make your CBI claim at 

the time you submit your information to 

EPA to be listed on the Schedule. 

(2) You must redact the CBI from all 

submitted information but include the 

CBI separately with your submission 

package. Clearly identify and mark the 

information as ‘‘Confidential Business 

Information’’ and place it in a separate 

inner envelope in your submission 

package labeled with ‘‘CONFIDENTIAL 

BUSINESS INFORMATION—TO BE 

OPENED BY THE PRODUCT 

SCHEDULE MANAGER ONLY.’’ 

■ 13. Add § 300.955 to subpart J to read 

as follows: 

§ 300.955 Addition of a product to the 

Schedule. 

(a) Submission. Submit your complete 

package to: U.S. Environmental 

Protection Agency, 1200 Pennsylvania 

Ave. NW., Mail Code: 5104A, Room 

1448, William J. Clinton North, 

Washington, DC 20460, Attention: 

Product Schedule Manager. 

(b) Package contents. Your package 

shall include, in this order: 

(1) A cover letter on company 

letterhead signed and dated by you 

certifying that: 

(i) All testing was conducted on 

representative product samples; 

(ii) Testing was conducted at a 

nationally or internationally accredited 

laboratory in accordance with the 


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methods specified in Appendix C to 

part 300, and other applicable methods 

as appropriate; and 

(iii) All test results and product 

technical data and information are true 

and accurate. 

(2) A numbered Table of Contents 

showing the information and data 

submitted under § 300.915(a) through 

(g); 

(3) All required data and information 

arranged in the same order as specified 

in § 300.915(a) through (g); and 

(4) A separate envelope containing 

Confidential Business Information as 

specified in § 300.950(b), if applicable. 

(c) EPA Review. EPA shall, within 90 

days of receiving a submission package: 

(1) Review the package for 

completeness and compliance with all 

data and information requirements in 

§§ 300.915, 300.950, and this section, 

verify information, and request 

clarification or additional information 

as necessary; 

(2) Make a product listing 

determination based on a technical 

evaluation of all data and information 

submitted, relevant information on 

impacts or potential impacts of the 

product or any of its components on 

human health or the environment, and 

the intended use of the product. EPA 

reserves the right to make a 

determination on whether the product 

will be listed, and under which 

category; and 

(3) Notify you, in writing, of its 

decision to list the product on the 

Schedule and in which category or 

categories, or of its decision and 

supporting rationale to reject the 

submission. If your submission is 

rejected: 

(i) You may revise the submission 

package to address test results, data, or 

information deficiencies and resubmit 

it. 

(ii) EPA’s 90-day review will not start 

until a complete package is resubmitted. 

(d) Request for review of decision. If 

your product is rejected for listing on 

the Schedule, you may request that the 

EPA Administrator review the 

determination. Your request must be in 

writing within 30 days of receipt of 

notification of EPA’s decision not to list 

the product on the Schedule. Your 

request must contain a clear and concise 

statement with supporting facts and 

technical analysis demonstrating why 

you believe EPA’s decision was 

incorrect. 

(1) The EPA Administrator or 

designee may request additional 

information from you and may offer an 

opportunity for you to meet with EPA. 

(2) The EPA Administrator or his 

designee will notify you in writing of 

the decision within 60 days of receipt of 

your request, or within 60 days of 

receipt of requested additional 

information. 

(e) Changes to a product listing. You 

must notify EPA in writing within 30 

days of any changes to information 

submitted under § 300.915(a)(1) through 

(8) and § 300.915(a)(19) through (21) for 

a product on the Schedule. In the 

notification, you must detail the specific 

changes, the reasons for such changes 

and supporting data and information. 

EPA may request additional information 

and clarification regarding these 

changes. If you change the chemical 

components and/or concentrations, you 

must retest the reformulated product 

according to the requirements for the 

product category and submit a complete 

new package for a review and 

consideration for listing on the 

Schedule by EPA. 

(f) Transitioning Listed Products from 

the Current Schedule to the New 

Schedule. All products on the current 

Schedule as of [EFFECTIVE DATE OF 

FINAL RULE] will remain conditionally 

listed until [DATE 24 MONTHS FROM 

THE EFFECTIVE DATE OF FINAL 

RULE] at which time all products that 

have not submitted and been listed in 

the new Schedule based on the 

amended test and listing criteria will be 

removed. Your product will be 

transitioned from the current Schedule 

to the new Schedule prior to [DATE 24 

MONTHS FROM THE EFFECTIVE 

DATE OF FINAL RULE] after you 

submit a new, complete package 

according to the amended test and 

listing criteria and EPA makes a 

favorable finding to list the product on 

the new Schedule. 

■ 14. Add § 300.965 to subpart J to read 

as follows: 

§ 300.965 Mandatory product disclaimer. 

The listing of a product on the 

Schedule does not constitute approval 

or recommendation of the product. To 

avoid possible misinterpretation or 

misrepresentation, any label, 

advertisement, or technical literature for 

the product must display in its entirety 

the disclaimer shown below. The 

disclaimer must be conspicuous and 

must be fully reproduced on all product 

literatures, labels, and electronic media 

including Web site pages. 

DISCLAIMER [PRODUCT NAME] is 

listed on the National Contingency Plan 

(NCP) Product Schedule. This listing 

does NOT mean that EPA approves, 

recommends, licenses, or certifies the 

use of [PRODUCT NAME] on an oil 

discharge. This listing means only that 

data have been submitted to EPA as 

required by Subpart J of the NCP. Only 

a Federal On-Scene Coordinator (OSC) 

may authorize use of this product 

according to the NCP. 

■ 15. Add § 300.970 to subpart J to read 

as follows: 

§ 300.970 Removal of a product from the 

Schedule. 

(a) The EPA Administrator may 

remove your product from the Schedule 

for reasons including, but not limited to: 

(1) Misleading, inaccurate, or 

incorrect statements within the product 

submission to EPA or to any person or 

private or public entity regarding the 

composition or use of the product to 

remove or control oil discharges, 

including on labels, advertisements, or 

technical literature; or 

(2) Alterations to the chemical 

components, concentrations, or use 

conditions of the product without 

proper notification to EPA as required 

by § 300.955(e); or 

(3) Failure to print the disclaimer 

provided in § 300.965 on all labels, 

advertisements, or technical literature, 

or 

(4) New or previously unknown 

relevant information concerning the 

impacts or potential impacts of the 

product to human health or the 

environment. 

(b) EPA will notify you in writing, at 

your address of record, of its reasons for 

deciding to remove the product from the 

Schedule. If EPA receives no appeal 

from you in 30 days, the product will 

be removed from the Schedule without 

further notice to you. 

(c) You may appeal the decision to 

remove your product from the Schedule 

within 30 days of receipt of EPA’s 

notification. Your appeal must contain a 

clear and concise statement with 

supporting facts and technical analysis 

demonstrating why you believe EPA’s 

decision was incorrect. The EPA 

Administrator will notify you in writing 

of his decision within 60 days of your 

appeal, or within 60 days of receipt of 

any requested additional information. 

■ 16. Revise Appendix C to Part 300 and 

appendix heading to read as follows: 

Appendix C to Part 300—Requirements 

for Product Testing Protocols and 

Summary Test Data: Dispersant Baffled 

Flask Efficacy and Toxicity Tests; 

Standard Acute Toxicity Test for 

Bioremediation Agents, Surface 

Washing Agents, Herding Agents, and 

Solidifiers; and Bioremediation Agent 

Efficacy Test. 

Table of Contents 

1.0 Applicability and Scope 

2.0 Baffled Flask Dispersant Efficacy Test 

(BFT) 

3.0 Dispersant Toxicity Testing 


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4.0 Standard Acute Toxicity Testing for 

Surface Washing Agents, Bioremediation 

Agents, Herding Agents, and Solidifiers. 

5.0 Bioremediation Agent Efficacy Test 

Protocol 

Illustrations 

Figure Number 

1. A Baffled Trypsinizing Flask 

Tables 

Table Number 

1. Constituent Concentrations for GP2 

Artificial Seawater 

2. Test Oil Characteristics 

3. Stock Solution Preparation 

4. Dispersant Calibration Example for Both 

Oils 

5. Sample Calculation with ANS 

6. Toxicity Testing Requirements for 

Dispersants 

7. Summary of Test Conditions—Dispersant 

Toxicity 

8. Toxicity Testing Requirements for Surface 

Washing Agents, Herding Agents, 

Bioremediation Agents and Solidifiers 

9. Summary of Test Conditions—Surface 

Washing Agents, Herding Agents, 

Bioremediation Agents and Solidifiers 

Toxicity 

10. Artificial Seawater Nutrient 

Concentrations 

11. Artificial Seawater Nutrient 

Concentrations for Bioremediation Agents 

Having No Nutrients Included 

12. Constituent Concentrations for Artificial 

Freshwater (Bushnell-Haas) 

13. Freshwater Nutrient Concentrations 

14. Artificial Freshwater Nutrient 

Concentration for Bioremediation Agents 

Having No Nutrients Included 

15. Bioremediation Efficacy Test—Summary 

of Experimental Setup 

16. Bioremediation Efficacy—Summary of 

Analytical Procedures 

17. QA/QC Checks 

Standard Operating Procedures Tables 

SOP 3–1 Amount of Stock Solutions 

Required to Make the Working Standards 

SOP 4–1 Ions Associated With Retention 

Time Groups 

SOP 4–2 Instrumental Conditions for Crude 

Oil Analysis 

SOP 4–3 Ion Abundance Criteria for DFTPP 

SOP 4–4 Target Compound List 

1.0 Applicability and Scope. This 

Appendix establishes laboratory protocols 

required under Subpart J (Use of Dispersants 

and Other Chemical and Biological Agents) 

of 40 CFR part 300 (National Oil and 

Hazardous Substances Pollution Contingency 

Plan) to make listing determinations for the 

Product Schedule. The protocols apply, 

based on product type, to dispersants, 

bioremediation agents, surface washing 

agents, herding agents, and solidifiers as 

defined in Subpart A (Introduction) of 40 

CFR part 300. 

2.0 Baffled Flask Dispersant Efficacy Test 

(BFT) 

2.1 Summary. This laboratory protocol 

establishes procedures to evaluate the degree 

to which a product effectively disperses oil 

spilled on the surface of seawater, using a 

modified 150-mL screw-cap trypsinizing 

flask (an Erlenmeyer flask with baffles) with 

a glass and Teflon® stopcock near the bottom 

to allow removal of subsurface water samples 

without disturbing the surface oil layer. The 

efficacy of a dispersant is measured using 

two types of oils (Intermediate Fuel Oil 120 

and Alaska North Slope) at two temperatures 

(5 °C and 25 °C). Six replicates are required 

at each condition with two method blank 

replicates at each temperature. A layer of oil 

is placed on the surface of artificial seawater, 

and the dispersant is added to the slick at a 

dispersant:oil ratio (DOR) of 1:25 (4%) by 

volume. A standard orbital shaker table 

provides turbulent mixing at a speed of 250 

revolutions per minute (rpm) for 10 minutes, 

immediately after which it is maintained 

stationary for 10 minutes to allow nondispersed oil to rise to the water’s surface. An 

undisturbed water sample is removed from 

the bottom of the flask through the stopcock, 

extracted with dichloromethane (DCM), and 

analyzed for oil content by UV-visible 

absorption spectrophotometry at wavelengths 

ranging between 340 and 400 nm. 

2.2 Apparatus. All equipment must be 

maintained and calibrated per standard 

laboratory procedures. 

2.2.1 Modified Trypsinizing Flask. A 

modified 150 mL glass screw-capped 

Erlenmeyer flask with baffles (e.g., Wheaton 

No. 355394 or equivalent) fitted with a 2 mm 

bore Teflon® stopcock and glass tubing, the 

center of which is no more than 1.3 cm from 

the bottom, as shown in Figure 1. 


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2.2.2 Orbital Shaker Table. An orbital 

shaker table with a variable speed control 

unit capable of maintaining 250 rpm. The 

orbital diameter must be approximately 1.0 

inch (2.5 cm) +/¥ 0.1 inch (0.25 cm). 

2.2.3 Spectrophotometer. A UV-visible 

spectrophotometer capable of measuring 

absorbance between 340 and 400 nm (e.g., 

Shimadzu UV–1800, Agilent 8453, or 

equivalent). Use standard transmissionmatched quartz 10-mm path length 

rectangular cells with PTFE cover for 

absorbance measurements. 

2.2.4 Glassware. Including: 25-ml 

graduated mixing cylinders (a graduated 

cylinder with a ground glass stopper); 50- 

and 100-ml graduated cylinders; 125-mL 

separatory funnels with Teflon stopcocks; 10 

ml volumetric flasks; 30 ml crimp style glass 

serum bottles; 1-, 2-, 5-mL pipettes; other 

miscellaneous laboratory items. 

2.2.5 Micropipettor. Use a micropipettor 

capable of dispensing 4 mL of dispersant and 

100 mL of oil (e.g., Brinkmann Eppendorf 

repeater pipettor with 100 mL and 5 mL 

syringe tip attachments or equivalent). 

2.2.6 Syringes. 25-, 100-, 250-, 1000-, 

2500-, 5000- ml gas-tight syringes. 

2.2.7 Constant temperature rooms or 

incubators to hold the shaker at 5 °C and 25 

°C. 

2.2.8 Analytical Balance. 

2.2.9 Chemical fume hood. 

2.3 Reagents 

2.3.1 Artificial seawater. Use the artificial 

seawater GP2 formulation shown in Table 1 

of this Appendix. 

2.3.2 Test oils. Use the two EPA standard 

reference oils, Alaska North Slope oil (ANS) 

and Intermediate Fuel Oil 120 (IFO 120). To 

obtain these oils at no charge (except for a 

minimal shipping fee), see the instructions at 

http://www.epa.gov/emergencies/content/

ncp/index.htm. Selected properties are 

summarized in Table 2 of this Appendix. 

2.3.3 Dichloromethane (DCM) (also 

known as methylene chloride), pesticide 

quality. 

2.3.4 Positive Control Dispersant. 

Dispersant sample with a known, 

reproducible efficacy. To obtain this control 

sample at no cost (except for shipping), see 

the instructions at http://www.epa.gov/

emergencies/content/ncp/index.htm. 

2.4 Container Handling and Storage 

2.4.1 Glassware. If the glassware has been 

used with oil before, rinse with DCM to 

remove as much of the oil adhering to the 

sides of the flask as possible; waste DCM may 

be used. Soak in warm water with detergent 

and individually wash with bristled brushes. 

First rinse with tap water, then follow with 

two de-ionized water rinses. Dry either on a 

rack or in a 110 °C drying oven). After drying, 

rinse with fresh DCM (use sparingly). 

2.4.2 Serum bottles and other nonvolumetric glassware. Bake for at least 4 

hours in a muffle furnace at 450 °C. 

2.5 Calibration Curve for the UV-visible 

spectrophotometer 

2.5.1 Stock Standard Solution 

Preparation. Stock standard solution 

concentrations are based on the mass 

measurements after each addition and 

density determinations of the oil/dispersant/ 

DCM solution using a density bottle or a 1- 

mL gas tight syringe. An example calculation 

is given in Table 3 of this Appendix 

according to the following equation: 

Use the reference oils and the specific 

dispersant being tested for a particular set of 

experimental test runs. Prepare the stock 

solution of dispersant-oil mixture in DCM, 

starting with 2 ml of the oil, then adding 80 

ml of the dispersant followed by 18 ml of 

DCM. Two sets of standards are needed, one 

for each oil and dispersant combination. 

2.5.2 Six-point Calibration Curve. For 

each reference oil, add specific volumes of its 

stock standard solution (given in Table 4 of 

this Appendix) to 30 ml of artificial seawater 

in a 125 ml separatory funnel. Extract the oil/ 

water mixture with triplicate 5 ml volumes 

of DCM. Follow each DCM addition by 15 

seconds of vigorous shaking, carefully 

releasing the initial pressure inside the 

separatory funnel by partially removing the 

glass stopper inside a fume hood after the 

first few shakes. Then, allow a 2-minute 

stationary period for phase separation for 

each extraction. Drain the extracts into a 25- 

mL graduated mixing cylinder. Release any 

entrained bubbles of DCM from the water 

layer by sideways shaking of the funnel. Use 

precaution not to drain water into the DCM 

extract as it can affect the absorbance 

readings. Adjust the final volume of the 

collected extracts to 20 mL in the mixing 

cylinder using DCM. Determine specific 

masses for oil concentrations in the standards 

as volumes of oil/dispersant solution 

multiplied by the concentration of the stock 

solution. An example calculation is given in 

Table 4 of this Appendix. Two calibration 

curves are needed, one for each oil and 

dispersant combination. 

2.6 Sample Preparation and Testing. See 

section 2.7 of this Appendix for a detailed 

description of the spectrophotometer’s linear 

calibration procedure. 

2.6.1 Six replicates of each oil and test 

dispersant are required at each temperature 

plus two additional tests of method blanks 

(artificial seawater without oil and 

dispersant), one at each temperature. A 

completed test consists of 26 baffled flask 

tests (a total of six replicates for each of two 

reference oil/test dispersant combinations at 

two temperatures (5 °C and 25 °C), plus two 

method blanks). 

2.6.2 A positive control run of 6 

replicates of a dispersant with known 

dispersion efficacy (see 2.3.4 above for how 

to obtain) is prepared with both oils at both 

temperatures to verify the protocol is being 

correctly performed. The lab must certify that 

a positive control was successfully 

conducted within a year of any testing 

submitted for a dispersant listing. 

2.6.3 Attach a 3-inch length of Teflon 

tubing to the stopcock of each of the 150-mL 

baffled flasks. Add 120 mL of artificial 

seawater to each flask. Put screw cap on 

flasks and place them at the appropriate 

temperature (either 5 °C or 25 °C) for 

equilibration. 

2.6.4 Calibrate and adjust the shaker table 

to 250 ± 10 rpm. 

2.6.5 Prepare and time separately each 

baffled flask. Sequentially add 100 mL of oil 

and 4 mL of dispersant to the flask layering 

them onto the center of the seawater to give 

a dispersant-to-oil ratio (DOR) of 1:25. Avoid 

any oil or dispersant splashing on the flask 

walls, as it may reduce efficacy or cause 

errors in the calculated results. Discard the 

sample and repeat the setup if: (1) Any oil 

or dispersant splashing occurs during the 

additions, or (2) the dispersant contacts the 

water first rather than the oil. 

2.6.6 For the oil, fill the tip of the 

pipettor, using a wipe to remove any oil from 

the sides of the tip. Holding the pipettor 

vertically, dispense several times back into 

the reservoir to ensure that the oil flows 

smoothly. Insert the syringe tip vertically 

into the baffled flask, and let the bottom of 

the pipettor rest on the neck of the flask. 

Slowly and carefully dispense the oil one 

time onto the center of the water’s surface. 

IFO 120 takes longer to drip, and ANS will 

splash if dispensed too fast. The remainder 

of the oil can either be returned to the oil 

bottle or set aside for use in the next test 

flask. Note to 2.6.6: If a Brinkmann 

Eppendorf repeater pipettor is used for 

dispensing the oil, attach a 5-mL syringe tip, 

and set the dial to 1. 

2.6.7 For the dispersant, use the same 

procedure as for the oil to dispense onto the 

center of the oil slick surface. As the 

dispersant first contacts the oil, it will 

usually push the oil to the sides of the flask. 

Replace the screw cap onto the flask. 

Note to 2.6.7: If a Brinkmann Eppendorf 

repeater pipettor is used for dispensing the 

dispersant, attach a 100-mL syringe tip, and 

set the dial to 2. 

2.6.8 Carefully place flask securely onto 

the shaker and agitate for 10 ± 0.25 minutes 

at 250 ± 10 rpm. 

2.6.9 Remove the flask from the shaker 

table and allow a stationary, quiescent period 

of 10 ± 0.25 minutes to allow undispersed 

and/or recoalesced oil droplets to refloat to 

the surface. 

2.6.10 Carefully open the screw cap, then 

the stopcock at the bottom, and discard the 

first several mL of seawater into a waste 

beaker to remove non-mixed water-oil 

initially trapped in the stopcock tubing. 

Collect a volume slightly greater than 30-mL 

into a 50-mL graduated cylinder. Adjust the 

collected volume to the 30-mL mark by 


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removing excess with a disposable glass 

Pasteur pipette. A web-like emulsion may 

form at the solvent/water interface during the 

water sample extraction. Avoid pulling any 

emulsion phase into the DCM extract as it 

may cloud the DCM-extract leading to error. 

2.6.11 Transfer the water-oil sample from 

the graduated cylinder into a 125-mL glass 

separatory funnel fitted with a Teflon 

stopcock. 

2.6.12 Add 5 mL DCM to the separatory 

funnel. Start shaking, releasing pressure into 

the fume hood by loosening the glass stopper. 

Shake vigorously at least 20 times for 15 

seconds. 

2.6.13 Allow the funnel to remain in a 

stationary position for 2 minutes to allow 

phase separation of the water and DCM. 

2.6.14 Drain the DCM layer from the 

separatory funnel into a 25 mL mixing 

cylinder. Avoid pulling any emulsion phase 

into the DCM extract as it may cloud the 

DCM extract. 

2.6.15 Repeat the DCM-extraction process 

two or three additional times until the DCM 

is clear. Collect each extract in the graduated 

cylinder. After the final extraction, lightly 

shake the separatory funnel sideways once or 

twice to dislodge entrained bubbles of DCM 

and drain. 

2.6.16 Adjust the final volume to a 

known quantity, 20 or 25 mL, in the mixing 

cylinder. IFO 120 samples may require 

dilution when dispersed chemically because 

of their high absorbance properties. Using a 

syringe, dispense 2.5 mL or 5.0 mL of an IFO 

120 sample into a 10-mL volumetric flask, 

and fill with DCM to make either a 1:4 or 1:2 

dilution, respectively. ANS samples adjusted 

to 25 mL typically don’t require dilution. 

2.6.17 If analysis cannot be conducted 

immediately, store the extracted DCM 

samples at 4 °C until time of analysis. Glassstoppered mixing cylinders may be used for 

short-term storage or prior to bringing the 

extracts up to volume. After bringing to 

volume, transfer the DCM extracts to 25–30 

ml crimp-style serum vials with aluminum/ 

Teflon seals. 

2.6.18 Complete all analysis within 10 

consecutive days from when the sample was 

collected. 

2.7 UV-Visible Spectrophotometer Linear 

Stability Calibration 

2.7.1 A six-point calibration of the UVvisible spectrophotometer is required at least 

once per day for each oil. The stability 

calibration criterion is determined with the 

six oil standards identified in Table 4 of this 

Appendix. 

2.7.2 Turn on spectrophotometer and 

allow it to warm up for at least 30 minutes 

before beginning analysis. Blank the 

instrument for the wavelengths between 340 

and 400 nm with DCM. 

2.7.3 If refrigerated, allow all extracts, 

standards and samples to warm to room 

temperature. 

2.7.4 Determine the absorbance of the six 

standards between the wavelengths of 340 

and 400 nm. This can be done by either one 

of the following methods: 

2.7.4.1 Trapezoidal Rule. Program the 

spectrophotometer to take readings every 5l 

or 10l and calculate the area under the curve 

using the Trapezoidal rule: 

where N+1 = number of absorbance 

measurements to delineate N equally 

spaced sections of the curve, and H = the 

distance (l) between each reading. For H 

= 5, N+1 = 13 measurements, for H = 10, 

N+1 = 7. The following formula 

illustrates readings taken every 10l. 

When using readings taken every 5l, each 

absorbance sum is multiplied by 5. 

2.7.4.2 Automatic Integration. Program 

the spectrophotometer to automatically 

integrate the area under the curve between 

340 nm and 400 nm. 

2.7.4.3 If the wavelengths must be 

manually set on the spectrophotometer, the 

older method of only measuring at 340 l, 370 

l, and 400 l may be used. Then calculate 

using the trapezoidal rule for N + 1 = 3, H 

= 30. While the resulting area count with the 

older method is less accurate, the final 

results are similar since the inaccuracy is 

systematic. 

2.7.5 After determining the area count for 

each standard, determine the response factor 

(RF) for the oil at each concentration using 

the following equation: 

2.7.6 Spectrophotometer stability for the 

initial calibration is acceptable when the RFs 

of the six standard extracts are less than 10% 

different from the overall mean value for the 

six standards, as calculated in Equation 5 of 

this Appendix and depicted in the example 

in Table 4 of this Appendix. 

2.7.7 If this criterion is satisfied, begin 

analysis of sample extracts. Absorbances 

greater than or equal to 3.5 are not included 

because absorbance saturation occurs at and 

above this value. If any of the standard oil 

extracts fails to satisfy the initial-stability 

criterion, the source of the problem (e.g., 

preparation protocol for the oil standards, 

spectrophotometer stability, etc.) must be 

corrected before analysis of the sample 

extracts begins. 

2.7.8 Determine the slope of the 

calibration points by using linear regression 

forced zero intercept: 


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2.8 Spectrophotometric Analysis and 

Calculations 

2.8.1 Once a successful calibration curve 

for each of the two reference oils has been 

created and verified, measure experimental 

replicates for each of the reference oils at 

each temperature followed by a standard 

check sample. 

2.8.2 The same procedure is followed for 

the positive controls. 

2.8.3 Determine the area for the 

absorbance values obtained for the 

experimental samples by using Equation 2 of 

this Appendix and illustrated by Equation 3 

of this Appendix. 

2.8.4 Calculate the Total Oil dispersed 

and the percentage of oil dispersed (%OD) 

based on the ratio of oil dispersed in the test 

system to the total oil added to the system, 

as follows: 

where: 

VDCM = final volume of the DCM extract (mL) 

Vtw = total seawater in Baffled Flask (120 mL) 

Vew = volume seawater extracted (30 mL) 

where: 

rOil = density of the specific test oil, mg/mL 

and 

VOil = Volume (mL of oil added to test flask 

(100 mL = 0.1 mL)) 

2.8.5 The %ODs for the six replicates 

within a particular treatment are then 

subjected to an outlier test, the Grubb’s Test 

or Maximum Normal Residual test (6). A 

convenient Internet-based calculator of a 

Grubbs outlier may be found at: http:// 

www.graphpad.com/quickcalcs/Grubbs1.cfm. 

If an outlier is detected (p < 0.05), analyze 

an additional replicate to obtain the required 

six replicates. 

2.8.6 Report the Dispersion Efficacy value 

for each oil and each temperature, which is 

the lower 95% confidence level of the 6 

independent replicates (DELCL95) for each oil/ 

temperature combination. Error bars are not 

needed as reporting the lower confidence 

level computationally takes the variability of 

the replicates into account as shown in 

Equation 9 of this Appendix. 

where %OD = mean percentage oil dispersed 

for the n = 6 replicates, S = standard 

deviation, and t (n-1,1-α) = 100 * (1-a)th

percentile from the t-distribution with 

n-1 degrees of freedom. For 6 replicates, 

t n-1,1-α = 2.015, where a = 0.05. An 

example of the calculations is given in 

Table 5 of this Appendix. 

2.9 Performance Criterion 

The dispersant product tested will remain 

in consideration for listing on the NCP 

Product Schedule if the dispersant efficacy 

(DELCL95), as calculated in section 2.8.6 of 

this Appendix, is: 

Oil Temp 

(°C) 

DELCL95

(%) 

ANS ................................. 5 ≥ 70 

ANS ................................. 25 ≥ 75 

IFO120 ............................. 5 ≥ 55 

IFO120 ............................. 25 ≥ 65 

2.10 Quality Control (QC) Procedures for 

Oil Concentration Measurements 

2.10.1 Absorbance readings. Perform at 

least 5% of all UV-visible spectrophotometric 

measurements in duplicate as a QC check on 

the analytical measurement method. The 

absorbance values for the duplicates must 

agree within ± 5% of their mean value. 

2.10.2 Method blanks. Analytical method 

blanks involve an analysis of artificial 

seawater blanks (artificial seawater without 

oil or dispersant in a baffled flask) through 

testing and analytical procedures. Analyze 

method blanks with a frequency of at least 

two per completed test. Oil concentrations in 

method blanks must be less than detectable 

limits. 

2.10.3 Accuracy. Determine accuracy by 

using a mid-point standard calibration check 

after each set of replicate samples analyzed. 

The acceptance criterion is based on a 

percent recovery of 90–110% using the 

following equation: 

2.10.4 Calibration QC checks. Before 

analyzing samples, the spectrophotometer 

must meet an instrument stability calibration 

criterion using the oil standards. The 

instrument stability for initial calibration is 

acceptable when the RFs (Equation 5 of this 

Appendix) for each of the six standard 

concentration levels are less than 10% 

different from the overall mean value. 

TABLE 1—CONSTITUENT CONCENTRATIONS FOR GP2 ARTIFICIAL SEAWATER

[Based on Spotte et al., 1984] 

Constituent Concentration 

(g/L) 

NaCl ...................................... 21.03 

Na2SO4 ................................. 3.52 

KCl ........................................ 0.61 

KBr * ...................................... 0.088 

Na2B4O7 ·10H2O * ................. 0.034 

MgCl2 ·6H20 .......................... 9.50 

CaCl2 ·2H2O ......................... 1.32 

TABLE 1—CONSTITUENT CONCENTRATIONS FOR GP2 ARTIFICIAL SEAWATER—Continued 

[Based on Spotte et al., 1984] 

Constituent Concentration 

(g/L) 

SrCl2 ·6H2O * ........................ 0.02 

NaHCO2 * .............................. 0.17 

* Use Stock Solution, 1 mL/L GP2 for 100X 

stock solution for Bromide, Borate, and Strontium. 

10 mL/L GP2 for bicarbonate—10X stock 

solution as it is not soluble in a 100X solution. 


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3432 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

Adjust to pH 8.0 prior to autoclaving. 

TABLE 2—TEST OIL CHARACTERISTICS

Oil Density, mg/

mL @ 15 °C 

API gravity 

(deg) 

Viscosity @ 

15 °C, (cSt) 

Category 

by API 

gravity 

Category 

by 

kinematic 

viscosity 

ANS .......................................................................................................... 884 28.2 40 Medium .... Light 

IFO120 ..................................................................................................... 948 17.5 1520 Heavy ...... Heavy 

TABLE 3—STOCK SOLUTION

PREPARATION

Item Amount 

Mass of Bottle, g ...................... 29.9666 

Mass of Bottle + oil, g .............. 31.5734 

Mass of bottle + disp + oil + 

DCM, g .................................. 55.0425 

Mass of oil, g ............................ 1.6068 

TABLE 3—STOCK SOLUTION

PREPARATION—Continued 

Item Amount 

Mass of disp + oil + DCM, g .... 25.0759 

Mass of 1 mL syringe, g ........... 14.5563 

Mass of 1 mL syringe + solution, g .................................... 15.8779 

TABLE 3—STOCK SOLUTION

PREPARATION—Continued 

Item Amount 

Density of solution, g/mL .......... 1.3216 

Volume of solution, mL ............. 18.9740 

Conc. Of stock solution, mg/mL 84.6850 


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EP22JA15.049</GPH>emcdonald on DSK67QTVN1PROD with PROPOSALS3

Table 5. Sample Calculation with ANS 

Abs Abs Area Dilution Extract Cone, Mass in Total Oil Efficiency 

Rep 340nm .. 400nm from Factor Volume Area mg/m 30mL, Dispersed, % Avg . 

spec (ml) L. mg mg 

I 2.096 .. 0.814 77.51 1 25 77.59 0.72 18.12 72.49 82.00 81.01 

2 1.985 .. 0.774 73.72 1 25 73.70 0.69 17.21 68.86 77.89 

,.., 

.) 2.012 .. 0.781 74.50 1 ..,) 74.54 0.70 17.41 69.64 78.78 

4 2.18 .. 0.841 80.25 1 25 80.19 0.75 18.73 74.93 84.76 

5 1.999 .. 0.785 73.87 1 25 73.93 0.69 17.27 69.07 78.13 

6 2.173 .. 0.841 79.86 I 25 79.96 0.75 18.68 74.71 84.51 

dup 2.162 .. 0.841 80.143 l 25 80.16 0.75 18.72 74.89 84.72 0.04 

2.18 .. 0.841 80.245 1 25 80.19 0.75 18.73 74.93 84.76 
3434 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

2.11 References for Section 2.0 

(1) U.S. Environmental Protection Agency 

(1994), ‘‘Swirling Flask Dispersant 

Effectiveness Test,’’ Title 40 Code of Federal 

Regulations, Pt. 300, Appendix C, pp 47458– 

47461. 

(2) Sorial, G.A., A.D. Venosa, K.M, Koran, 

E. Holder, and D.W. King. 2004. ‘‘Oil spill 

dispersant effectiveness protocol: I. Impact of 

operational variables.’’ ASCE J. Env. Eng. 

130(10):1073–1084. 

(3) Sorial, G.A., A.D. Venosa, K.M, Koran, 

E. Holder, and D.W. King. 2004. ‘‘Oil spill 

dispersant effectiveness protocol: II. 

Performance of revised protocol.’’ ASCE J. 

Env. Eng. 130(10):1085–1093. 

(4) Venosa, A.D., D.W. King, and G.A. 

Sorial. 2002. ‘‘The baffled flask test for 

dispersant effectiveness: A round robin 

evaluation of reproducibility and 

repeatability.’’ Spill Sci. & Technol. Bulletin 

7(5–6):299–308. 

(5) Spotte, S., G. Adams, and P.M. Bubucis. 

1984. ‘‘GP2 medium is an synthetic seawater 

for culture or maintenance of marine 

organisms,’’ Zoo Biol, 3:229–240. 

(6) Grubbs, F. 1969. ‘‘Sample Criteria for 

Testing Outlying Observations,’’ Annals of 

Mathematical Statistics, pp. 27–58. 

3.0 Dispersant Toxicity Testing 

3.1 Summary. This laboratory protocol 

includes testing for: (1) Dispersant standard 

static acute toxicity tests for the mysid 

shrimp, Americamysis bahia (48-hr duration) 

and the inland silverside, Menidia beryllina 

(96-hr duration); (2) dispersant/oil mixture 

static acute toxicity tests for Americamysis 

bahia and Menidia beryllina (48-hr and 96- 

hr duration, respectively); (3) dispersant 

developmental assay for the purple sea 

urchin, Strongylocentrotus purpuratus, (72- 

hr duration); and (4) dispersant 7-day static 

subchronic tests with Americamysis bahia 

and Menidia beryllina (Table 6 of this 

Appendix). 

TABLE 6—TOXICITY TESTING REQUIREMENTS FOR DISPERSANTS

Test procedure 

Test substance 

96-hr static 

acute: 

Menidia 

beryllina 

48-hr static 

acute: 

Americamysis 

Bahia 

72-hr sea 

urchin Developmental Assay 

7-day subchronic: M. 

beryllina & 

A. bahia 

Dispersant only .................................................................................................................... yes ........... yes ............... yes ........... yes. 

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

3.2 Preparation of Stock Solutions 

3.2.1 Dispersant. Prepare a 1000 mL/L 

primary stock solution prior to test initiation 

by adding 1.1 mL of dispersant to 1100 mL 

of dilution water consisting of salinity 

adjusted uncontaminated natural or artificial 

seawater, in a glass vessel. Using a laboratory 

top stirrer equipped with a stainless steel 

blade, center the stirrer blade in the mixing 

vessel one inch off the bottom. Initially mix 

the resulting stock solution for approximately 

five seconds at speeds of < 10,000 rpm to 

avoid foaming. Thereafter, set the speed to 

provide a 70% vortex. Using a glass pipette, 

remove appropriate aliquots of stock solution 

from between the mixing vessel wall and 

edge of the vortex and place directly into the 

dilution water within an exposure vessel. 

Suspend mixing of the stock solution after 

the removal of each aliquot. Base the 

preparation of exposure solutions on the 

nominal concentration of the stock solution 

and follow procedures outlined in sections 

3.5 and 3.6 of this Appendix. 

3.2.2 Dispersant-Reference Oil(s) 

Mixtures. Use IFO 120 and ANS oils. To 

obtain these oils at no charge (except for a 

minimal shipping fee) see http://

www.epa.gov/emergencies/content/ncp/

index.htm. Assessment of dispersantreference oil mixture (DOM) toxicity is 

determined for each reference oil using the 

aqueous phase of a chemically enhancedwater accommodated fraction (CE–WAF). 

Repeat the following procedure for each 

reference oil tested. Fit a glass aspirator 

bottle (approximately 23L) equipped with a 

hose bib at the base with a length of silicon 

tubing containing a hose clamp. Fill the 

bottle with 19L of seawater leaving a 20% 

headspace above the liquid, place on a 

magnetic stir plate then add and center a stir 

bar. Add the respective crude oil at 25g/L 

using a silicon tube attached to a glass funnel 

that reaches just below the water surface. 

Using this method reduces the production of 

air bubbles on the oil surface slick. Adjust 

the stir plate to obtain an oil vortex of 25% 

of the total volume of the seawater, then add 

the dispersant to be tested at a ratio of 1:10 

dispersant:oil (2.5 g/L). Securely seal the 

bottle to reduce the loss of volatiles using a 

silicon stopper and wraps of Parafilm and stir 

for 18 hours, then allow the solution to settle 

for 6 hours. Maintain the temperature at 25 

°C during stirring and settling. Purge the hose 

at the base of the bottle of any material 

followed by removal of the CE–WAF 

(aqueous phase) into a clean glass container 

without disturbing the surface oil slick. The 

CE–WAF should be remixed and 1–2 L 

removed for chemical analysis of total 

petroleum hydrocarbons (TPH) following the 

procedures outlined in section 3.4 of this 

Appendix. The remaining volume will be 

used for the preparation of exposure 

solutions following procedures outlined in 

section 3.3 of this Appendix. To reduce time 

and cost, mix sufficient amounts of 

dispersant product-reference oil mixture CE– 

WAF to allow preparation of exposure 

solutions for conducting simultaneous acute 

tests with both Americamysis bahia and 

Menidia beryllina. 

3.3 Preparation of Exposure Concentrations 

3.3.1 Concentration Selection. 

Preliminary rangefinder tests may be 

necessary using a series of logarithmic 

concentrations (e.g. 0.1, 1, 10, 100 ml 

dispersant product/L or mg TPH/L) to 

determine the appropriate exposure 

concentration range necessary to determine 

LC50 values and 95% confidence intervals. 

For definitive tests, conduct a minimum of 

five test concentrations using a geometric 

ratio between 1.5 and 2.0 (e.g. 2, 4, 8, 16, and 

32). Note that when testing only the 

dispersant product, the highest test 

concentration must not exceed the 

dispersant’s self-dispersibility limit. 

3.3.2 Exposure Concentrations. Exposure 

solutions are prepared by adding the 

appropriate amount of stock solution directly 

to dilution water in each test chamber. Mix 

each exposure solution using five rotations in 

one direction followed by five rotations in 

the opposite direction using a solid glass stir 

rod. 

3.3.3 Reference Toxicants. Separate 

toxicity tests must be performed with a 

reference toxicant for each species tested. 

Conduct additional reference toxicity tests 

any time a change in the population or 

source of a test species occurs. Use sodium 

dodecyl sulfate (SDS), also known as dodecyl 

sodium sulfate (DSS), and sodium lauryl 

sulfate (SLS) as the reference toxicant for 

exposures conducted with Menidia beryllina 

and Americamysis bahia. Use copper 

chloride as the reference toxicant for 

exposures conducted with the sea urchin 

developmental test. Use reagent grade quality 

SDS and copper chloride for tests. 

Information on procedures for conducting 

reference toxicant tests with these species 

can be found in the specific EPA methods 

documents cited in sections 3.5.1, 3.6.1 and 

3.7.1 of this Appendix. 

3.4 Chemical Analysis of Stock Solutions. 

Add the 1L sample of CE–WAF (Section 3.2.2 

of this Appendix) solutions directly to amber 

glass bottles with Teflon®-lined cap. Collect 

a replicate sample in the event of accidental 

loss or if reanalysis of the stock solution 

becomes necessary. Adjust sample to a pH=2 

using 50% hydrochloric acid, immediately 

refrigerate and analyze within 48 hours of 

collection. Analyze samples for C9–C32 TPH 

by gas chromatography-flame ionization 

detection (GC–FID) following EPA SW–846, 

Method 8015B–DRO (4). Report TPH 

concentration of stock solutions as 

milligrams TPH/L and use in the calculation 

of exposure concentrations for all toxicity 

tests conducted with CE–WAF. 


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3.5 Static Acute Tests With M. beryllina and 

A. bahia 

3.5.1 General. Use EPA’s Methods for 

Measuring the Acute Toxicity of Effluents 

and Receiving Waters to Freshwater and 

Marine Organisms (EPA–821–R–02–012) (1) 

for testing each species separately with 

dispersant product or a mixture of dispersant 

product and reference oil (DOM). 

3.5.2 Test Solutions. Modify procedures 

in EPA–821–R–02–012 specifically dealing 

with the handling and toxicity testing of 

effluents or receiving water samples as 

follows: Prepare stock solutions following 

section 3.2 of this Appendix and exposure 

concentrations following section 3.3 of this 

Appendix. 

3.5.3 Number of Treatments, Replicates 

and Organisms. Conduct a minimum of three 

replicates of at least five exposure treatments 

plus a minimum of three replicate dilution 

water controls. Expose ten organisms per 

replicate treatment. 

3.5.4 Exposure Period. Test duration is 

48-hr for Americamysis bahia and 96-hr for 

Menidia beryllina. Mortality must be 

recorded at each 24 hour period of each test. 

3.5.5 Test Acceptability. For each test 

performed, survival of control animals must 

be >90% and test results must allow 

determination of statistically valid LC50 and 

95% confidence interval values except in 

cases where the LC50 is >1000 ml/L or is 

determined to be greater than the limits of 

water solubility of dispersibility. 

3.5.6 Static Acute Test Summary. A 

summary of required test conditions is 

provided in Table 7 of this Appendix. 

3.6 Sea Urchin Developmental Test With 

Dispersant Product 

3.6.1 General. Use Section 15, ‘‘Purple 

Urchin, Strongylocentrotus purpuratus and 

Sand Dollar, Dendraster excentricus Larval 

Development Test Method’’ of EPA’s ShortTerm Methods for Estimating the Chronic 

Toxicity of Effluents and Receiving Waters to 

West Coast Marine and Estuarine Organisms 

(EPA/600/R–95–136) (2). 

3.6.2 Test Organism. Tests of dispersant 

products are to follow methods for the purple 

urchin only. Tests with the sand dollar are 

not required. 

3.6.3 Test Solutions. Modify procedures 

in EPA/600/R–95–136, Section 15 

specifically dealing with the handling and 

toxicity testing of effluents or receiving water 

samples as follows: Prepare stock solutions 

following section 3.2.1 of this Appendix and 

exposure concentrations following section 

3.3 of this Appendix. 

3.6.4 Number of Treatments and 

Replicates. Conduct a minimum of four 

replicates of five exposure treatments plus a 

minimum of four replicate dilution water 

controls. 

3.6.5 Exposure Duration and Test 

Endpoint. Examine the effects of the 

dispersant product on normal development 

of sea urchin embryos over a period of 72 

hours. An IC50 (the exposure concentration at 

which normal development is inhibited in 

50% of the embryos) with 95% confidence 

intervals are to be determined in place of an 

IC25. The concentration of dispersant causing 

inhibition of development in 50% of exposed 

embryos (IC50) with the lower and upper 95% 

confidence intervals (LCI95 and ULCI95) must 

be calculated at the end of the exposure 

period. Mortality determinations are not 

required. 

3.6.6 Test Acceptability. Requirements of 

the assay are: (i) ≥ 80% normal larval 

development in the control treatment, (ii) the 

minimum significant difference (MSD) that 

can be statically detected relative to the 

control is ≤25%, (iii) test results which 

support the determination of a statistically 

valid IC50 and 95% confidence interval 

unless the LC50 is >1000 ml/L or is greater 

than the limits of water solubility of 

dispersibility. 

3.6.7 Urchin Developmental Test 

Summary. A summary of required test 

conditions is provided in Table 7 of this 

Appendix. 

3.7 Seven-Day Subchronic Tests With M. 

beryllina and A. bahia 

3.7.1 General. Use Section 13, Method 

1006.0, ‘‘Inland Silverside (Menidia 

beryllina) Larval Survival and Growth 

Method,’’ and Section 14, Method 1007.0, 

‘‘Mysid (Mysidopsis [renamed Americamysis] 

bahia) Survival, Growth, and Fecundity 

Method’’ of EPA’s Short-Term Methods for 

Estimating the Chronic Toxicity of Effluents 

and Receiving Waters to Marine and 

Estuarine Organisms (EPA–821–R–02–014) 

(3) for testing of dispersant product. 

3.7.2 Test Solutions. Modify procedures 

in EPA–821–R–02–014, sections 13 and 14 

specifically dealing with the handling and 

toxicity testing of effluents or receiving water 

samples as follows: Prepare stock solutions 

following section 3.2.1 of this Appendix and 

exposure concentrations following section 

3.3 of this Appendix. Exposure solutions 

should be renewed every 24 hr for the 

duration of the test. 

3.7.3 Number of Treatments, Replicates 

and Organisms. (i) Menidia beryllina: 

Conduct a minimum of four replicates of at 

least five exposure treatments plus a 

minimum of four replicate dilution water 

controls. Expose ten M. beryllina per 

replicate treatment. (ii) Americamysis bahia: 

Conduct a minimum of eight replicates of at 

least five exposure treatments plus a 

minimum of eight replicate dilution water 

controls. Expose five A. bahia per replicate 

treatment. 

3.7.4 Exposure Duration and Test 

Endpoint. The test duration is seven days for 

both species. Test endpoints for Menidia 

beryllina are survival and growth (dry 

weight) and for Americamysis bahia is 

survival, growth (dry weight) and fecundity. 

Calculate an LC50 and 95% confidence 

interval for survival and IC25 and IC50 with 

95% confidence intervals for growth (and 

fecundity for A. bahia only). Report the 

lowest observed effect concentration (LOEC) 

and no observed effect concentration (NOEC) 

for each endpoint. 

3.7.5 Test Acceptability. Requirements of 

the assay are: (i) ≥80% survival in the control 

treatment for each species, (ii) dry weights 

must meet the specific requirements as 

stipulated in Method 1006.0 for Menidia 

beryllina and Method 1007.0 for 

Americamysis bahia, (iii) egg production 

must occur in 50% of female Americamysis 

bahia in the replicate control treatments. 

3.7.6 Subchronic Test Summary. A 

summary of required test conditions for each 

species is provided in Table 7 of this 

Appendix. 

3.8. Laboratory Report. The laboratory 

must include, for each toxicity test report, all 

applicable information, data and analyses as 

follows: 

3.8.1 Test Objective: Protocol title and 

source, endpoint(s); 

3.8.2 Product Information: Product name, 

manufacturer contact information, lot 

number, production date, date received/

chain of custody; 

3.8.3 Contract Facility: Contact 

information; 

3.8.4 Dilution Water: Source, 

pretreatment, physical and chemical 

characteristics (pH, salinity); 

3.8.5 Test Conditions: Date and time of 

test (start and end), test chambers type and 

volume, volume of solution per chamber, 

number of organisms per chamber, number of 

replicate chambers per treatment, feeding 

frequency, amount and type of food, test 

concentrations, test temperature (mean and 

range), test salinity (mean and range); 

3.8.6 Test Organisms: Common and 

scientific name, source contact information, 

age and date purchased, acclimation 

conditions (e.g., temperature, salinity, both 

mean and range), age at test start; 

3.8.7 Reference toxicant: Date received, 

lot number, date of most recent test, results 

and current Cumulative Sum Chart, dilution 

water used, physical and chemical methods 

used; 

3.8.8 Quality Assurance: Verification of 

laboratory accreditation, including 

subcontractor facilities; 

3.8.9 Test Results: Raw data in tabular 

and graphical form, daily records of affected 

organisms in each concentration replicate 

and controls, table of required endpoints (i.e., 

LC50 with 95% confidence interval (CI), IC25

and IC50 with 95% CI, LOEC and NOEC), 

statistical methods used to calculate 

endpoints, summary tables of test conditions 

and QA data; 

3.8.10 Analytical Results: Method 

summary including Limit of Detection 

(LOD)/Limit of Quantitation (LOQ), 

deviations and reasons if any, sample 

summary, results including chromatograms 

and data qualifiers, QA summary including 

calibration curves, method blank and 

surrogate recovery, analytical results 

summary; and 

3.8.11 Conclusions: Relationship between 

test endpoints and threshold limit. 


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3436 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

TABLE 7—SUMMARY OF TEST CONDITIONS—DISPERSANT TOXICITY

Acute M. beryllina Acute A. bahia Subchronic M. 

beryllina Subchronic A. bahia Development S. 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 

than 3 °C during the test. 

15 ± 1 °C. 

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 volume 1.200 mL ...................... 200 mL .................... 500–750 mL .............. 150 mL .................... 10 mL. 

Age of test organism 2.9–14 days .................. 1–5 days .................. 7–11 days .................. 7 days ...................... 1 hr old fertilized eggs. 

No. organisms per 

test chamber.

10 ............................... 10 ............................ 10 ............................... 5 .............................. 25 embryos per mL. 

No. of replicate 

chambers per concentration.

3 ................................. 3 .............................. 4 ................................. 8 .............................. 4. 

Feeding regime ........ Refer to specific feeding procedures provided in each test method None. 

Aeration .................... None, unless DO falls below 4.0 mg/L, then aerate all chambers. Rate:<100 bubbles/minute 

Test concentrations .. 5 exposure concentrations and a control (minimum required) 

Test acceptability (required).≥90% survival in controls.≥90% survival in 

controls.

For controls: ≥80% 

survival; average 

dry weight ≥0.5mg 

where test starts 

with 7 day old larvae, or ≥ 0.43 mg 

for larvae preserved 

for ≤7days.

For controls: ≥80% 

survival; average 

dry weight ≥0.20 

mg; ≥ 50% of control females 

produce eggs.

≥80% normal shell development in controls. 

1 Recommended minimum value. 

2 Less than or equal to 24-hr range in age. 

3.9 References for Section 3.0 

(1) U.S. EPA. 2002. Methods for Measuring 

the Acute Toxicity of Effluents and 

Receiving Waters to Freshwater and 

Marine Organisms. Fifth Edition. U.S. 

Environmental Protection Agency, 

Washington, DC (EPA–821–R–02–012). 

(2) U.S. EPA. 1995. Short-Term Methods for 

Estimating the Chronic Toxicity of 

Effluents and Receiving Waters to West 

Coast Marine and Estuarine Organisms. 

First Edition. U.S. Environmental 

Protection Agency, Washington, DC 

(EPA/600/R–95–136) 

(3) U.S. EPA. 2002. Short-Term Methods for 

Estimating the Chronic Toxicity of 

Effluents and Receiving Waters to Marine 

and Estuarine Organisms U.S. 

Environmental Protection Agency, 

Washington, DC (EPA–821–R–02–014). 

(4) U.S. EPA. 2008. Test Methods for 

Evaluating Solid Waste, Physical/

Chemical Methods U.S. Environmental 

Protection Agency, Washington, DC 

(SW–846) http://www.epa.gov/osw/

hazard/testmethods/sw846/online/

index.htm. 

4.0 Standard Acute Toxicity Testing of 

Surface Washing Agents, Bioremediation 

Agents, Herding Agents, and Solidifiers. 

4.1 Summary. This laboratory protocol 

includes testing for: (1) Saltwater standard 

static acute toxicity tests for test products 

with the mysid shrimp, Americamysis bahia 

(48-hr duration) and the inland silverside, 

Menidia beryllina (96-hr duration); and (2) 

freshwater standard static acute toxicity tests 

for test products with the daphnid, 

Ceriodaphnia dubia (48-hr duration) and the 

fathead minnow, Pimephales promelas (96-hr 

duration) (see Table 8 of this Appendix). 

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

AGENTS AND SOLIDFIERS

Application environment 

Test procedure 

96-hr static 

acute: 

Menidia 

beryllina 

48-hr static 

acute: 

Americamysis 

bahia 

96-hr static 

acute: 

Pimephales 

promelas 

48-hr static 

acute: 

Ceriodaphnia 

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 

EPA’s Methods for Measuring the Acute 

Toxicity of Effluents and Receiving Waters to 

Freshwater and Marine Organisms (EPA– 

821–R–02–012) [1] for preparation of the 

appropriate dilution water for each species 

tested. Use of clean natural or synthetic 

seawater for tests conducted with saltwater 

species is acceptable. 

4.3 Preparation of Stock Solutions 

4.3.1 Liquid Surface Washing Agents 

and/or Herding Agents. Prepare a 1000 mL/ 

L stock solution prior to test initiation by 

adding 1.1 mL of test product to 1100 mL of 

dilution water in a glass vessel. Place on a 

magnetic stir plate then add and center a stir 

bar and adjust the stir plate to obtain a vortex 

of 25% of the total volume of the liquid. Mix 

the resulting stock solution for approximately 

five minutes at room temperature. Using a 

glass pipette, remove appropriate aliquots of 

stock solution from between the mixing 

vessel wall and edge of the vortex and place 

directly into the dilution water within an 

exposure vessel. Base the preparation of 

exposure solutions on the nominal 

concentration of the stock solution and 

follow procedures outlined in sections 4.6 

and/or 4.7 of this Appendix, as appropriate. 

4.3.2 Bioremediation Agents. For 

products consisting of two or more liquid 

and/or solid components, prepare the 

product following the manufacturers 

recommended procedure and ensure the test 

product mixture is completely blended. 

Prepare a 1000 mL/L stock solution prior to 

test initiation by adding 1.1 mL of the test 

product mixture to 1100 mL of dilution water 

in a glass vessel. Place on a magnetic stir 

plate then add and center a stir bar and 

adjust the stir plate to obtain a vortex of 25% 

of the total volume of the liquid. Mix the 

resulting stock solution for approximately 

five minutes at room temperature. Using a 

glass pipette, remove appropriate aliquots of 

stock solution from between the mixing 

vessel wall and edge of the vortex and place 

directly into the dilution water within an 

exposure vessel. Base the preparation of 

exposure solutions on the nominal 

concentration of the stock solution and 

follow procedures outlined in sections 4.5 

and/or 4.6 of this Appendix, as appropriate. 

4.3.3 Solid Phase Products. Assessment 

of the toxicity of solidifiers and other solid 

phase products are determined using the 

aqueous phase of water-accommodated 

fractions (WAFs) of the test product. Fit a 

glass aspirator bottle (approximately 23L) 

equipped with a hose bib at the base with a 

length of silicon tubing containing a hose 

clamp. Fill the bottle with 19L of dilution 

water leaving a 20% headspace above the 

liquid, place on a magnetic stir plate then 

add and center a stir bar. Add the test 

product at 25 g/L and securely seal the bottle 

using a silicon stopper and wraps of 

parafilm. Adjust the stir plate to obtain a 

vortex of 25% of the total fluid volume, stir 

for 18 hours then settle for 6 hours. Maintain 

the temperature at 25 °C during stirring and 

settling. Purge the hose at the base of the 

bottle of any material followed by removal of 

the WAF (aqueous phase) into a clean glass 

container without disturbing the product on 

the surface. The WAF should be remixed and 

used for the preparation of exposure 

solutions following procedures outlined in 

section 4.4 of this Appendix. 

4.4 Preparation of Exposure Concentrations 

4.4.1 Concentration Selection. 

Preliminary rangefinder tests may be 

necessary using a series of logarithmic 

concentrations (e.g. 0.1, 1, 10, 100 ml test 

product/L) to determine the appropriate 

exposure concentration range necessary to 

determine LC50 values and 95% confidence 

intervals. For definitive tests, conduct a 

minimum of five test concentrations using a 

geometric ratio between 1.5 and 2.0 (e.g. 2, 

4, 8, 16, and 32). Note that when testing the 

product, the highest test concentration 

should not exceed the test product’s selfdispersibility limit. 

4.4.2 Exposure Concentrations. Exposure 

solutions are prepared by adding the 

appropriate amount of stock solution directly 

to dilution water in each test chamber. Mix 

each exposure solution using five rotations in 

one direction followed by five rotations in 

the opposite direction using a solid glass stir 

rod. 

4.4.3 Reference Toxicants. Separate 

toxicity tests must be performed with a 

reference toxicant for each species tested. 

Conduct additional reference toxicity tests 

any time a change in the culture population 

or source of a test species occurs. Use reagent 

grade quality sodium dodecyl sulfate (SDS), 

also known as dodecyl sodium sulfate (DSS), 

and sodium lauryl sulfate (SLS) as the 

reference toxicant. Information on 

procedures for conducting reference toxicant 

tests with these species can be found in 

section 4 of EPA’s Methods for Measuring the 

Acute Toxicity of Effluents and Receiving 

Waters to Freshwater and Marine Organisms 

(EPA–821–R–02–012) (3). 

4.5 Saltwater Static Acute Tests With 

Menidia beryllina and Americamysis bahia 

4.5.1 General. Use EPA’s Methods for 

Measuring the Acute Toxicity of Effluents 

and Receiving Waters to Freshwater and 

Marine Organisms (EPA–821–R–02–012) (1) 

for testing each species separately with the 

test product. 

4.5.2 Test Solutions. Modify procedures 

in EPA–821–R–02–012 specifically dealing 

with the handling and toxicity testing of 

effluents or receiving water samples as 

follows: Prepare stock solutions following the 

appropriate sections (4.3.1, 4.3.2, or 4.3.3) of 

this Appendix and exposure concentrations 

following section 4.4 of this Appendix. 

4.5.3 Number of Treatments, Replicates 

and Organisms. Conduct a minimum of three 

replicates of at least five exposure treatments 

plus a minimum of three replicate dilution 

water controls. Expose ten organisms per 

replicate treatment. 

4.5.4 Exposure Period. Test duration is 

48-hr for A. bahia and 96-hr for M. beryllina. 

Mortality must be recorded at each 24 hour 

period of each test. 

4.5.5 Test Acceptability. For each test 

performed, survival of control animals must 

be > 90% and test results must allow 

determination of statistically valid LC50 and 

95% confidence interval values except in 

cases where the LC50 is >1000 ml/L or is 

determined to be greater than the limits of 

water solubility or dispersibility. 

4.5.6 Static Acute Test Summary. A 

summary of required test conditions is 

provided in Table 9 of this Appendix. 

4.6 Freshwater Static Acute Tests With 

Pimephales promelas and Ceriodaphnia 

dubia 

4.6.1 General. Use EPA’s Methods for 

Measuring the Acute Toxicity of Effluents 

and Receiving Waters to Freshwater and 

Marine Organisms (EPA–821–R–02–012) (1) 

for testing each species separately with the 

test product. 

4.6.2 Test Solutions. Modify procedures 

in EPA–821–R–02–012 specifically dealing 

with the handling and toxicity testing of 

effluents or receiving water samples as 

follows: Prepare stock solutions following the 

appropriate sections (4.3.1, 4.3.2, or 4.3.3) of 

this Appendix and exposure concentrations 

following section 4.4 of this Appendix. 

4.6.3 Number of Treatments, Replicates 

and Organisms. P. promelas: Conduct a 

minimum of three replicates of at least five 

exposure treatments plus a minimum of three 

replicate dilution water controls. Expose ten 

organisms per replicate treatment. C. dubia: 

Conduct a minimum of four replicates of at 

least five exposure treatments plus a 

minimum of four replicate dilution water 

controls. Expose five organisms per replicate 

treatment. 

4.6.4 Exposure Period. Test duration is 

48-hr for C. dubia and 96-hr for P. promelas. 

Mortality must be recorded at each 24 hour 

period of each test. 

4.6.5 Test Acceptability. For each test 

performed, survival of control animals must 

be > 90% and test results must allow 

determination of statistically valid LC50 and 

95% confidence interval values except in 

cases where the LC50 is >1000 ml/L or is 

determined to be greater than the limits of 

water solubility of dispersibility. 

4.6.6 Static Acute Test Summary. A 

summary of required test conditions is 

provided in Table 9 of this Appendix. 

4.7 Laboratory Report 

The laboratory must include, for each 

toxicity test report, all applicable 

information, data and analyses as follows: 

4.7.1 Test Objective: Protocol title and 

source, endpoint(s); 

4.7.2 Product Information: Product name, 

manufacturer contact information, lot 

number, production date, date received/

chain of custody; 

4.7.3 Contract Facility: Contact 

information; 

4.7.4 Dilution Water: Source, 

pretreatment, physical and chemical 

characteristics (pH, salinity); 

4.7.5 Test Conditions: Date and time of 

test (start and end), test chambers type and 

volume, volume of solution per chamber, 

number of organisms per chamber, number of 

replicate chambers per treatment, feeding 

frequency, amount and type of food, test 

concentrations, test temperature (mean and 

range), test salinity (mean and range); 

4.7.6 Test Organisms: Common and 

scientific name, source contact information, 

age and date purchased, acclimation 

conditions (e.g., temperature, salinity, both 

mean and range), age at test start; 

4.7.7 Reference toxicant: Date received, 

lot number, date of most recent test, results 


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and current Cumulative Sum Chart, dilution 

water used, physical and chemical methods 

used; 

4.7.8 Quality Assurance: Verification of 

laboratory accreditation, including 

subcontractor facilities; 

4.7.9 Test Results: Raw data in tabular 

and graphical form, daily records of affected 

organisms in each concentration replicate 

and controls, table of required endpoints (i.e., 

LC50, 95% CI, inhibited concentration for 

50% of the species (IC50), lower observed 

effect concentration (LOEC) and no observed 

effect concentration (NOEC)), statistical 

methods used to calculate endpoints, 

summary tables of test conditions and QA 

data; and 

4.7.10 Conclusions: Relationship between 

test endpoints and threshold limit. 

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

AND SOLIDIFIERS TOXICITY

Saltwater Acute 

M. beryllina 

Saltwater Acute 

A. bahia 

Freshwater Acute 

P. promelas 

Freshwater Acute 

C. dubia 

Test type .......................................................... Static non-renewal ..... Static non-renewal .... Static non-renewal ..... Static non-renewal. 

Test duration .................................................... 96 hours .................... 48 hours .................... 96 hours .................... 48 hours. 

Salinity .............................................................. 20 ± 2‰ ..................... 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 

(minimum).

3 ................................ 3 ................................ 3 ................................ 4. 

Feeding regime ................................................ Refer to specific feeding procedures provided in each test method

Aeration ............................................................ None, unless DO falls below 4.0 mg/L, then aerate all chambers. Rate: <100 bubbles/minute 

Test concentrations .......................................... 5 exposure concentrations and a control (minimum required) 

Test acceptability (required) ............................ ≥90% survival in controls 

1 Recommended minimum value. 

2 Less than or equal to 24-hr range in age. 

4.8 References for Section 4 

(1) U.S. EPA. 2002. Methods for Measuring 

the Acute Toxicity of Effluents and Receiving 

Waters to Freshwater and Marine Organisms. 

Fifth Edition. U.S. Environmental Protection 

Agency, Washington, DC (EPA–821–R–02– 

012). 

5.0 Bioremediation Agent Efficacy Test 

Protocol 

5.1 Summary. This protocol quantifies 

changes in weathered Alaska North Slope 

(ANS) crude oil composition of alkanes and 

aromatics resulting from the use of a 

bioremediation agent in either artificial 

seawater or freshwater. The manufacturer 

may test either one or both freshwater or 

saltwater, depending on the product’s 

intended use. Biodegradation of the alkanes 

and aromatics is monitored for 28 days at 20– 

23 °C. Product flasks at Day 28 are compared 

to Day 0 flasks to determine reductions in 

alkanes and aromatics. A positive control of 

a known oil-degrading bacterial culture 

supplied by EPA is tested. A negative, sterile 

control is also set up containing exposure 

water, weathered crude oil, product, and a 

sterilant, sodium azide. The purpose of the 

negative, killed control is to make sure the 

disappearance of the oil constituents at day 

28 is due to biodegradation and not some 

physical loss such as volatilization. The day 

28 GC/MS results from the killed control 

must not be less than 90% of the day 0 

results. The sample preparation procedure 

extracts the oil phase into the solvent 

dichloromethane (DCM) (also known as 

methylene chloride) with a subsequent 

solvent exchange into hexane. The hexane 

extracts are analyzed by a high resolution gas 

chromatograph/mass spectrometer (GC/MS) 

operated in the selected ion monitoring mode 

(SIM) at a scan rate of >5 scans per second. 

Note to 5.1: Artificially distilled at 521 °F 

(272 °C) to remove the low molecular weight 

hydrocarbons to approximate natural 

weathering processes that occur after a spill. 

5.2 Apparatus. All equipment must be 

maintained and calibrated per standard 

laboratory procedures. 

5.2.1 Assorted flasks and other glassware; 

5.2.2 Graduated cylinders (100 mL); 

5.2.3 Deionized water; 250 mL 

borosilicate glass Erlenmeyer flasks; 

5.2.4 Pasteur pipettes; 

5.2.5 Multichannel pipettor (5–50 mL and 

50–200 mL); 

5.2.6 Autoclave; environmental room or 

incubator; 

5.2.7 Balance accurate to 0.1 mg; 

5.2.8 Orbital shaker table with clamps 

sized to hold flasks securely; 

5.2.9 GC/MS instrument equipped with a 

DB–5 capillary column (30 m, 0.25 mm ID, 

and 0.25 mm film thickness) or equivalent, 

and a split/splitless injection port operating 

in the splitless mode, such as a Agilent 6890 

GC/5973 MS (or equivalent) equipped with 

an auto-sampler for testing multiple samples; 

and 

5.2.10 Fixed Rotor Centrifuge. 

5.3 Reagents and Culture Medium 

5.3.1 Stock Seawater Preparation. 

Prepare the artificial seawater GP2 (Spotte et 

al., 1984) following the procedures in section 

2.3 of this Appendix, to obtain the final 

concentration of the salts listed in Table 1 of 

this Appendix, except for the sodium 

bicarbonate (NaHCO3) which is prepared 

separately. Autoclave the artificial seawater. 

Filter sterilize the concentrated solution of 

sodium bicarbonate through a 0.45 mm 

membrane filter and add to the autoclaved 

and cooled artificial seawater GP2 to obtain 

the final concentration listed in Table 1 of 

this Appendix. 

5.3.2 Seawater for the positive control 

flasks. Prepare sodium triphosphate (a.k.a., 


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sodium tripolyphosphate) (Na5P3O10), 

potassium nitrate (KNO3), and ferric chloride 

hexahydrate (FeCl3 · 6H2O) as a concentrated 

solution. Filter sterilize through a 0.45 mm 

membrane filter and add to autoclaved 

artificial seawater to obtain the final nutrient 

concentrations listed in Table 10 of this 

Appendix. Calibrate the pH meter at room 

temperature (approximately 20–23 °C) using 

commercial buffers of pH 4.0, 7.0, and 10.0, 

as appropriate, prior to use. Adjust the pH of 

the artificial seawater with concentrated 

hydrochloric acid (HCl) or 10 normality 

sodium hydroxide (10 N NaOH), as 

appropriate. 

TABLE 10—ARTIFICIAL SEAWATER

NUTRIENT CONCENTRATIONS

Constituent Final concentration, g/L 

* FeCl3 · 6H2O ...................... 0.050 

KNO3 ..................................... 2.890 

* Na5P3O10 ............................ 0.297 

* Added aseptically after the GP2 has been 

autoclaved to limit phosphorus and iron 

precipitation. 

5.3.3 Seawater for bioremediation agents 

that do not include nutrients. If a 

bioremediation agent contains living 

microorganisms but not nutrients (or limiting 

concentrations of nutrients), then nutrients 

may be added by the manufacturer. However, 

the total concentration of the nutrients added 

to the bioremediation agent must not exceed 

the final concentrations listed in Table 11 of 

this Appendix. 

TABLE 11—ARTIFICIAL SEAWATER NUTRIENT CONCENTRATIONS FOR BIOREMEDIATION AGENTS HAVING NO

NUTRIENTS INCLUDED

Constituent Final concentration, g/L 

as Iron (Fe) ........................... 0.010 

as Nitrogen (N) ..................... 0.400 

as Phosphorus (P) ................ 0.075 

If nutrients are supplied by the product 

manufacturer, the specific composition and 

concentration used in the efficacy testing 

must be submitted. 

5.3.4 Freshwater Preparation. The 

artificial freshwater, which is a modification 

of Bushnell-Haas medium (Haines et al., 

2005), is prepared following the 

concentrations listed in Table 12 of this 

Appendix and then autoclaved. The pH is 

adjusted to 7.4 before autoclaving. 

Constituents removed from the original 

formulation are KNO3, K2HPO4 and KH2PO4. 

TABLE 12—CONSTITUENT CONCENTRATIONS FOR ARTIFICIAL

FRESHWATER

[Bushnell-Haas] 

Constituent 

Final concentration 

(mg/L) 

MgSO4 · 7H2O ...................... 200 

CaCl2 · 2H2O ........................ 20 

FeCl3 · 6H2O ......................... 50 

MnSO4 · H2O ........................ 0.0302 

H3BO3 ................................... 0.0572 

ZnSO4 · 7H2O ....................... 0.0428 

(NH4)6Mo7O2 ......................... 0.0347 

5.3.5 Freshwater for the positive control. 

To prepare the freshwater for the positive 

controls, prepare the nutrients potassium 

phosphate monobasic (KH2PO4), potassium 

phosphate dibasic (K2HPO4) and potassium 

nitrate (KNO3) as a concentrated solution. 

Filter sterilize and add to autoclaved 

artificial freshwater to obtain the final 

concentrations given in Table 13 of this 

Appendix. Calibrate the pH meter at room 

temperature (approximately 20–23 °C) using 

commercial buffers of pH 4.0, 7.0, and 10.0, 

as appropriate, prior to use. Adjust the pH of 

the artificial freshwater to 7.4 with 1 N HCl 

or 1 N NaOH, as appropriate. 

TABLE 13—FRESHWATER NUTRIENT

CONCENTRATIONS

Constituent 

Final concentration 

(g/L) 1

KNO3 ..................................... 2.89 

KH2PO4 ................................. 1.00 

K2HPO4 ................................. 1.00 

1Adjust pH to 7.4 prior to autoclaving 

5.3.6 Freshwater for bioremediation 

agents that contain living microorganisms 

but not nutrients or limiting concentrations 

of nutrients. If a bioremediation agent does 

not include nutrients, then nutrients may be 

added. However, the total concentration of 

the nutrients added to the bioremediation 

agent must not exceed the final 

concentrations provided in Table 14 of this 

Appendix. 

TABLE 14—ARTIFICIAL FRESHWATER

NUTRIENT CONCENTRATIONS FOR

BIOREMEDIATION AGENTS HAVING

NO NUTRIENTS INCLUDED

Constituent Final concentration, g/L 1

as Iron (Fe) ........................ not added since 

iron is already 

in the freshwater solution. 

as Nitrogen (N) .................. 0.400. 

as Phosphorus (P) ............. 0.400. 

1Adjust to pH 7.4 prior to autoclaving. 

If nutrients are supplied by the product 

vendor, the specific composition and 

concentration used in the efficacy testing 

must be submitted. 

5.3.7 Oil Preparation. The test oil, 

weathered ANS521 crude oil, can be 

obtained from EPA at no charge (except for 

a minimal shipping fee). See http://

www.epa.gov/emergencies/content/ncp/

index.htm for more information. 

5.3.8 Sodium azide sterilant. Prepare a 

stock solution of NaN3 for addition to the 

negative killed control. The final 

concentration in the killed controls will be 

0.5 g/L. 

5.4 Experimental Setup and Procedure 

5.4.1 Autoclave clean borosilicate glass 

Erlenmeyer flasks (250 mL) for 20 minutes at 

121 °C at 15 psig. 

5.4.2 Label flasks with the appropriate 

code (negative control, positive control, or 

product; day to be sampled (0 or 28); letter 

indicating replicate number) to reflect the 

following treatment design in Table 15 of this 

Appendix: 

TABLE 15—BIOREMEDIATION EFFICACY TEST—SUMMARY OF EXPERIMENTAL SETUP

Treatment 

Number of replicates at 

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 + supplemented nutrients (if necessary)).6 6 GC/MS 

Test Type 2: Product containing proprietary nutrients but no live microorganisms (oil + exposure 

water + product + EPA culture).

6 6 GC/MS 

Test Type 3: Product (such as an enzyme) containing no live microorganisms and no nutrients (oil + 

exposure water + product).

6 6 GC/MS 

* 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 presterilized artificial exposure water (seawater 

or freshwater) into each flask. For the 

positive control flasks, use exposure water 

containing nutrients. Alternatively, the 

artificial exposure water can be dispensed 

into clean flasks and then autoclaved. 

5.4.4 Tare the labeled flasks containing 

exposure water and other additions, as 

necessary, on the balance with a minimum 

accuracy of 0.01 g. Add drop-wise 0.50 g oil 

(this results in a final oil concentration of 5 

g/L) using a sterile Pasteur pipette to the 

center of the flask taking care to avoid 

splashing the oil onto the sides of the flasks. 

Record the precise weight. ANS521 may be 

previously warmed in a hot water bath to 

facilitate its flow. Take precautions when 

handling and charging the flasks to minimize 

the likelihood of contamination by 

exogenous microbes, including using a new 

sterile pipette for each series of flasks. 

5.4.5 Preparation of the EPA culture for 

both the positive control flasks and the flasks 

containing non-living bio-stimulation 

products. Use two vials containing 

approximately 5 mL of the known EPA 

culture frozen in glycerol. Thaw both vials at 

room temperature, transfer the contents of 

both thawed vials to a single sterile 

centrifuge tube, rinse tubes with two volumes 

each of sterile exposure water, centrifuge at 

between 6,000 and 7,000 ×s gravity (6,000– 

7,000 × g) for 15 minutes using a fixed rotor 

to fully pellet the cells. 

5.4.6 Positive control flasks contain 

exposure water, oil, nutrients, and the EPA 

culture. 

5.4.7 Negative killed control flasks for all 

products shall contain exposure water, oil, 

product, the EPA culture for products not 

containing a living culture, and the sodium 

azide sterilant at a final concentration of 0.5 

g/L. Add the sodium azide sterilant prior to 

adding any product or EPA culture. For the 

negative killed control flasks and product 

flasks, prepare and add the product to the 

flasks in a concentration specified by the 

manufacturer or vendor. 

5.4.8 For non-living products that contain 

nutrient only, use the EPA culture as the 

inoculum. 

5.4.9 For other non-living products (e.g., 

enzymes), do not add nutrients or the EPA 

culture as the inoculum as they are not 

needed. 

5.4.10 For products containing microbial 

cultures, prepare 6 flasks the same way as in 

Steps a-d, but without the EPA culture. A 

product that contains its own nutrients must 

not be amended with nutrients, unless the 

product contains insufficient nutrients. Since 

this is a closed flask test, nutrients could be 

limiting if they are at the same concentration 

as used in the field. This could cause the 

product to fail the test. Thus, the 

manufacturer has the option to supplement 

its product with a higher concentration of 

nutrients than that contained in the product. 

Any nutrient supplements to a product must 

be reported and must not exceed the 

concentration limits in Table 10 (for 

seawater) and 13 (for freshwater) of this 

Appendix, as applicable. 

5.4.11 Cap all flasks either with cotton 

stoppers or loosely applied aluminum foil to 

allow gas exchange with the atmosphere. Set 

aside the T=0 flasks for immediate extraction 

and analysis. Place the rest of the flasks onto 

the orbital shaker table. Do not tip the flasks 

excessively to avoid stranding oil above the 

mixing area of the flask. Set the orbital shaker 

to 200 rpm and shake the flasks for 28 days 

at 20–23° C. 

5.4.12 Submit all information on added 

cultures and nutrients for testing in the data 

report. 

5.5 Sampling and Chemical Analysis 

5.5.1 Summary. At each sampling event 

(Days 0 and 28), product and control flasks 

are sacrificed for analysis of residual oil 

concentrations (SOP 4 of this Appendix). 

Record all physical observations for each 

flask (such as degree of emulsification, 

whether the oil has congealed into tar balls, 

wall growth, color, etc.) at each sampling. 

The analytical procedure is summarized in 

Table 16 of this Appendix. Dichloromethane 

(DCM) is the solvent used for the initial 

extraction. Solvent-exchange the extract into 

hexane prior to injection into the gas 

chromatograph. The solvent exchange is 

done to prevent asphaltenes from 

contaminating the column. 

TABLE 16—BIOREMEDIATION EFFICACY—SUMMARY OF ANALYTICAL PROCEDURES

Matrix Measurement Sampling/measurement 

method 

Analysis 

method 

Sample container/quantity of 

sample 

Preservation/storage 

Holding 

times 

DCM ......... N/A ....................................... Solvent Exchange to 

Hexane.

N/A .......... Capped Vial with Teflon 

septa, 30 mL.

4 °C ......... 6 months. 

Hexane ..... Hydrocarbon Concentration SOP 4 .................................. GC/MS ..... Capped Vial with Teflon 

septa, 10 mL.

4 °C ......... 6 months. 

5.5.2 Hydrocarbon Extraction. To 

measure extraction efficiency, 500 mL of the 

surrogate recovery standard (compounds and 

concentrations described in SOP 1 in this 

Appendix) is added to each flask. Add 50 mL 

DCM to each flask. Use magnetic stir bars to 

stir the flasks for 20 minutes to transfer the 

oil into the DCM phase. Allow the flasks to 

stand one hour for phase separation. If an 

emulsion remains after one hour, centrifuge 

the emulsion in Teflon® centrifuge tubes for 

at least ten minutes in a low speed centrifuge 

at 3,000 × gravity (3,000 × g) to break the 

emulsion and recover the DCM phase. Pass 

the DCM extract through a funnel plugged 

with glass wool and containing 

approximately 20 g anhydrous, granular 

sodium sulfate (Na2SO4) to remove water. 

Collect the extract in 30 mL serum vials, 

capped with Teflon lined septa and 

aluminum crimp seals, and store at 4 °C for 

up to 6 months. 

5.5.3 Solvent Exchange. Perform a solvent 

exchange (DCM to hexane) prior to GC/MS 

analysis to prevent injection of asphaltenes 

into the GC/MS column. Using a Class A 

volumetric pipette, transfer10 mL of DCM 

extract to 16 x 125 mm test tubes with Teflon 

lined screw caps. Place the test tubes in a 37° 

C water bath under a stream of dry nitrogen 

gas. Reduce the sample to 1 mL and return 

to volume with hexane. Repeat the blow 

down and re-suspension twice to exchange 

the hydrocarbons from DCM into the hexane. 

5.5.4 Hydrocarbon Analysis. Quantify the 

concentrations of 25 alkanes (including 

hopane) and 31 aromatics (SOP 4, Table SOP 

4.1 of this Appendix) using an Agilent 6890 

GC/5973 MS or equivalent equipped with a 

30-m × 0.25-mm ID × 0.25-mm film thickness 

DB–5 or equivalent fused silica column. To 

prepare the samples, transfer 1.0 mL of the 

hexane extract into a 2 mL autosampler vial 

with Teflon lined cap. Add 20 mL of internal 

standard solution to each vial with a syringe 

or positive displacement pipettor. SOP 2 of 

this Appendix outlines the procedure for 

preparing the internal standard solution. 

Load vials onto the autosampler tray and 

analyze in selected ion monitoring mode 

(SIM). Sum the individual alkane 

concentrations for the total alkane 

concentration and the individual aromatic 

concentrations for total aromatic 

concentrations in each flask. 

5.6 Quality Assurance/Quality Control (QA/ 

QC) 

5.6.1 Objectives. The critical variables to 

be analyzed for each set of experimental 

conditions are the individual petroleum 

hydrocarbons, i.e., the alkanes ranging in 

carbon number from nC–14 to nC–35, plus 

pristane and phytane, and the 2- to 4-ring 

polycyclic aromatic hydrocarbons (PAHs) 

and their alkylated homologs as listed in SOP 

4 of this Appendix. The quality assurance 

objectives for precision, accuracy, and 

detection limits are ± 20%, 75–125% 

recovery, and 22.5 mg/L, respectively. For 

more details, refer to the SOPs of this 

Appendix. 

5.6.2 Precision Objectives. Precision is 

presented as relative percent difference (RPD) 

for duplicate measurements and as relative 

standard deviation (RSD, or coefficient of 

variance) for triplicate measurements, 

applicable to replication of treatments as 

separate samples. 

5.6.3 Accuracy Objectives. These are 

based on the check standards and standard 

oil samples run concurrently with the sample 

analyses for GC/MS analysis of critical 


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compounds. Critical compounds in the check 

standards and in the oil standards must fall 

within 75–125% of expected values for the 

analysis to be valid. Six surrogate 

compounds (SOP 1 of this Appendix) added 

to each sample before extraction can also 

serve as a surrogate for determining accuracy. 

The measured surrogate concentrations must 

fall within 75–125% of expected values. 

5.6.4 Calibration Range. Conduct all 

measurements within the linear calibration 

range of the instrument. The calibrated 

concentration range for GC/MS analysis is 1 

mg/L to 30 mg/L. If the measured 

concentration of any critical compound is 

above the calibration range, dilute the sample 

and re-analyze to quantify that particular 

compound within the linear calibration 

range. 

5.6.5 Quality Control. Table 17 of this 

Appendix summarizes the QC checks for 

each measurement. See the corresponding 

SOP in this Appendix for detailed 

descriptions of QC checks, frequency, 

acceptance criteria, and corrective actions. 

TABLE 17—QA/QC CHECKS

Sample 

matrix Measurement QA/QC check Frequency Acceptance criteria Corrective action 

DCM ......... GC/MS hydrocarbon 

analysis.

Blanks ........................... Once per calibrated run Peak area of interfering 

peaks <10% of lowest 

standard peak area.

Flush with solvent, 

clean injection port, 

and/or bake column. 

DCM ......... GC/MS hydrocarbon 

analysis.

DFTPP Check Standard Once per calibrated run Must pass all DFTPP 

criteria.

If any criteria fail, retune 

and rerun DFTPP 

check standard. 

DCM ......... GC/MS hydrocarbon 

analysis.

Initial Calibration Samples.Once per calibrated run Response Factor RSD 

≤25%.

If RSD for any one 

compound >25%, recalibrate. 

DCM ......... GC/MS hydrocarbon 

analysis.

Calibration Check 

Standards.

Every 10–15 samples ... ± 25% of expected values.If >5 compounds are 

out of range, recalibrate and rerun samples. 

Hexane ..... GC/MS hydrocarbon 

analysis.

Surrogates .................... Every Sample ............... ± 30% of expected values.Re-inject. 

Hexane ..... GC/MS hydrocarbon 

analysis.

Biomarker Concentration.Every Sample ............... ± 25% of average values.Re-inject. 

5.7 Pass/Fail Criteria 

5.7.1 Calculate the mean and standard 

deviation of the hopane-normalized total 

aromatics (sum of all resolved aromatics) and 

hopane-normalized total alkane 

concentrations (sum of all resolved alkanes) 

from the 6 independent replicates at days 0 

and 28. To normalize, divide the sum of the 

alkane analytes and the sum of the aromatic 

analytes in each replicate by the hopane 

concentration in the corresponding replicate. 

5.7.2 From those data, calculate the 95% 

Upper Confidence Level (UCL95) at days 0 

and 28 using the following formula (Equation 

11 of this Appendix): 

Where: 

xt28 = total hopane-normalized alkane or total 

hopane-normalized aromatic mean of 6 

replicates at days 0 and 28, 

t95, 5 df = the 95% one-tailed t-value with 5 

degrees of freedom (2.015), 

s = the standard deviation of the 6 replicates 

at day 0 and 28, and 

n = no. of replicates = 6. 

5.7.3 Using Equation 12 of this Appendix, 

calculate the % reduction of each oil fraction 

from day 0 to day 28, using the day 0 and 

28 UCL95 hopane-normalized values for each 

fraction: 

Where: 

t28(UCL95) = UCL95 of the hopane-normalized 

total alkane or total aromatic mean of 6 

replicates on day 28, and 

t0(UCL95) = UCL95 of the hopane-normalized 

total alkane or total aromatic mean of 6 

replicates on day 0. 

5.7.4 A product is successful in saltwater 

if the % reduction of total alkanes (aliphatic 

fraction) from the GC/MS analysis is greater 

than or equal to 95% and the % reduction 

of total aromatics (aromatic fraction) is 

greater than or equal to 70% at day 28 based 

on the UCL95 (Equation 12 of this Appendix). 

For freshwater, a product is successful if the 

% reduction of total alkanes and total 

aromatics is greater than or equal to 95% and 

40%, respectively. The benchmark reduction 

ranges in aliphatic and aromatic fractions for 

the positive control are the same as for the 

products specified above. The average 

concentration of the biomarker hopane at day 

28 must not differ from the average 

concentration at day 0 by more than 12% in 

the positive control. If the conditions for the 

positive control are not met, the entire 

procedure must be repeated. 

5.8 Data Verification and Reporting. GC/ 

MS data files are generated by MS 

ChemStation software (the Agilent standard 

software for GC/MS) or equivalent for each 

injection. Data files contain summed ion 

chromatograms and selected ion 

chromatograms. Calibration curves are 

generated within MS ChemStation software, 

and all data files are calculated against the 

calibration curve by MS ChemStation. Data 

verification would be done by crosschecking 

between analysts for 10% of the raw data and 

its reduction process. 


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5.9 Laboratory Report. The summary of 

findings from a product test must include the 

data listings for each analyte that was 

analyzed (i.e., all individual alkanes and 

aromatics in the list of required analytes). 

Express all concentrations as mg analyte/L 

exposure water. 

5.10 Standard Operating Procedures (SOPs) 

1–4 

5.10.1 SOP 1. Preparation of Surrogate 

Recovery Standards 

5.10.1.1 Preparation: 

5.10.1.1.1 Solvents: Dichloromethane 

(DCM), Optima (Fisher) grade or equivalent. 

5.10.1.1.2 Reagents: D36-Heptadecane 

(C17), D50-Tetracosane (C24), D66- 

Dotriacontane (C32), D10–1- 

Methylnaphthalene, D10-Phenanthrene, D10- 

Pyrene, 5-beta-cholestane (coprostane). 

Note: Deuterated reagents are available 

from Cambridge Isotope Laboratories, 

Andover, MA. 

5.10.1.1.3 Equipment: Micro-spatula, 

Small beakers, Glass funnel, Analytical 

balance (0.0001g), Vials with Teflon-lined 

caps, Teflon wash bottle with Optima grade 

DCM, Volumetric flask (250 mL), class A, 

Pasteur pipettes. 

5.10.1.2 Procedure: 

5.10.1.2.1 Using a calibrated analytical 

balance, weigh 100 mg (0.100 g) of each 

reagent into separate 10–25 mL beakers. 

5.10.1.2.2 Dissolve the reagents in their 

beakers by adding 10 mL DCM. Use a Pasteur 

pipette to transfer the solutions to a single 

250 mL volumetric flask. 

5.10.1.2.3 Wash the beakers 3 or 4 times 

with DCM. Use a Pasteur pipette to transfer 

each of the washings to the 250 mL 

volumetric flask. 

5.10.1.2.4 Dilute the solution to the 250 

mL volume mark on the volumetric flask 

with DCM. 

5.10.1.2.5 Use a glass stopper to seal the 

flask and homogenize the solution by 

inverting the flask 5 or more times. The final 

concentration of this solution is 400 mg/L for 

each of the reagents. 

5.10.1.2.6 Transfer the solution into 40 

mL storage vials and cap with Teflon-lined 

caps and label each with the date of 

preparation, operator, sample names, and 

concentrations. 

5.10.1.2.7 Weigh each vial and record its 

weight on the label. This weight is used to 

monitor possible evaporation during storage. 

5.10.1.2.8 Store these vials at 0 °C or 

lower. 

5.10.1.2.9 Before using, allow the 

solution to come to room temperature, and 

then shake it well. 

5.10.1.2.10 Weigh the vial before using it, 

and compare the weight with the last weight 

recorded on the vial. 

5.10.1.2.11 If the weights are consistent, 

the integrity of the solution can be assumed. 

If not, investigate and resolve the cause. 

Prepare a new solution if the integrity has 

been compromised. 

5.10.1.3 Quality Control: Inject 20 mL of 

the surrogate stock solution into 1 mL DCM. 

Add 20 mL of the internal standard solution 

(SOP 2 of this Appendix). Analyze this 

solution by GC/MS using a calibrated method 

(SOPs 3 and 4 of this Appendix). The 

expected concentration of each of the 

corresponding surrogate compounds is 8 ± 2 

mg/L. If the measured value does not fall 

within this range, prepare and measure 

another independent surrogate solution. If 

the measured concentration of the second 

surrogate solution is within the allowable 

tolerance range, the calibration and 

instrument conditions are acceptable; 

properly discard the first surrogate solution. 

If the concentration of the second surrogate 

solution is also out of range, then clean and 

recalibrate the instrument until the problem 

is resolved. 

5.10.2 SOP 2. Preparation of Internal 

Standard Solution 

5.10.2.1 Preparation 

5.10.2.1.1 Solvents: Dichloromethane 

(DCM), Optima (Fisher) grade or equivalent. 

5.10.2.1.2 Reagents: D34 n-Hexadecane 

(C16), D42 n-Eicosane (C20), D62 nTriacontane (C30), D8-Naphthalene, D10- 

Anthracene, D12-Chrysene, 5-alphaAndrostane. 

Note: Deuterated reagents are available 

from Cambridge Isotope Laboratories, 

Andover, MA. 

5.10.2.1.3 Equipment: Micro-spatula, 

Small beakers, Glass funnel, Analytical 

balance (0.0001g), calibrated and checked for 

accuracy, Amber vials with Teflon-lined 

caps, labeled, Teflon wash bottle with DCM, 

Volumetric flask (200 mL), class A, Pasteur 

pipettes. 

5.10.2.2 Procedure: 

5.10.2.2.1 Using a calibrated analytical 

balance, weigh 100 mg (0.100 g) of each of 

the reagents into separate small beakers. 

5.10.2.2.2 Dissolve the reagents in their 

beakers by adding 10 mL DCM; using a 

Pasteur pipette, transfer the solutions to a 

single 200 mL volumetric flask. 

5.10.2.2.3 Wash the beakers 3 or 4 times 

with DCM; use a Pasteur pipette to transfer 

each of the washings to the 200 mL volume 

mark on the volumetric flask. 

5.10.2.2.4 Dilute the solution with DCM 

to the 200 mL volume. 

5.10.2.2.5 Seal the flask with a glass 

stopper and homogenize the solution by 

inverting the flask a minimum of 5 times. 

The final concentration of this solution is 500 

mg/L of each reagent. 

5.10.2.2.6 Transfer the solution into 40 

mL storage vials and cap with Teflon-lined 

caps. Label each vial with the date of 

preparation, operator, sample names, and 

concentrations. 

5.10.2.2.7 Weigh each vial, and record its 

weight on the label. This weight is used to 

monitor possible evaporation during storage. 

5.10.2.2.8 Store this solution at 0 °C or 

lower. 

5.10.2.2.9 Before using, allow the 

solution to come to room temperature, and 

then shake it well. 

5.10.2.2.10 Weigh the vial before using it, 

and compare the weight with the last weight 

recorded on the vial. 

5.10.2.2.11 If the weights are consistent, 

the integrity of the solution can be assumed. 

If not, investigate and resolve the cause. 

Prepare a new solution if the integrity has 

been compromised. 

5.10.2.3 Quality Control: Inject 20 mL of 

the internal standard solution into 1 mL 

DCM. Analyze this solution by GC/MS. The 

only peaks corresponding to the internal 

standards must appear. If other peaks appear, 

particularly close to the internal standard 

peaks, discard the internal standard solution 

and prepare a new solution. 

5.10.3 SOP 3. Preparation of Working 

Standards, Check Standards, and Oil 

Standards for GC/MS Consistency. 

5.10.3.1 Preparation: 

5.10.3.1.1 Solvent: Dichloromethane 

(DCM), Optima (Fisher) grade or equivalent. 

5.10.3.1.2 Stock solutions: 

5.10.3.1.2.1 Oil analysis standard: 44 

compounds, 100 mg/L in hexane/DCM (9:1), 

four, 1-mL vials required. Available from 

Absolute Standards, Inc., Hamden, CT, Part 

# 90311. 

5.10.3.1.2.2 Nine compound PAH 

standard: 1,000 mg/L in DCM, one vial. 

Available from Absolute Standards, Inc., 

Hamden, CT, Part # 90822. 

5.10.3.1.2.3 1,2-Benzodiphenylene 

sulfide, (synonym for 

naphthobenzothiophene). Prepare a 2 mg/mL 

stock solution. Available from Sigma-Aldrich 

Co., Part # 255122, purity 99%. 

5.10.3.1.2.4 Hopane solution (17 b (H), 

21b (H), 0.1 mg/mL in isooctane. Available 

from Sigma-Aldrich Co. Part # 07562. 

5.10.3.1.2.5 Surrogate solution: 400 mg/L 

of each reagent in DCM (see SOP 1 of this 

Appendix). 

5.10.3.1.2.6 Internal standard solution, 

500 mg/L in DCM (see SOP 2 of this 

Appendix). 

5.10.3.1.3 Alaska North Slope Crude Oil 

521 (ANS521). 

5.10.3.1.4 Equipment: 

5.10.3.1.4.1 Glass storage vials with 

Teflon-lined caps (2 mL and 40 mL capacity); 

5.10.3.1.4.2 Volumetric flasks, Class A, 5 

mL, 10 mL, and 100 mL. 

5.10.3.1.4.3 Glass syringes capable of 

dispensing 25–500 mL with an accuracy and 

precision of ± 1%, or equivalent. 

5.10.3.1.4.4 Wheaton repetitive 

dispenser, Model 411 STEP–PETTE or 

equivalent. 

5.10.3.1.4.5 Teflon wash bottle filled with 

Optima grade DCM or equivalent grade DCM. 

5.10.3.1.4.6 Pasteur pipettes. 

The volumes of stock solutions required to 

make the working standards are listed in 

Table SOP 3.1 of this Appendix. 


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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 

Working standards concentration, mg/L 

Oil Analysis 

Mix (44 

compounds, 

100 mg/L) 

μL 

Aromatics 

Mix (9 compounds, 

1000 mg/L) 

μL 

1,2-Benzodiphenylene 

sulfide 

(NBT) (2 

mg/mL) 

μL 

Surrogate 

solution 

(100 mg/L) 

μL 

Hopane solution (100 

mg/L) 

μL 

Volumetric 

Flask Volume 

mL 

ISTD (500 

mg/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 

preparation 

of STD 2.5 

& STD 1).

0 

STD 2.5 (0.5 mg/L hopane) .................. Use 5 mL of STD 5-Utility and dilute to 10 mL 200 

STD 1 (0.2 mg/L hopane) ..................... Use 2 mL of STD 5-Utility and dilute to 10 mL 200 

* Make extra STD 5 for use as check standard. 

5.10.3.2 Procedure for Working Standards 

and Check Standards: 

5.10.3.2.1 Label three 5 mL volumetric 

flasks as STD30, STD20, STD10, and two 10 

mL volumetric flasks as STD5, and STD5- 

utility. 

5.10.3.2.2 Add 1–2 mL of DCM to each 

volumetric flask. 

5.10.3.2.3 Using glass syringes, add the 

appropriate volume of stock solution A (as 

listed in Table SOP 3.1 of this Appendix) to 

the flasks labeled STD30, STD20, STD10, 

STD5, and STD5-utility. 

5.10.3.2.4 Wash the walls of the inner 

neck of the flasks with several drops of DCM 

to rinse off the residue of the stock solution 

into the flasks. 

5.10.3.2.5 Repeat Step 3 and Step 4 to 

dispense stock solutions B–E (do not add 

stock solution F, internal standard solution, 

at this step). 

5.10.3.2.6 Dilute to volume with DCM for 

all the above flasks, seal with glass stoppers, 

and invert several times to homogenize the 

solutions. 

5.10.3.2.7 Label two additional 10 mL 

volumetric flasks as STD2.5 and STD1. Wet 

with 1–2 mL DCM. 

5.10.3.2.8 Dispense 5 mL of STD5-utility 

solution into flask STD2.5, and 2 mL of 

STD5-utility solution into flask STD1. 

5.10.3.2.9 Dilute to volume with DCM, 

seal with glass stoppers, and invert several 

times to homogenize the solutions. 

5.10.3.2.10 Using a 100 mL glass syringe, 

dispense 100 mL of internal standard solution 

into flasks STD30, STD20, and STD10. 

Dispense 200 mL into flasks STD5, STD2.5, 

and STD1 to give a final concentration of 10 

mg/L internal standard. 

5.10.3.2.11 Seal with glass stoppers, and 

invert the flasks several times to homogenize 

the solutions. 

5.10.3.2.12 Transfer the solutions into 2 

mL storage vials, and cap with Teflon-lined 

caps. 

5.10.3.2.13 Label each vial with date of 

preparation, analyst, sample names, and 

concentrations. 

5.10.3.2.14 Weigh each storage vial and 

record its weight on the label. This weight is 

used to monitor possible evaporation during 

storage. 

5.10.3.2.15 Store this solution at 0 °C or 

below. 

5.10.3.2.16 Before using, allow the 

solution to come to room temperature, and 

shake it well. 

5.10.3.2.17 Weigh the vial before 

opening, and compare the weight with the 

last weight recorded on the vial. If the 

weights are consistent, the integrity of the 

solution can be assumed. If not, investigate 

and resolve the cause. Do not use the 

solution if the integrity has been 

compromised. 

5.10.3.3 Procedure for Oil Standard. In a 

100 mL volumetric flask, weigh 0.500 g of the 

standard ANS521 crude oil, add 2 mL of 

surrogate solution (see SOP 1 of this 

Appendix), and bring to volume with DCM. 

Add 2 mL of internal standard solution (see 

SOP 2 of this Appendix). Follow steps 

5.10.3.2.11 through 5.10.3.2.17 of this SOP, 

substituting 40 mL storage vials for the 2 mL 

vials. 

5.10.3.4 Quality Control/Quality 

Assurance: 

5.10.3.4.1 Run the six standard solutions 

using the GC/MS method (SOP 4) on a tuned 

GC/MS. Use the EnviroQuant software or 

equivalent to calculate the average Relative 

Response Factor (RRF) and the relative 

standard deviation (RSD) of the RRFs for 

each analyte over the six concentrations. The 

RRF is defined as: 

5.10.3.4.2 The RSD of the RRFs for all 

analytes must be 25% or less according to 

EPA Method 525.2. 

5.10.4 SOP 4. GC/MS Method for the 

Analysis of Crude Oil Samples. 

5.10.4.1 Instrument Specifications: 

5.10.4.1.1 Use an Agilent 6890 GC 

coupled with an Agilent 5973 mass selective 

detector (MSD) and an Agilent 6890 series 

auto sampler or equivalent, equipped with a 

DB–5 capillary column (30 m, 0.25 mm I.D., 

and 0.25 mm film thickness) or equivalent, 

and a split/splitless injection port operating 

in the splitless mode. Data acquisition occurs 

either in the SIM (selected ion monitoring) 

mode for quantitative analysis or in SCAN 

mode for qualitative analysis. In SIM mode, 

the dwell time of each ion is set to be 10 

milliseconds and the ions are split up into 

groups by retention time. One way to divide 

the ions is by retention time grouping as 

shown in Table SOP 4–1 of this Appendix. 

The number of ions in each ion group must 

be constant, yielding the same scan rate for 

each group. 

TABLE SOP 4–1—IONS ASSOCIATED

WITH RETENTION TIME GROUPS

Group Ions 

1 ............... 57, 66, 128, 136, 142, 152, 156, 

166, 170, 184 

2 ............... 57, 66, 166, 170, 178, 180, 184, 

188, 192, 194, 198, 208 

3 ............... 57, 66, 178, 184, 188, 192, 194, 

198, 202, 206, 208, 212, 220, 

226 


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TABLE SOP 4–1—IONS ASSOCIATED

WITH RETENTION TIME GROUPS— 

Continued 

Group Ions 

4 ............... 57, 66, 192, 198, 202, 206, 208, 

212, 216, 220, 226, 230, 234, 

245 

5 ............... 57, 66, 191, 217, 228, 240, 242, 

248, 256, 262, 264, 270, 276, 

284 

5.10.4.1.2 Table SOP 4.2 of this Appendix 

summarizes the instrumental conditions for 

crude oil analysis. Use only ultra-high purity 

helium (99.999% pure) as the carrier gas. In 

series, connect a moisture trap, an oxygen 

trap, and an organic trap to the carrier gas 

line before it enters the column. 

TABLE SOP 4.2—INSTRUMENTAL

CONDITIONS FOR CRUDE OIL ANALYSIS

Instrument .............. Agilent 6890 Series II 

Gas Chromatograph 

(GC) with an Agilent 

5973MSD and an 

Agilent 6890 auto 

sampler, or equivalent. 

Column .................. DB–5 capillary column 

(30 m, 0.25 mm I.D., 

and 0.25-μm film 

thickness) or equivalent. 

Carrier Gas ............ Helium, ultra-high purity 

grade (99.999%). 

Inlet Temperature .. 300 °C. 

Transfer Line (detector) Temperature.310 °C. 

Oven Temperature 

Program.

50 °C for 4 minutes, 

then 7 °C/min to 310 

°C, hold for 18 minutes. 

TABLE SOP 4.2—INSTRUMENTAL CONDITIONS FOR CRUDE OIL ANALYSIS— 

Continued 

Flow Rate ............... Constant flow at 1mL/

min. Linear velocity: 

36.2 cm/sec. 

Injection Volume .... 1 μL. 

Split/Splitless Mode Splitless. 

Total Run Time ...... 59.18 minutes. 

5.10.4.2 Procedure for preparing the 

instrument: 

5.10.4.2.1 Lower the injection port 

temperature and the oven temperature to 50° 

C or less to avoid oxidation of the column. 

5.10.4.2.2 Replace the liner with a clean, 

silanized liner. Do not touch the liner with 

bare fingers. A small piece of muffled glass 

wool may be inserted to protect the column. 

5.10.4.2.3 Return the injection port and 

oven to the appropriate temperatures. 

5.10.4.2.4 Wait five minutes after the 

temperature equilibrates before using the 

instrument. 

5.10.4.3 Procedure for tuning the MSD: 

5.10.4.3.1 Perform an air/water check. 

The value reported for the relative abundance 

of water (m/z 18), nitrogen (m/z 28), oxygen 

(m/z 32), or carbon dioxide (m/z 44) shall be 

less than 5% of the base peak for the system 

to be considered leak free. 

5.10.4.3.2 Tune the MSD using the 

Standard Autotune program and the 

decafluorotriphenylphosphine (DFTPP) Tune 

program to reduce instrument variability. 

The Autotune report file is referenced by the 

instrument when performing an air/water 

check and thus must be run at least once per 

month. Run standards and samples using 

DFTPP Tune parameters, and retune the 

instrument using DFTPP Tune at least once 

per week. The tune programs use three 

fragment ions of perfluorotributylamine 

(PFTBA) as a standard for tuning: m/z 69, 

219, and 502. Tune reports must meet the 

following criteria: 

5.10.4.3.2.1 Symmetrical peaks; 

5.10.4.3.2.2 Mass assignments within ± 

0.2 amu’s from 69, 219, and 502; 

5.10.4.3.2.3 Peak widths within 0.5 ± 0.1 

amu’s; 

5.10.4.3.2.4 Relative abundance is 100% 

for ion 69, at least 35% for ion 219, and at 

least 1% for ion 502; 

5.10.4.3.2.5 Relative abundances for 

isotope masses 70, 220, and 503 ± 0.2 amu’s 

are 0.5–1.5%, 2–8%, and 5–15%, 

respectively; and 

5.10.4.3.2.6 Air and water peaks at m/z = 

18, 28, 32, and 44 amu’s must be very small 

and consistent with historical values. 

5.10.4.4 Maintaining a log book. Maintain 

an instrument logbook, and make entries for 

each use. Include the following information 

in the logbook: operator name, helium 

cylinder tank pressure and outlet pressure, 

vacuum gauge reading, any maintenance 

performed on the instrument (such as 

changing the injection port liner, gold seal, 

guard column, source cleaning), sequence 

name, data path, samples in order of 

injection, method information, GC column 

number, and the Standard Auto Tune report 

and DFTPP Tune report. 

5.10.4.5 Running a Solvent Blank: 

Following a liner change or at the start of a 

new run, run an injection of a pure solvent 

to confirm that the system is free of excessive 

or interfering contamination. Analyze the 

solvent in SCAN mode using the same 

temperature program used for sample 

analysis. If contamination is present, analyze 

additional samples of fresh solvent until the 

interfering contamination is removed. 

5.10.4.6 Checking the DFTPP Tune: Prior 

to running the first calibration standard, 

verify the instrument tune conditions by 

running a 10 ng/mL DFTPP check standard to 

check the mass measuring accuracy of the 

MS, the resolution sensitivity, the baseline 

threshold, and the ion abundance ranges. 

Run the standard using the DFTPP method 

provided with the instrument. Each of the 

criteria identified in Table SOP 4.2 of this 

Appendix must be met before using the 

instrument for analysis: 

TABLE SOP 4.3—ION ABUNDANCE CRITERIA FOR DFTPP 

Mass, M/z Relative to 

mass Relative abundance criteria Purpose of checkpoint 

51 .............................................................. 442 10–80% of the base peak ........................ Low mass sensitivity. 

68 .............................................................. 69 <2% of mass 69 ....................................... Low mass resolution. 

70 .............................................................. 69 <2% of mass 69 ....................................... Low mass resolution. 

127 ............................................................ 442 10–80% of the base peak ........................ Low-mid mass sensitivity. 

197 ............................................................ 198 <2% of mass 198 ..................................... Mid mass resolution. 

198 ............................................................ 442 Base peak or >50% of 442 ...................... Mid mass resolution and sensitivity. 

199 ............................................................ 198 5–9% of mass 198 .................................... Mid mass resolution and isotope ratio. 

275 ............................................................ 442 10–60% of the base peak ........................ Mid-high mass sensitivity. 

365 ............................................................ 442 >1% of the base peak .............................. Baseline threshold. 

441 ............................................................ 443 Present and < mass 443 .......................... High mass resolution. 

442 ............................................................ 442 Base peak or >50% of 198 ...................... High mass resolution and sensitivity. 

443 ............................................................ 442 15–24% of mass 442 ................................ High mass resolution and isotopic ratio. 

5.10.4.7 Calibrating with a Multiple-Point 

Calibration Curve. A 5- or 6-point calibration 

curve is obtained by running 5 or 6 working 

standards (see SOP 3) on the tuned GC/MS 

instrument. Calculate the relative response 

factor (RRF) for each compound relative to its 

corresponding deuterated internal standard 

as indicated in Table SOP 4.3 of this 

Appendix. The relative standard deviation 

(RSD) of the RRFs for each compound must 

be less than 25%. Run an independently 

prepared check standard immediately after 

the calibration standards to validate the 

accuracy of the calibration curve. 

5.10.4.8 Running Samples. Once the 

calibration curve has been validated, samples 

can be analyzed. Dispense 1,000 mL of sample 

extract into labeled auto-sampler vials. Add 


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20 mL of the internal standard solution (see 

SOP 2 of this Appendix) to the extract using 

a syringe or a positive displacement pipettor. 

Run a check standard every 10 samples to 

ensure the consistency of the instrument. The 

RRF for each compound in the check 

standard must be within 25% of the average 

RRF obtained in the initial calibration. 

5.10.4.9 Quantification: Once a 

calibration table has been generated, quantify 

each data file using the ‘‘Calculate and 

Generate’’ function in the MS ChemStation 

software, or equivalent software. Review 

individual peak integration manually to 

ensure proper baseline integration. The 

quantification of a compound is based on the 

peak area of the primary ion (Q Ion) 

indicated in Table SOP 4.4 of this Appendix. 

TABLE SOP 4.4—TARGET COMPOUND LIST

Compound name Quantitation 

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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3446 Federal Register / Vol. 80, No. 14 / Thursday, January 22, 2015 / Proposed Rules 

TABLE SOP 4.4—TARGET COMPOUND LIST—Continued 

Compound name Quantitation 

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: 

Aanalyte = the peak area of the analyte, 

Cistd = the concentration of the internal 

standard, 

Aistd = the area of the internal standard, 

RRF = the relative response factor, and 

100 is the conversion factor to convert mg/ 

L DCM to mg/g oil added. 

5.10.4.11 If some analytes are not 

commercially available, the RRFs of other 

compounds (usually the parent compound) 

are used to quantify those analytes. For 

example, the RRF of C3-naphthalene may be 

used to calculate the concentrations of C3- 

and C4-naphthalenes. See Table SOP 4.4 of 

this Appendix for details. The quantification 

of these alkylated PAHs is relative because it 

is assumed that the molecular ions of the 

alkylated PAHs have the same RRFs as the 

parent compound ions. Nevertheless, these 

relative concentrations are useful for 

monitoring the fate of these compounds 

during the course of any analysis, as long as 

their concentrations are measured in a 

consistent way throughout the analysis. 

5.10.4.12 Concentration calculations for 

all target compounds are performed using 

EnviroQuant software or equivalent. Data for 

each sample can be printed directly using a 

customized report template. Data can also be 

automatically entered into a spreadsheet 

within the EnviroQuant software. 

5.10.5 Quality Assurance/Quality 

Control. The following criteria must be met 

before any samples are analyzed: 

5.10.5.1 Air/water check to verify the 

system is leak free. 

5.10.5.2 AutoTune and DFTPP Tune pass 

all criteria. 

5.10.5.3 DFTPP check standard passes all 

criteria. 

5.10.5.4 Solvent blank scan indicates the 

GC/MS system is free of interfering 

contamination. 

5.10.5.5 Prepare and monitor a control 

chart of a standard oil analysis. 

Concentrations of the analytes in the control 

chart must be no more than 25% different 

from their historical averages. 

5.10.5.6 Relative response factors for 

analytes in the check standards inserted 

between every 10 samples must be no more 

than 25 percent different from the average 

RRF of those same analytes in the calibration 

curve. Peak shapes must be symmetrical. 

5.11 References for Section 5 

(1) Haines, J.R., E.J. Kleiner, K.A. McClellan, 

K.M. Koran, E.L. Holder, D.W. King, and 

A.D. Venosa. 2005. ‘‘Laboratory 

evaluation of oil spill bioremediation 

products in salt and freshwater systems.’’ 

J. Ind. Microbiol. Biotech 32: 171–185. 

Appendix E to Part 300 [Removed] 

■ 17. Remove Appendix E to Part 300. 

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

BILLING CODE 6560–50–P 


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