Guidelines Establishing Test Procedures for the Analysis of Oil and Grease and Non-Polar Material Under the Clean Water Act and Resource Conservation and Recovery Act; Final Rule

ENVIRONMENTAL PROTECTION AGENCY

40 CFR Parts 136 and 260

[FRL-6341-9]

RIN 2040-AC63

Guidelines Establishing Test Procedures for the Analysis of Oil

and Grease and Non-Polar Material Under the Clean Water Act and

Resource Conservation and Recovery Act; Final Rule

AGENCY: Environmental Protection Agency (EPA).

ACTION: Final rule.

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SUMMARY: This action approves use of EPA Method 1664, Revision A: N-

Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel

Treated N-Hexane Extractable Material (SGT-HEM; Non-polar Material) by

Extraction and Gravimetry (hereafter Method 1664) for use in EPA's

Clean Water Act (CWA) programs. This action also deletes Method 9070,

adds revised Method 9071B, and incorporates Method 1664 by reference

for use in EPA's Resource Conservation and Recovery Act (RCRA)

programs. Method 1664 is also approved for determination of non-polar

material (NPM) as silica gel treated n-hexane extractable material

(SGT-HEM) to support phaseout of use of CFC-113 for determination of

NPM in EPA's CWA and RCRA programs.

These actions are being taken as a part of EPA's effort to reduce

dependency on use of chlorofluorocarbons (CFCs) to protect Earth's

ozone layer and to meet the CFC phaseout agreed to in the Montreal

Protocol and required by the Clean Air Act Amendments of 1990. Method

1664 uses normal hexane (n-hexane) as the extraction solvent in place

of 1,1,2-trichloro-1,2,2-trifluoroethane (CFC-113; Freon-113), a Class

1 CFC.

DATES: This regulation is effective June 14, 1999. For judicial review

purposes, this final rule is promulgated as of 1:00 p.m. Eastern

Standard Time on May 28, 1999 in accordance with 40 CFR 23.7.

The incorporation by reference of Method 1664 is approved by the

Director of the Federal Register May 14, 1999.

ADDRESSES: Copies of the public comments received, EPA responses, and

all other supporting documents (including references included in this

notice) are available for review at the U.S. Environmental Protection

Agency, Water Docket, 401 M Street SW, Washington, DC 20460. For access

to docket materials, call 202-260-3027 on Monday through Friday,

excluding Federal holidays, between 9:00 a.m. and 3:30 p.m. Eastern

Time for an appointment.

Copies of Method 1664 are available from the National Technical

Information Service (NTIS), 5285 Port Royal Road, Springfield, VA

22161, (703) 605-6000 or (800) 553-6847. The NTIS publication number is

PB99-121949.

Copies of the Third Edition of SW-846 and Updates I, II, IIA, IIB,

and III (document number 955-001-00000-1) are available from the

Superintendent of Documents, U.S. Government Printing Office,

Washington, DC 20402, (202) 512-1800. Update IIIA is available through

EPA's Methods Information Communication Exchange (MICE) Service. MICE

can be contacted by phone at (703) 821-4690. Update IIIA can also be

obtained by contacting the U.S. Environmental Protection Agency, Office

of Solid Waste (5307W), OSW Methods Team, 401 M Street, SW, Washington,

DC, 20460. Copies of the Third Edition and all of its updates are also

available from the National Technical Information Service (NTIS), 5285

Port Royal Road, Springfield, VA 22161, (703) 605-6000 or (800) 553-

6847. In addition, a CD-ROM version of SW-846, Third Edition, as

amended by Updates I through III is available from NTIS (PB97-501928).

In the future, the CD-ROM will be updated by NTIS to include additional

updates, including Update IIIA.

An electronic version of Method 1664 and Method 9071B are also

available via the Internet at http://www.epa.gov/OST.

FOR FURTHER INFORMATION CONTACT: For information regarding Method 1664

and its use in Clean Water Act programs, contact Maria Gomez-Taylor,

Engineering and Analysis Division (4303), USEPA Office of Science and

Technology, 401 M Street, SW, Washington, DC 20460, or call (202) 260-

1639. For information regarding Update IIIA and the use of Method 1664

in the Resource Conservation And Recovery Act programs, contact Gail

Hansen, Office of Solid Waste (5307W), USEPA, 401 M Street, SW,

Washington, DC 20460, or call (703) 308-8855.

SUPPLEMENTARY INFORMATION:

Potentially Regulated Entities

EPA Regions, as well as States, Territories and Tribes authorized

to implement the National Pollutant Discharge Elimination System

(NPDES) program, issue permits that comply with the technology-based

and water quality-based requirements of the Clean Water Act. In doing

so, the NPDES permitting authority, including authorized States,

Territories, and Tribes, make a number of discretionary choices

associated with permit writing, including the selection of pollutants

to be measured and, in many cases, limited in permits. If EPA has

``approved'' standardized testing procedures (i.e., promulgated through

rulemaking) for a given pollutant, the NPDES permit must include one of

the approved testing procedures or an approved alternate test

procedure. Therefore, entities with NPDES permits could be affected by

the standardization of testing procedures in this rulemaking. These

entities may be affected because NPDES permits may incorporate the

standardized testing procedure approved for use in today's rulemaking.

In addition, when a State, Territory, or authorized Tribe provides

certification of federal licenses under Clean Water Act section 401,

States, Territories and Tribes are directed to use the standardized

testing procedures. Under the RCRA program, this method may be required

as part of a hazardous waste delisting petition. Categories and

entities that may ultimately be affected include:

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Examples of potentially

Category regulated entities

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Regional, State and Territorial States, Territories, and Tribes

Governments and Indian Tribes. authorized to administer the

NPDES permitting program;

States, Territories, and

Tribes providing certification

under Clean Water Act section

401; Governmental NPDES

permittees; Regional and State

offices implementing delisting

petitions.

Industry............................... Industrial NPDES permittees;

delisting petitioners.

Municipalities......................... Publicly-owned treatment works

with NPDES permits.

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This table is not intended to be exhaustive, but rather provides a

guide for readers regarding entities likely to be affected by this

action. This table lists the types of entities that EPA is now aware

could potentially be affected by this action. Other types of entities

not listed in the table could also be affected. If you have questions

regarding the applicability of this action to a particular entity,

consult the person listed in the preceding FOR FURTHER INFORMATION

CONTACT section.

Outline of Preamble

I. Authorities

A. Clean Water Act

B. Resource Conservation and Recovery Act

C. Clean Air Act Amendments of 1990

II. Background and History

[[Page 26316]]

A. Regulatory Background

B. Data Gathering

1. EPA's Freon Replacement Studies

2. Water Pollution Performance Evaluation Data

3. Data Received from Commenters

III. Explanation of Today's Action

A. Application of Method 1664 in Clean Water Act Program

1. General Use

2. Search for Other Uses of CFCs in Clean Water Act Program

B. Application of Method 1664 in Resource Conservation and

Recovery Act Program

C. Use of Solid-phase Extraction (SPE)

D. Differences in Results Produced by CFC-113 and n-Hexane and

Determinations of Compliance

IV. Timing of Required Use of Method 1664 and Phaseout of Use of

CFC-113

V. Improvements and Changes to Method 1664 Since Proposal

A. Names and Name Changes

1. Oil and Grease

2. Non-polar Material

B. Other Changes and Improvements

1. Changes to Quality Control

2. Miscellaneous Changes and Improvements

VI. Public Participation and Response to Comments

A. Regulatory Issues

B. Health and Safety Concerns

C. Economic Concerns

D. Solid-phase Extraction (SPE)

1. Comments Supporting Use of SPE

2. Comments Expressing Concern About the Use of SPE

E. Grace period for CFC-113

F. Use of Silica-gel Treated n-Hexane Extractable Material

Procedure

G. Detection and Quantitation

H. Matrix Effects

I. Method Modifications

J. Matrix Spike/Matrix Spike Duplicate

K. Precision and Recovery

L. Differences in Results Produced by n-Hexane and CFC-113

M. Method Validation and QC Acceptance Criteria

N. Quality Control

O. Sample Collection and Preservation

P. Miscellaneous Issues

VII. Regulatory Requirements

A. Executive Order 12866

B. Unfunded Mandates Reform Act

C. Regulatory Flexibility Act

D. Paperwork Reduction Act

E. Submission to Congress and the General Accounting Office

F. National Technology Transfer and Advancement Act

G. Executive Order 13045

H. Executive Order 12805

I. Executive Order 13084

I. Authorities

A. Clean Water Act

These regulations are being promulgated under the authority of

sections 301, 304, and 501(a) of the Clean Water Act (CWA), 33 U.S.C.

1311, 1314(h), 1361(a).

B. Resource Conservation and Recovery Act

These regulations are being promulgated under the authority of

sections 1006, 2002(a), 3001-3007, 3010, 3013-3018, and 7004 of the

Solid Waste Disposal Act (SWDA), as amended by the Resource

Conservation and Recovery Act of 1976 (RCRA), as amended (42 U.S.C.

6905, 6912(a), 6921-6927, 6930, 6934-6930, and 6974).

C. Clean Air Act Amendments of 1990

These regulations are consistent with intent of sections 604, 606,

and 608 of the 1990 Clean Air Act Amendments (CAAA) to phase out

production of Class I CFCs and reduce use and emissions of Class I CFCs

to the lowest achievable level, and with section 613 of CAAA to reduce

the Federal procurement of products and services that employ CFCs.

II. Background and History

A. Regulatory Background

This final rule affects regulations implementing analytical methods

under the Clean Water Act and the Resource Conservation and Recovery

Act. This final rule supports, in part, EPA's Stratospheric Ozone

Protection Program in the Office of Air and Radiation (OAR). The

regulatory background for each of these programs is not given in detail

in this rule; rather, pertinent proposals and rules are referenced, as

follows:

EPA provided a history of analytical methods under 40 CFR part 136

on February 7, 1991 (56 FR 5090) in the proposal of EPA Method 1613.

The Agency presented a brief background on the use of analytical

methods as support for effluent limitations, permit applications, and

compliance monitoring, and a brief description of the alternate test

procedure program (ATP) in the proposal of several new 40 CFR part 136

methods on October 18, 1995 (60 FR 53988). The details of Method 1664

and issues surrounding its use were given at proposal on January 23,

1996 (61 FR 1730).

The EPA Office of Solid Waste gave a brief description of the

regulatory framework for SW-846 methods in a final rule promulgating

the third update to the SW-846 methods on June 13, 1997 (62 FR 32452).

Method 1664 is approved as ``guidance'' under the RCRA programs (see

Section III.B.). Other methods may be used under the conditions stated

in the RCRA regulations (see 40 CFR part 268).

The regulatory background for development of effluent guidelines

and standards is given in proposed and final rules for these guidelines

and standards. See, for example, Section III of the final rule for the

Coastal Subcategory of Oil and Gas Extraction promulgated on December

16, 1996 (61 FR 66086).

The background and history of applicability of EPA's Stratospheric

Ozone Protection Program to analytical methods requiring use of CFCs in

EPA's CWA programs was given in a proposal for an earlier EPA method

for determination of oil and grease on July 3, 1991 (56 FR 30519). The

Montreal Protocol and Section 604 of the Clean Air Act Amendments of

1990 impose limits on the production and consumption of certain ozone-

depleting substances including CFC-113 (see 40 CFR part 82).

B. Data Gathering

Data gathered to support today's final rule were Freon replacement

studies and other data gathered prior to proposal, data collected in

EPA's Water Pollution (WP) Performance Evaluation (PE) Study 038, and

data received from commenters.

1. EPA's Freon Replacement Studies

EPA summarized details of EPA studies that support today's final

rule at proposal (see 61 FR 1730) and presented information in reports

of EPA's Phase I Freon Replacement Study (EPA-821-R-93-011), Phase II

Freon Replacement Study (EPA-820-R-95-003), and Method Validation Study

(821-R-95-036). These reports are included in the Water Docket for the

proposed rule.

2. Water Pollution Performance Evaluation Data

EPA has collected data on the performance of laboratories

conducting routine analyses of wastewaters through water pollution

performance evaluation (PE) studies. For water pollution PE study 038

conducted in late calendar year 1997, EPA accepted data from

laboratories determining oil and grease using either CFC-113 or n-

hexane. The results of this study are summarized in Table 1 and show

that, for this study, CFC-113 and n-hexane extracted identical average

amounts of oil and grease.

Table 1.--Results of Performance Evaluation Study 038 for Determination

of Oil and Grease

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Number

Solvent of Mean (mg/ Standard

samples L) deviation

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CFC-113.................................. 1,101 11.4 2.1

n-hexane................................. 353 11.4 2.4

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[[Page 26317]]

3. Data Received From Commenters

As detailed in other sections of this preamble and in the detailed

comments and responses included in the Docket, EPA utilized data

submitted in response to the proposal of Method 1664 for improvements

included in the version of Method 1664 being approved for use today.

All comments are included in the Water Docket.

III. Explanation of Today's Action

Today's final rule approves Method 1664 determination of n-hexane

extractable material (HEM; oil and grease) and silica-gel treated n-

hexane extractable material (SGT-HEM; non-polar material) in EPA's CWA

and RCRA programs. Today's action has an economic benefit to regulated

entities measuring oil and grease and non-polar material (NPM) in that

the cost of CFC-113 is considerably greater than the cost of n-hexane

as a result of the production phase-out of CFCs and increased tariffs

on their use. The costs for CFCs being phased out can be expected to

rise as production ceases and tariffs increase further. Because n-

hexane is a product of oil refining on a large scale, the impact of the

additional demand for n-hexane is expected to be insignificant. As

pointed out by commenters, however, laboratory use of CFC-113 was small

in comparison to other uses. Indeed, many commenters claimed that

because of safety problems and the disparity in results produced by use

of CFC-113 vs. n-hexane, use of CFC-113 should be continued

indefinitely. Based on these comments and an extension of the

laboratory use exemption to 2005, EPA has decided to allow continued

use of methods that use CFC-113 and to approve use of Method 1664 for

those regulated entities that desire to switch to use of n-hexane.

A. Application of Method 1664 in EPA's Clean Water Act Programs

1. General Use

Method 1664 will be used in EPA's wastewater program for regulation

development, permit applications, and compliance monitoring. More than

600 industrial subcategories are regulated under Clean Water Act

pollution control programs (see the rules for these industrial

subcategories at 40 CFR parts 400-510). Nearly all of these regulations

contain nationwide effluent guidelines and standards limiting the

amount of oil and grease that may be discharged from facilities in

these subcategories. EPA estimates that more that 10,000 National

Pollutant Discharge Elimination System (NPDES) permits contain a limit

for oil and grease, potentially necessitating an estimated minimum of

25,000 measurements annually.

2. Search for Other Uses of CFCs in Clean Water Act Program

EPA performed computerized string searches of 40 CFR parts 100-149,

and of Subchapter N, ``Effluent Guidelines and Standards,'' at 40 CFR

parts 400-500 for ``TPH'', ``Freon-113'', ``CFC-113'',

``chlorofluoro'', ``413.1'', and related terms in an attempt to locate

references to CFC-113 and Method 413.1 for determination of oil and

grease. EPA could find no references other than in 40 CFR part 136 and

to the procedure for petroleum hydrocarbons in the Coil Coating

standards at 40 CFR 465.03(c). EPA intends to consider allowing use of

Method 1664 through subsequent rulemaking for the Coil Coating Point

Source Category.

B. Application of Method 1664 in Resource Conservation and Recovery Act

Program

Analytical methods found acceptable for testing under Subtitle C of

RCRA are contained in OSW publication SW-846, Test Methods for

Evaluating Solid Waste, Physical/Chemical Methods. Use of some of these

methods is required by some of the hazardous waste regulations under

Subtitle C of RCRA. In other situations, SW-846 functions as a guidance

document setting forth acceptable, although not required, methods to be

implemented by the user, as appropriate, in satisfying RCRA-related

sampling and analysis requirements. As of Update III to SW-846, the two

SW-846 methods for determination of oil and grease have been Method

9070 for waters and aqueous wastes, and Method 9071A for solid and

semi-solid material such as soil, sediment, and sludge. Method 9070 is

virtually identical to presently approved CWA methods for determination

of oil and grease. Method 9071A employs drying of the sample with

magnesium sulfate and Soxhlet extraction with CFC-113 for the

determination. These methods are not specifically required by any RCRA

regulation, although they can be required as part of a hazardous waste

de-listing demonstration.

In today's final rule, SW-846 is being amended further to delete

Method 9070 and to include revised Method 9071B as Update IIIA.

Specifically, Method 9071B addresses the use of n-hexane instead of

CFC-113 as the extraction solvent, in a manner consistent with the use

of n-hexane in Method 1664. In addition, in place of Method 9070, which

uses CFC-113 as the extraction solvent in the testing of waters and

aqueous wastes, the Agency is incorporating by reference Method 1664 in

the RCRA regulations. As part of Update IIIA, SW-846 refers the

regulated community to Method 1664 for testing previously conducted

using Method 9070.

EPA compared results of Soxhlet extraction of solids and sludges

with various solvents, including CFC-113 and n-hexane, in the Phase I

Freon Replacement Study (EPA-821-R-93-011). Results of this study

showed that, as with testing of waters which was described in the Phase

I study report that was included in the Docket at proposal, CFC-113 and

n-hexane extract different amounts of material. However, for petroleum-

based samples, the amount of material extracted by CFC-113 and n-hexane

was not significantly different. This is the same conclusion that was

reached regarding extraction of waters. As a result, and for the other

reasons allowing use of Method 1664 detailed at proposal and in other

sections of this preamble as supported by the information contained in

the Water Docket, EPA believes that changes to SW-846 as a result of

Update IIIA, i.e., the use of Method 1664 in place of Method 9070 and

the addition of Method 9071B to SW-846, are appropriate and logical

outgrowths of the Agency's efforts to reduce dependency on the use of

CFCs.

C. Use of Solid-Phase Extraction (SPE)

SPE uses a cartridge or disk for removal of the oil and grease from

the sample. A detailed description of the SPE technique was provided at

proposal (61 FR 1730). Even prior to proposal of Method 1664, vendors

of SPE devices had requested that SPE be an allowed technique in the

Method. Proposed Method 1664 allowed use of SPE, but required a

demonstration that SPE produced results equivalent to results produced

by the separatory funnel liquid-liquid extraction technique (LLE)

written in Method 1664. Vendors and other commenters objected to this

requirement, claiming that SPE provided sufficient advantages in

solvent reduction, reduced analysis time, reduced emulsion formation,

and other advantages so that its use should be allowed without prior

demonstration of equivalency. EPA discussed the issue extensively at

proposal and in public workshops and meetings, and specifically

solicited data demonstrating equivalency of results produced by SPE and

LLE. Data received were mixed, with some data demonstrating that

results produced are equivalent and other data demonstrating that

results produced are significantly different. EPA reopened the comment

period (61

[[Page 26318]]

FR 26149) to allow submission of further data, and EPA provided a

notice of availability (62 FR 51621) of these and other data so that

EPA could consider these data for today's final rule.

Discussions of the detailed issues on SPE are summarized in Section

VI of this preamble and given in the detailed comments and responses

included in the Docket. Based on comments received and supporting data,

EPA is allowing the use of SPE in the version of Method 1664 being

approved today without a prior demonstration of equivalency. However,

EPA has added a note at the beginning of the extraction procedure

(Section 11.3) in Method 1664 to indicate that it is the discharger/

generator's responsibility to assure that the results produced are

equivalent. If there is doubt about this equivalency, liquid/liquid

extraction is definitive for the measurement.

EPA also acknowledges that if a Region, State, or other permitting

authority has concerns about the difference in results produced by SPE

and LLE, that authority may specify in the permit the use of one of the

two techniques.

D. Differences in Results Produced by CFC-113 and n-Hexane and

Determinations of Compliance

Since EPA announced results of the Phase I Freon Replacement Study

in 1993, several commenters expressed concerns about the impact of

differences resulting from substitution of CFC-113 with n-hexane on

determinations of compliance under the NPDES program and pretreatment

programs. EPA discussed this issue at proposal (61 FR 1730; January 23,

1996), and discussed the issue in workshops, conferences, and seminars

between proposal and development of today's final rule.

After proposal, EPA received numerous requests from States and EPA

Regions for guidance on implementation of Method 1664. On July 9, 1996,

EPA issued guidance to Pretreatment Coordinators and Regional NPDES

Contacts. A copy of the memorandum is included in the Docket for

today's final rule. In part, this memorandum states the following:

``EPA acknowledges that, due to the diverse nature of

discharges, there may be instances in which n-hexane will extract an

amount of oil and grease greater or less than the amount extracted

by Freon-113. If these instances affect compliance, the permitting

authority may wish to consider establishing a conversion factor,

multiplier, or divisor to account for these differences in the

permit. EPA emphasizes that few, if any, instances will likely be

found in which the differences affect compliance and, therefore,

urges direct substitution of the presently approved methods with

Method 1664 when the date of substitution is announced in the

Federal Register.''

By today's final rule, EPA still believes that the approach

outlined in the memorandum appropriately accommodates any significant

discrepancies that could arise in determining compliance with

limitations or standards for oil and grease using the new method. Based

on the results from the Freon Replacement Studies, EPA found that, on

average, n-hexane extracted approximately 96% of the material extracted

using CFC-113. Therefore, while there may be some effluent matrices

where n-hexane will extract more material than CFC-113, on the whole,

most dischargers would have little risk of a determination of non-

compliance with existing limits. The slightly smaller amount of oil and

grease extracted by n-hexane (96% versus 100% by CFC-113) is not

statistically significant because errors in oil and grease measurement

are in the order of 10 percent relative standard deviation. A coarse

estimate of 95% confidence limits around the 96% recovery by n-hexane

is 96 plus or minus 20%, or the true difference lies somewhere between

76-116%. This encompasses 100% or no difference. Given the lack of

significance of the 4% difference, the measurement error that would be

encountered in the side-by-side comparison (estimated at 10% for each

measurement), the potentially significant cost of a side-by-side

comparison with each discharge and the low anticipated likelihood that

a significant difference would be found (based on EPA's studies), EPA

does not recommend a side-by-side comparison for each discharge.

Instead, EPA continues to recommend a direct replacement of the

approved Freon methods with Method 1664.

However, to accommodate regulated entities concerned about

differences produced, EPA is not withdrawing approved use of methods

employing CFC-113, a Class I ozone depleting substance. If a

discharger/industrial user has concerns about measuring oil and grease,

the discharger/industrial user may choose to perform a side-by-side

comparison of Method 1664 and any of the approved methods that it

previously used to measure compliance with the limitation or standard

for oil and grease. For the side-by-side comparison, EPA suggests, at a

minimum, analysis of three replicates of each sample by each method on

any seven days over a minimum 30-day period, for a total of 42 analyses

(21 by the previously used method and 21 by Method 1664). For this

side-by-side comparison the laboratory should use the LLE procedure

(not the optional SPE procedure) in Method 1664 because of the possible

confounding of results that could occur when two variables (SPE and the

solvent) are changed simultaneously. EPA suggests that all six results

associated with any result less than the minimum level ( The hexadecane/stearic acid standard solution has been

diluted by a factor of 2 and twice as much standard

[[Page 26320]]

is spiked to avoid reported precipitation problems with this standard.

Instructions have been amplified to rinse all glassware

surfaces with solvent after transfer of sample or standards from one

container to another to avoid reported problems that sample and

standards cannot be recovered quantitatively.

Performance data from EPA's validation study have been

added to Section 13.

A procedure was added for drying the sample to constant

weight. The procedure was provided by the American Petroleum Institute.

The section on safety was expanded to address in greater

detail personnel monitoring and the hazards of handling n-hexane.

A requirement was added that certain pieces of equipment

such as the hot plate, centrifuge, and fume hood be specified as

explosion proof.

The QC acceptance criteria have been widened based on

EPA's validation study.

A procedure for collecting four grab samples over the

course of a day for laboratory compositing was added.

The term ``discharge'' was defined to be consistent with

the words ``discharge'' and ``matrix type'' in EPA's Streamlining

Initiative proposed on March 28, 1997 (62 FR 14976).

A suggestion for back-extraction was added to aid in

removal of salt from extracts of produced water samples to address

concerns expressed by the American Petroleum Institute.

References to the solvent removal process were changed

from ``evaporation'' to ``distillation'' to indicate that the process

recovers the solvent. Similarly, the word ``waste'' was changed to

``distillate'' to preclude indications that the distillate may be

hazardous waste.

Use of a greater amount of silica gel is now allowed so

that greater amounts of polar material can be adsorbed in the SGT-HEM

procedure, and the ratio of amount of silica gel to the amount HEM has

been clarified.

The top-loading analytical balance and centrifuge are made

optional because they may not be needed.

A limit has been placed on the amount of spiking solution

that may be added to a sample for the matrix spike and matrix spike

duplicate. The purpose of adding this limit is to preclude adding large

amounts of acetone to the sample, thus possibly allowing the spiking

material to be dissolved in the aqueous phase and not recovered in the

extraction.

VI. Public Participation and Response to Comments

The Agency proposed Method 1664 for use on January 23, 1996 (61 FR

1730). The comment period at proposal closed on March 25, 1996. On May

24, 1996 (61 FR 26149), EPA reopened the comment period for the purpose

of accepting additional data and inviting comments. The reopened

comment period closed on July 23, 1996. EPA continued to receive data

and comments after the close of the reopened comment period. Because

EPA desired to use some of these data to support the information and

decisions in today's final rule, EPA issued a notice of data

availability and request for comment on October 2, 1997 (62 FR 51621).

The comment period on the notice closed on November 3, 1997.

In the proposal and for the reopened comment period, EPA solicited

data comparing various extraction solvents, data comparing use of SPE

with the LLE procedures in Method 1664, and comments on the other

operational aspects of Method 1664. EPA is pleased with the content and

nature of the comments received. Many contained analytical data and/or

constructive comments for improvement of the Method. As a result, EPA

has modified Method 1664, where appropriate, to respond to commenters'

suggestions. Significant comments received are summarized below, along

with EPA's response. To the extent practicable, the comments have been

categorized by subject. Detailed comments and their accompanying

responses are included in the Docket for today's final rule.

EPA thanks commenters for data and constructive suggestions and

believes that the version of Method 1664 being promulgated today will

provide reliable data for compliance monitoring.

A. Regulatory Issues

Comment: Oil and grease is not a viable parameter for National

Pollutant Discharge Elimination System (NPDES) compliance and there is

no objectivity in permitting with an empirically based method.

Response: Oil and grease is a conventional pollutant designated

pursuant to section 304(a)(4) of the Federal Water Pollution Control

Act (FWPCA) and codified at 40 CFR 401.16, and therefore must be

monitored for NPDES compliance under an effluent guideline or when

deemed appropriate by a regulatory authority.

Comment: As with Method 413.1, Method 1664 measures non-oil and

grease substances such as surfactants, soaps, and emulsifiers that will

unduly subject dischargers to continual permitting and compliance

difficulties.

Response: EPA recognizes that it may be inappropriate to include

certain substances in the determination of oil and grease. However,

discharges of pollutants, including surfactants, soaps, emulsifiers,

and other substances, is prohibited under the Clean Water Act unless in

compliance with an NPDES permit. EPA has provided the SGT-HEM (NPM)

procedure in Method 1664 to allow development of effluent guidelines

and in permitting situations for those instances in which removal of

these substances is appropriate, and to allow a regulatory authority to

specify measurement of SGT-HEM for compliance monitoring.

B. Health and Safety Concerns

Comment: n-Hexane is a safety hazard compared to CFC-113. n-Hexane

has a flash point of -23 deg.C (-9 deg.F), has explosive limits in air

in the range of 1.2-6.9 percent, and poses a serious fire risk when

heated or exposed to flame. There are multiple ignition sources in a

laboratory, including Bunsen burners and high temperature furnaces.

Method 1664 should be performed in an explosion-proof hood.

Response: EPA agrees that n-hexane is comparatively more hazardous

than CFC-113. Proposed EPA Method 1664 contained explicit precautions

concerning the handling of n-hexane and the recommendation that

material safety data sheets (MSDSs) be made available to laboratory

personnel. EPA also included references to information on laboratory

safety. EPA has expanded and re-emphasized these precautions in the

version of Method 1664 being approved today.

Comment: EPA needs to modify Method 1664 to give information on the

toxicity of n-hexane and on safety precautions required for safe

handling and storage. n-Hexane is a known neurotoxin.

Response: EPA has expanded the section on safety and the health

effects of n-hexane in the version of Method 1664 being approved for

use in today's final rule.

C. Economic Concerns

Comment: Method 1664 is more complicated and more labor intensive,

requires a greater analysis time, and will be more expensive to

practice.

Response: EPA agrees that Method 1664 will require a somewhat

longer analysis time because of the increase in time required for

extraction, n-hexane evaporation, and QC. However, regulated entities

and their laboratories will benefit from lower costs for the n-

[[Page 26321]]

hexane extraction solvent because CFC-113 is becoming difficult to

obtain as well as expensive. EPA believes that any cost increases will

be small and that the benefit outweighs the cost because it will reduce

the use of ozone-depleting chlorofluorocarbons, thus protecting the

Earth's ozone layer. Further, EPA is not withdrawing allowed use of

methods that employ CFCs. If a regulated entity desires to continue use

of a Freon-based method for economic reasons, the entity may continue

to use that method.

Comment: Disadvantages of using n-hexane include: the lower density

that causes n-hexane to float on the water sample making extraction

more difficult and time consuming than with CFC-113 that sinks; the

higher water solubility of n-hexane requiring more drying agent or use

of phase-separation paper; the greater tendency to form emulsions than

CFC-113; and the higher boiling point of n-hexane requiring an

evaporation time longer than 30 minutes at 85 deg.C.

Response: EPA pointed out the disadvantages of the use of n-hexane,

including some of the disadvantages above, when EPA Method 1664 was

proposed. None of these disadvantages precludes n-hexane from being

used as the extraction solvent in Method 1664. Indeed, and as pointed

out by a commenter, n-hexane was used as the extraction solvent for oil

and grease prior to the advent of CFC-113 in laboratories that were,

undoubtedly, less well equipped to handle toxic and flammable

substances. Tests performed to date using n-hexane in Method 1664

reveal that none of the disadvantages prevent use of this solvent. EPA

agrees that the techniques in Method 1664 and the other methods that

the Agency publishes must be performed carefully in order to ensure

reliable results.

D. Solid-phase Extraction (SPE)

1. Comments Supporting Use of SPE

Comment: Many commenters stated that SPE should be a standard

procedure in Method 1664. Some suggested that SPE should be the

standard procedure and that LLE should be optional.

Response: EPA believes that LLE should remain the standard

procedure because, except for a change necessitated by the change from

CFC-113 to n-hexane, the procedures in Method 1664 are virtually

identical to procedures in existing methods, the equipment used is the

same, and because n-hexane with LLE produced results closest to results

produced by CFC-113 in EPA's Freon replacement studies.

Comment: Method 1664, as proposed, requires a demonstration of

equivalency of SPE and other method modifications on each and every

discharge. This requirement is a barrier in the way of laboratories

that receive samples from different sources and a barrier to use of

innovative technologies on a national level. EPA should allow use of

SPE and other modifications without this demonstration or should allow

nationwide application to the matrices for which applicability has been

demonstrated.

Response: EPA has allowed use of SPE without a required

demonstration of equivalency in the version of Method 1664 approved

today. However, EPA has added a note to Method 1664 that it is the

discharger's responsibility to assure that results produced are

equivalent. Nearly all permits were developed using LLE and CFC-113.

Method 1664 allows the use of SPE. However, two things change when SPE

is used: the solvent and the extraction technique. EPA is concerned

that this double change may cause a discharger to violate a permit

limit simply because the results obtained are not equivalent (i.e., SPE

may produce different results). Therefore, if there is any doubt about

SPE with n-hexane producing results significantly different from

results produced by LLE with n-hexane, dischargers and laboratories

should perform a side-by-side test to demonstrate that equivalent

results are produced.

2. Comments Expressing Concerns about the Use of SPE

Comment: Results produced by SPE and LLE are not equivalent.

Comparisons of results produced by LLE, SPE cartridge, and SPE disk in

our laboratory showed statistically significant differences on 3 of 4

discharges tested. Further, infrared (IR) spectra and gas

chromatography with a flame ionization detector (GC/FID) demonstrate

that different material is being extracted by each of the extraction

techniques.

Response: EPA has seen data that demonstrate differences and other

data that demonstrate equivalence in results produced by LLE and SPE,

and EPA has decided, based on comments and data received, that SPE

should be allowed in the version of Method 1664 approved today.

However, EPA has added the note to Method 1664 that, although SPE may

be used, it is the discharger/industrial user's responsibility to

assure that results produced using SPE are equivalent to results

produced using liquid-liquid extraction (LLE).

E. Grace Period for CFC-113

Comments: Six months is too long to allow existing stocks of CFC-

113 to be used up. Use should cease immediately. Use of CFC-113 should

be allowed until existing stocks are used up, regardless of how long it

takes. Six months is the correct period for stocks of CFC-113 to be

used up. The date of the changeover should be the first day of the

month to simplify compliance monitoring. NPDES permittees should be

given 36 months to determine if they can be compliant with the new

method. Use of Method 1664 should not be required for at least one year

after the method is approved. Method 413.1 should not be withdrawn for

at least two years after the effective date of Method 1664. The

additional time should be used to generate data and establish new

permit limits as needed.

Response: The comments on this issue are diverse but most

commenters supported a grace period for switching to Method 1664. Based

on comments received, on EPA's desire to allow existing stocks of CFC-

113 to be used up, on EPA's desire not to mandate the use of Method

1664 if a CFC-based method is specified in the permit, and on extension

of the laboratory exemption for use of CFCs until 2005, approved

methods employing CFC-113 remain approved.

F. Use of Silica-gel Treated, n-Hexane Extractable Material (SGT-HEM)

Procedure

Comment: Hexane-extractable material and silica-gel treated, n-

hexane-extractable material (SGT-HEM) should be better defined.

Response: HEM and SGT-HEM are method-defined analytes, i.e., they

are defined by the procedure used to measure them, in this case Method

1664.

Comment: When will it be necessary to perform the (SGT-HEM)

procedure for total petroleum hydrocarbons (TPH)?

Response: Monitoring of TPH (now SGT-HEM or ``non-polar material;''

NPM) is presently required in the monitoring and reporting requirements

under the Coil Coating point source category at 40 CFR 465.03(c). EPA

intends to consider allowing use of Method 1664 through subsequent

rulemaking for that category and in other categorical effluent

guidelines. In today's rulemaking, EPA is also making the SGT-HEM

procedure available to permitting authorities for instances in which

only the non-polar material component of oil and grease needs to be

monitored. The SGT-HEM procedure allows monitoring of these substances.

[[Page 26322]]

G. Detection and Quantitation

Comment: Many commenters provided MDL data.

Response: The MDLs that the commenters provided and the resulting

MLs are consistent with the range of MDLs and MLs that EPA obtained in

the Agency's MDL studies. The average (mean) of these MDLs is 2.1 mg/L

and the median is 1.4 mg/L. The pooled single-operator MDL, using the

34 MDLs listed above plus the 5 MDLs EPA reported at proposal (61 FR

1736-1737, January 23, 1996), and calculated as the root-mean-square of

the standard deviations multiplied by a student's t value of 2.33 for

234 degrees of freedom, is 2.0 mg/L. These MDLs are all equal or close

to the value of 1.4 mg/L that EPA proposed and support an ML in the

range of 5--10 mg/L. Based on EPA's data and data provided by

commenters, EPA has retained the MDL at 1.4 mg/L and the ML at 5 mg/L

for both HEM and for SGT-HEM in the version of Method 1664 approved for

use in today's final rule.

Comment: Several commenters state that estimates of detection and

quantitation in Method 1664 are one or more of the following: they

cannot be achieved; are scientifically unsound; are neither realistic

nor reproducible; are flawed; were developed in an arbitrary and

capricious manner; use an inappropriate multiplication factor; are

based on spikes into reagent water instead of wastewaters; do not

consider effluent characteristics; were developed using analytical

standards; are based on a protocol that has never been subjected to

peer review and public comment; are not representative of expected

performance by qualified laboratories; represent performance of

``expert'' or ``research-grade'' laboratories; are not a statistical

predictor of laboratory performance; and were not validated on an

interlaboratory basis.

Response: EPA disagrees that the MDLs and MLs in Method 1664 were

developed inappropriately. EPA has received nearly identical sets of

comments from many of the same industry organizations on many recent

methods that EPA has proposed for use in its wastewater programs. (See,

for examples, responses to comments in the final rules promulgating use

of Method 1613 (57 FR 31805, 62 FR 48394) and use of Method 1650 and

1653 (63 FR 18503 )). EPA responds to these comments briefly and

collectively here with the same responses provided in those comments

and responses. Responses to some of the individual issues raised by

commenters are further amplified in other responses.

EPA has used the MDL successfully for estimating the lowest level

at which a substance can be detected since 1984. The MDL procedure was

subjected to peer review when the original article on the MDL was

published in Environmental Science and Technology in 1981 (ES&T 15,

1426-1435). The MDL procedure is subjected to public comment with every

MDL that EPA publishes in test methods proposed in the Federal Register

for use in EPA programs. EPA believes that the MDL procedure is viable

and provides an estimate of the lowest concentration of an analyte that

can be detected. For Method 1664, EPA did not select the lowest or

highest MDL from the five MDL studies that EPA performed prior to

proposal; rather, the Agency selected the central value of the five

MDLs determined, and provided the rationale for this selection process

at proposal (61 FR 1736--1737). This MDL is supported by MDLs in

comments received from laboratories that do not necessarily represent

``expert'' or ``research-grade'' laboratories.

With respect to the comment on lack of interlaboratory validation

of the MDL and ML, EPA performed an interlaboratory validation of

Method 1664 at levels consistent with historical interlaboratory method

validation studies performed by EPA, ASTM, AOAC-International, the

organizations that publish Standard Methods for the Examination of

Water and Wastewater (Standard Methods), and by other organizations

that validate methods. EPA and all of these organizations have not

historically performed interlaboratory studies to estimate detection

and quantitation limits. EPA used data from multiple single laboratory

studies instead to support the MDL and ML. Commenters making this

comment did not perform interlaboratory detection limit studies to

demonstrate that EPA's estimates are flawed.

EPA will continue to examine the issues of detection and

quantitation. The Agency initiated a study recently to evaluate these

concepts and plans to involve the public on these issues.

H. Matrix Effects

Comment: Method 1664 produces severe emulsion problems. These

emulsions were not formed when using Method 413.1. Breaking these

emulsions requires additional handling, increasing the potential for

inaccuracy. Bad emulsions can never be completely broken.

Response: Section 11.3.5 of Method 1664 contains the following

suggestions for overcoming emulsions: ``stirring, filtration through

glass wool, use of solvent phase separation paper, centrifugation, use

of an ultrasonic bath with ice, addition of NaCl, or other physical

methods. Alternatively, solid-phase, continuous, or other extraction

techniques may be used to prevent emulsion formation, provided that the

requirements in Section 9.1.2 are met.''

Comment: EPA must recognize the problems that the high salt content

of produced water creates.

Response: A small amount of water may be soluble in the n-hexane

used as the extracting solvent in Method 1664. In turn, a small amount

of salt may be dissolved in the hexane/water mixture. However, after

extraction, the solution is passed through granular, anhydrous sodium

sulfate to remove all traces of water. In turn, this process should

remove the residual salt. If not, the extract can be back-extracted

with reagent water to remove all traces of residual salt. After back-

extraction, the solution can be again filtered through sodium sulfate

to remove residual traces of water.

I. Method Modifications

Comment: We endorse the concept of performance-based methods to

allow for advances in technology and reductions in the cost of analyses

and encourage EPA to continue to move in this direction.

Response: In response to this and similar requests, EPA proposed an

implementation of a performance-based measurement system (PBMS) in the

Streamlining Initiative on March 28, 1997 (62 FR 14976) and solicited

comment on an alternative PBMS approach on October 6, 1997 (62 FR

52098). The Streamlining Initiative allows modification of a reference

method so long as equivalent or superior performance can be

demonstrated. The alternative PBMS approach allows modification of a

method or use of any other method based on performance demonstrated

equal or superior to a reference method (as with Streamlining) or to a

set of data quality objectives (DQOs). The alternative PBMS approach

does not allow modification of methods for method-defined analytes,

such as oil and grease, because the analyte being measured is defined

by the method used. EPA expects to make a final determination on PBMS

for method-defined analytes in the future, as the Agency gains

experience in dealing with any potential issues, and as comments from

stakeholders on these and other PBMS approaches are received.

Comment: Please clarify the ``specific discharge'' as it relates to

``the

[[Page 26323]]

discharger must demonstrate that the modified method produces results

equivalent to those produced by Method 1664 for each specific

discharge.''

Response: Specific discharge is equivalent to ``matrix type''

defined in the regulatory language proposed in EPA's Streamlining

Initiative (62 FR 14994, March 28, 1997) and means a sample medium with

common characteristics across a given industrial subcategory. Examples

include: C-stage effluents from chlorine bleach mills in the Pulp,

Paper, and Paperboard industrial category; effluent from the continuous

casting subcategory of the Iron and Steel industrial category; publicly

owned treatment work (POTW) sludge; and in-process streams in the

Atlantic and Gulf Coast Hand-shucked Oyster Processing subcategory. For

further explanation of this definition, please see the proposed

Streamlining Initiative.

Comment: Declaring that performance-based modifications can be made

perpetuates the incorrect notion that empirically determined analytes

are not affected when the practice and manner of determining them

changes. When a protocol defines an analyte, deviation from that

protocol should not be permitted.

Response: EPA agrees with this comment, but only in part. The

commenter presumably would not argue that the result of the analysis

will be affected by the size of the funnel that contains the sodium

sulfate used for removal of residual water. In allowing modification of

Method 1664, the Agency identified and distinguished changes that would

not adversely affect method performance (and analyte measurement) from

changes that would. As a result, laboratories may modify extraction and

concentration procedures, but not allow changes to the determinative

technique (gravimetry), provided that equivalent or superior

performance of the modification is demonstrated on a reference matrix

(reagent water) and on the discharge to which the modification will be

applied. EPA believes that this middle ground is the best that can be

done to allow modifications and protect the reliability of the data

produced with a modification.

J. Matrix Spike/Matrix Spike Duplicate (MS/MSD)

Comment: The relative percent difference criteria for the MS/MSD

are too stringent and do not account for natural variations in grab

samples.

Response: EPA changed the requirement for an MSD to a suggestion

but believes that the MS/MSD will work with flowing streams. In the

Phase I and Phase II studies that EPA performed in support of

development of EPA Method 1664, flowing streams were split using the

procedures given in the note in Section 8.2 of EPA Method 1664 and

provided reliable replicates for testing. For the Phase II study, the

discharge streams sampled were adjusted to provide background

concentrations of oil and grease. No difficulty was encountered

recovering spikes into these samples or achieving precise results with

replicates.

Comment: The requirement for an MS/MSD at a frequency of 10 percent

and per sample batch is excessive and unnecessarily burdensome.

Response: EPA agrees that this requirement is unnecessarily

restrictive and has reduced the frequency of the MS to 5 percent and

has changed the requirement for the MSD to a suggestion.

K. Precision and Recovery

Comment: The precision and recovery criteria are unrealistic and

will not be achievable by most laboratories.

Response: EPA believes that the difficulties in achieving the

precision and recovery criteria in EPA Method 1664 are attributable to

precipitation of hexadecane and stearic acid from the standard solution

and to failure of laboratories to adequately rinse all traces of the

standard from glassware. EPA has modified the version of EPA Method

1664 being approved today to halve the concentration of hexadecane and

stearic acid in the standard solution and require spiking twice as

much. EPA also has noted that the sample container and other surfaces

that the sample contacts must be carefully rinsed with solvent to

effect quantitative transfer of oil and grease and NPM from the sample

to the extract.

L. Differences in Results Produced by n-Hexane and CFC-113

Comment: Changing to n-hexane may cause dischargers to exceed

permit limitations because the new method may result in higher oil and

grease values. EPA should provide guidance to permit writers and

enforcement staff for dealing with this positive bias.

Response: EPA believes that the possibility that the change in

solvent will result in non-compliance is minimal based on the results

from the Freon Replacement Studies conducted prior to proposal. If a

discharger believes that the change to n-hexane will cause false

readings of noncompliance, the discharger should discuss the situation

with the permitting authority. EPA cautions that to demonstrate that

the noncompliance is the result of the change to n-hexane alone,

comparative data must be obtained using CFC-113 and n-hexane on a

sufficient number of real-world samples and the difference must be

statistically significant. For guidance in this demonstration, the

commenter is referred to Section III.D. of this preamble and the

statistical tests for significance in reports for EPA's Phase I and

Phase II Freon Replacement studies that were included in the Docket at

proposal.

Comment: EPA's proposal to replace previously approved methods with

EPA Method 1664 is arbitrary and capricious and will render obsolete

all effluent limitation guidelines and permit limitations for oil and

grease that were based on the Freon method.

Response: First, EPA is not withdrawing the previously approved

methods in today's rulemaking. Second, as discussed earlier, EPA

believes that the use of n-hexane will generally not affect the oil and

grease results significantly and, therefore, the possibility that the

change in solvent will result in non-compliance is minimal. Third, in

studies comparing different extraction solvents for measurement of oil

and grease, and in the proposal of Method 1664, EPA acknowledged and

again acknowledges that no two extraction solvents will produce exactly

the same results for a method-defined analyte such as oil and grease.

By providing for recalculation of compliance targets based on side-by-

side data, EPA believes that the Agency has taken reasonable steps to

minimize the impact of using Method 1664 rather than the Freon method

in those cases when the difference in results may cause a non-

compliance with a permit limitation.

Comment: Two commenters stated that samples collected and analyzed

under the previously approved methods are used to determine a

discharger's compliance with local and Federal categorical limits and

that it may be appropriate for EPA to re-evaluate all of these limits.

Response: There are more than 600 industrial subcategories and

nearly all contain a limit for oil and grease. Extensive time and

expense would be required for re-evaluation of all limits in all of

these subcategories. EPA conducted side-by-side evaluations on 39

facilities in 24 industrial categories in the Phase I Freon Replacement

Study and on 25 facilities in 16 industrial categories in the Phase II

study. Based on the results from these studies, EPA does not believe

that a re-evaluation of the categorical limits is neccesary at this

[[Page 26324]]

time and supports the use of Method 1664 instead of the Freon method to

determine compliance with the categorical limits. However, EPA

periodically re-evaluates categorical effluent limitations and plans to

use Method 1664 to support this effort. Until each categorical standard

is re-evaluated, EPA has decided to allowed the continued use of the

CFC-113 methods. However, because compliance targets can be adjusted on

a case-by-case basis, EPA encourages the replacement of CFC-113 with n-

hexane consistent with EPA's efforts to reduce dependency on the use of

chlorofluorocarbons.

M. Method Validation and QC Acceptance Criteria

Comment: EPA Method 1664 was not validated properly because

inappropriate sample concentrations of 57 and 170 mg/L were used in the

Twin Cities Round-robin study (TCRR).

Response: EPA disagrees that EPA Method 1664 was validated

improperly. Laboratories that participated in the TCRR study validated

the Method at concentrations of 40 mg/L for HEM and 20 mg/L for NPM in

the initial precision and recovery (IPR) and ongoing precision and

recovery (OPR) tests, and at concentrations of 57 and 170 mg/L for

``real-world'' samples from a petroleum and non-petroleum source,

respectively. It is customary to validate analytical methods at

concentrations in the middle of the concentration range to avoid

attempting to compare results for which HEM is not detected and to

allow lowered recoveries to be measured reliably, should lowered

recoveries occur. For additional information on this issue, see the

response to comments on the detection/quantitation issue.

N. Quality Control

Comment: The QC specified in Section 9 is excessive, especially

for every discharge point.

Response: As stated elsewhere in these comment responses, the

frequency requirement for an MSD has been changed to a suggestion and

the frequency of the MS and OPR have been reduced to a minimum of 5

percent. EPA does not believe that a requirement to assess the

precision and recovery on every 20th sample is excessive.

O. Sample Collection and Preservation

Comment: EPA should add a compositing procedure to EPA Method

1664. Samples can be composited in the laboratory by collecting

individual 250-mL samples over the course of a day, pouring each 250-mL

sample into the separatory funnel, rinsing each of the four bottles

(and caps) sequentially with 30 mL of n-hexane, and using the 30 mL of

n-hexane for the extraction.

Response: EPA has added the above compositing procedure to EPA

Method 1664.

Comment: Change the temperature requirement to 4 2

deg.C with the note that a lower storage temperature may be used so

long as the sample is not frozen.

Response: EPA chose a temperature range of 0-4 deg.C to be

consistent with holding time study data and to allow storage at 0

deg.C.

P. Miscellaneous Issues

Comment: The frequency of verification of balance calibration is

excessive. One commenter suggests verification before and after every

20 samples. Another commenter suggests verification before and after

daily measurements. A third commenter suggests that calibration

verification is unnecessary. A fourth commenter suggests monthly

verification.

Response: Calibration is verified prior to the first batch,

between batches, and after the last batch. EPA does not believe that

this is excessive. (An analytical batch is between 4 and 23

measurements.)

Comment: Method ruggedness has not been established, method

validity has not been confirmed on a wide range of sample matrices, and

the method is still empirical. The method needs further review and

validation on real-world samples.

Response: Based on EPA's Phase II and method validation studies,

and data supplied by commenters, EPA believes that Method 1664 has been

adequately validated and is sufficiently rugged for its intended use.

Method 1664 will always be empirical because oil and grease and NPM are

method-defined analytes.

Comment: The flask used for collection of distillate should be

referred to as a ``distillate collection flask'' rather than a ``waste

collection flask'' because the word ``waste'' can imply hazardous

waste.

Response: EPA agrees and has changed ``waste collection flask'' to

``distillate collection flask''.

Comment: Method 1664 requires that a smaller sample volume should

be extracted when a sample contains >1000 mg/L of oil and grease.

Should the smaller volume be diluted to one liter for extraction, or

should the smaller volume be extracted without dilution?

Response: The smaller volume should be diluted to one liter so

that changes to the Method are minimized. EPA has clarified this

dilution in Method 1664.

Comment: The higher boiling point of n-hexane will cause loss of

the more volatile constituents of oil and grease and therefore produce

greater variability in results.

Response: The average amount of oil and grease determined when

using n-hexane vs CFC-113 (96%), as detailed in other responses to

comments, may be attributable to loss of some volatile constituents.

Comment: What is to be the fate of Method 418.1? Method 418.1 and

SW-846 Method 9071 should not be used if continued use of Method 413.1

is disallowed.

Response: Method 418.1 is a CFC-113/infrared (IR) method for

determination of oil and grease. Although listed in Methods for

Chemical Analysis of Water and Wastes (EPA 600/4-79-020; NTIS PB84-

128677), Method 418.1 has not been approved for use at 40 CFR Part 136.

EPA plans a collaborative study with Canada for development of an IR

method that does not use CFC-113 and may propose an IR method depending

on the outcome of that study.

A solvent change from CFC-113 to n-hexane is being made in SW-846

Method 9071. Method 1664 replaces Method 9070 as the approved SW-846

method for determination of oil and grease in water, as detailed in

section III.B of this preamble.

Comment: EPA should include a thorough discussion of oil and

grease as a ``method-defined analyte'' in the final rule so that all

stakeholders clearly understand the results generated by Method 1664.

Response: EPA explained in section V of the proposal (61 FR 1737,

January 23, 1996) that determination of oil and grease is dependent on

how the measurement is made and cited examples of biochemical oxygen

demand and total suspended solids as other method-defined analytes.

Method-defined analytes are those analytes that are defined by the

procedure used to measure them. For oil and grease, the nature and the

amount of the substances extracted from complex wastewater discharges

and then measured is determined by the extracting solvent and

technique.

Comment: Many commenters suggested that Section 11.4.4 be changed

to require solvent evaporation and desiccation to constant weight. One

commenter suggested specific wording for this change. Another commenter

suggested a desiccation time of 24 hours.

Response: Section 11.4.4 has been changed to the specific wording

suggested by the first commenter but

[[Page 26325]]

has not been modified to include a 24-hour time requirement so that

constant weight achieved in a shorter time can be considered valid.

Comment: It should be EPA's responsibility to certify each

laboratory and not the responsibility of each and every company that

uses the laboratory.

Response: EPA does not certify laboratories under the Clean Water

Act and RCRA analytical programs. The States have this responsibility.

EPA is working with the States and other interested parties under the

auspices of the National Environmental Laboratory Accreditation Program

(NELAP) to accredit laboratory auditing organizations.

VII. Regulatory Requirements

A. Executive Order 12866

Under Executive Order 12866, (58 FR 51735 (October 4, 1993)) the

Agency must determine whether a regulatory action is ``significant''

and therefore subject to OMB review and the requirements of the

Executive Order. The Order defines ``significant regulatory action'' as

one that is likely to result in a rule that may: (1) Have an annual

effect on the economy of $100 million or more or adversely affect in a

material way the economy, a sector of the economy, productivity,

competition, jobs, the environment, public health or safety, or State,

local, or tribal governments or communities; (2) create a serious

inconsistency or otherwise interfere with an action taken or planned by

another agency; (3) materially alter the budgetary impact of

entitlements, grants, user fees, or loan programs or the rights and

obligations of recipients thereof; or (4) raise novel legal or policy

issues arising out of legal mandates, the President's priorities, or

the principles set forth in the Executive Order.''

It has been determined that this rule is not a ``significant

regulatory action'' under the terms of Executive Order 12866 and is

therefore not subject to OMB review.

B. Unfunded Mandates Reform Act

Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), Pub.

L. 104-4, establishes requirements for Federal agencies to assess the

effects of their regulatory actions on State, local, and tribal

governments and the private sector. Under section 202 of the UMRA, EPA

generally must prepare a written statement, including a cost-benefit

analysis, for proposed and final rules with ``Federal mandates'' that

may result in expenditures to State, local, and tribal governments, in

the aggregate, or to the private sector, of $100 million or more in any

one year. Before promulgating an EPA rule for which a written statement

is needed, section 205 of the UMRA generally requires EPA to identify

and consider a reasonable number of regulatory alternatives and adopt

the least costly, most cost-effective or least burdensome alternative

that achieves the objectives of the rule. The provisions of section 205

do not apply when they are inconsistent with applicable law. Moreover,

section 205 allows EPA to adopt an alternative other than the least

costly, most cost-effective or least burdensome alternative if the

Administrator publishes with the final rule an explanation why that

alternative was not adopted. Before EPA establishes any regulatory

requirements that may significantly or uniquely affect small

governments, including tribal governments, it must have developed under

section 203 of UMRA a small government agency plan. The plan must

provide for notifying potentially affected small governments, enabling

officials of affected small governments to have meaningful and timely

input in the development of EPA regulatory proposals with significant

Federal intergovernmental mandates, and informing, educating, and

advising small governments on compliance with the regulatory

requirements.

Today's final rule contains no Federal mandates (under the

regulatory provisions of Title II of UMRA) for State, local, or tribal

governments or the private sector. EPA has determined that this rule

contains no regulatory requirements that might significantly or

uniquely affect small governments. This rule would impose no

enforceable duty on any State, local or Tribal governments or the

private sector, nor would it significantly or uniquely affect them.

This rule makes available an additional testing procedure which would

merely standardize the procedures when testing is otherwise required by

a regulatory agency. Therefore, today's rule is not subject to the

requirements of sections 202, 203 and 205 of UMRA.

C. Regulatory Flexibility Act

Under the Regulatory Flexibility Act (RFA), 5 U.S.C. 601 et seq.,

as amended by the Small Business Regulatory Enforcement Fairness Act

(SBREFA), EPA generally is required to conduct a regulatory flexibility

analysis describing the impact of the regulatory action on small

entities as part of rulemaking. However, under section 605(b) of the

RFA, if EPA certifies that the rule will not have a significant

economic impact on a substantial number of small entities, EPA is not

required to prepare a regulatory flexibility analysis. Pursuant to

section 605(b) of the Regulatory Flexibility Act, 5 U.S.C. 605(b), the

Administrator certifies that this rule will not have a significant

economic impact on a substantial number of small entities. This

regulation merely approves an additional testing procedure for the

measurement of oil and grease and non-polar material but does not

require its use. The new approved method uses n-hexane which has a much

lower cost than Freon-113, which is used in the currently approved

methods.

D. Paperwork Reduction Act

This rule contains no information collection requirements.

Therefore, no information collection request has been submitted to the

Office of Management and Budget (OMB) for review and approval under the

Paperwork Reduction Act of 1980, 44 U.S.C. 3501 et seq.

E. Submission to Congress and the General Accounting Office

The Congressional Review Act, 5 U.S.C. section 801 et seq., as

added by the Small Business Regulatory Enforcement Fairness Act of

1996, generally provides that before a rule may take effect, the agency

promulgating the rule must submit a rule report, which includes a copy

of the rule, to each House of the Congress and to the Comptroller

General of the United States. EPA will submit a report containing this

rule and other required information to the U.S. Senate, the U.S. House

of Representatives and the Comptroller General of the United States

prior to publication of the rule in the Federal Register. A major rule

cannot take effect until 60 days after it is published in the Federal

Register. This rule is not a ``major rule'' as defined by 5 U.S.C.

section 804(2). This rule will take effect on the effective date shown

at the beginning of this preamble.

F. National Technology Transfer and Advancement Act

Under Section 12(d) of the National Technology Transfer and

Advancement Act (NTTAA), the Agency is required 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, business practices,

etc.) that are developed or adopted by voluntary consensus standards

bodies. Where

[[Page 26326]]

available and potentially applicable consensus standards are not used

by EPA, the Act requires the Agency to provide Congress, through the

Office of Management and Budget (OMB), an explanation of the reasons

for not using such standards. EPA's search of the technical literature

has revealed that there are no consensus methods for determination of

hexane extractable material (HEM) and silica gel treated hexane

extractable material (SGT-HEM), although the American Society of

Testing and Materials (ASTM) is in the process of developing an

analytical method for the determination of HEM. If ASTM or another

voluntary consensus standard body approves such a method and EPA

believes that the method is suitable for compliance monitoring and

other purposes, EPA will promulgate the method in a subsequent rule.

G. Executive Order 13045

The Executive Order, ``Protection of Children from Environmental

Health Risks and Safety Risks,'' (62 FR 19885), applies to any rule

initiated after April 21, 1997, or proposed after April 21, 1998, that:

(1) is determined to be ``economically significant'' as defined under

E.O. 12866, and (2) concerns an environmental health or safety risk

that EPA has reason to believe may have a disproportionate effect on

children. If the regulatory action meets both criteria, the Agency must

evaluate the environmental health or safety effects of the planned rule

on children, and explain why the planned regulation is preferable to

other potentially effective and reasonably feasible alternatives

considered by the Agency.

This regulation is not subject to the Executive Order because EPA

published a notice of proposed rulemaking before April 21, 1998 and

further because this is not an economically significant rule as defined

under E.O. 12866. However, EPA's policy since November 1, 1995, has

been to consistently and explicitly consider risks to infants and

children in all risk assessments generated during its decision making

process including the setting of standards to protect public health and

the environment.

EPA's Office of Water has historically considered risks to

sensitive populations (including fetuses, infants, and children) in

establishing risk assessments for setting health or safety standards.

This regulation does not involve the development of a standard to

mitigate environmental health or safety risks. This regulation instead

approves an additional analytical method for compliance monitoring.

However, because the extraction solvent used in Method 1664, n-hexane,

has been associated with neurotoxic effects, EPA investigated the

available health information to determine whether the fetus may be

adversely affected as a result of pregnant women being exposed to n-

hexane in the laboratory environment. Based on animal studies, the

available information on developmental effects does not indicate any

potential risks to the fetus due to exposure to n-hexane.

H. Executive Order 12875

Under Executive Order 12875, ``Enhancing the Intergovernmental

Partnership,'' EPA may not issue a regulation that is not required by

statute and that creates a mandate upon a State, local or tribal

government, unless the Federal government provides the funds necessary

to pay the direct compliance costs incurred by those governments, or

EPA consults with those governments. If EPA complies by consulting,

E.O. 12875 requires EPA to provide to the Office of Management and

Budget a description of the extent of EPA's prior consultation with

representatives of affected State, local and tribal governments, the

nature of their concerns, any written communications from the

governments, and a statement supporting the need to issue the

regulation. In addition, Executive Order 12875 requires EPA to develop

an effective process permitting elected officials and other

representatives of State, local and tribal governments ``to provide

meaningful and timely input in the development of regulatory proposals

containing significant unfunded mandates.''

Today's rule does not create a mandate on State, local or tribal

governments. The rule does not impose any enforceable duties on these

entities. This rule makes available an additional testing procedure

that would merely standardize the procedures when testing is otherwise

required by a regulatory agency. Accordingly, the requirements of

section 1(a) of Executive Order 12875 do not apply to this rule.

I. Executive Order 13084

Under Executive Order 13084, ``Consultation and Coordination with

Indian Tribal Governments,'' EPA may not issue a regulation that is not

required by statute, that significantly or uniquely affects the

communities of Indian tribal governments, and that imposes substantial

direct compliance costs on those communities, unless the Federal

government provides the funds necessary to pay the direct compliance

costs incurred by the tribal governments, or EPA consults with those

governments. If EPA complies by consulting, Executive Order 13084

requires EPA to provide to the Office of Management and Budget, in a

separately identified section of the preamble to the rule, a

description of the extent of EPA's prior consultation with

representatives of affected tribal governments, a summary of the nature

of their concerns, and a statement supporting the need to issue the

regulation. In addition, E.O. 13084 requires EPA to develop an

effective process permitting elected and other representatives of

Indian tribal governments ``to provide meaningful and timely input in

the development of regulatory policies on matters that significantly or

uniquely affect their communities.''

Today's rule does not significantly or uniquely affect the

communities of Indian tribal governments. Further, this rule does not

impose substantial direct compliance costs on tribal governments. This

rule makes available an additional testing procedure which would merely

standardize the procedures when testing is otherwise required by a

regulatory agency. Accordingly, the requirements of section 3(b) of

Executive Order 13084 do not apply to this rule.

List of Subjects

40 CFR Part 136

Environmental protection, Analytical methods, Incorporation by

reference, Monitoring, Reporting and recordkeeping requirements, Waste

treatment and disposal, Water pollution control.

40 CFR Part 260

Environmental protection, Administrative practice and procedure,

Analytical methods, Confidential business information, Hazardous waste,

Incorporation by reference, Reporting and recordkeeping requirements.

Dated: May 7, 1999.

Carol M. Browner,

Administrator.

For the reasons set out in the preamble, title 40, chapter I of the

Code of Federal Regulations, is amended as follows:

PART 136--GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS

OF POLLUTANTS

1. The authority for part 136 continues to read as follows:

Authority: Secs. 301, 304(h), 307, and 501(a) Pub. L. 95-217, 91

Stat. 1566, et seq. (33 U.S.C. 1251, et seq.) (the Federal Water

Pollution Control Act Amendments of 1972 as amended by the Clean

Water Act of 1977.)

2. In Sec. 136.3, paragraph (a), Table IB is amended by revising

entry 41 to read as follows:

[[Page 26327]]

Sec. 136.3 Identification of test procedures.

(a) * * *

* * * * *

Table IB--List of Approved Inorganic Test Procedures

--------------------------------------------------------------------------------------------------------------------------------------------------------

Reference (method number or page)

--------------------------------------------------------------------------------------------------------------------

Parameter, units and method STD methods 18th

EPA 1, 35 ed. ASTM USGS\2\ Other

--------------------------------------------------------------------------------------------------------------------------------------------------------

* * * * * * *

41. Oil and grease--Total 413.1.......................... 5520 B\38\

recoverable, mg/L: Gravimetric

(extraction).

Oil and grease and non-polar 1664, Rev. A...................

material, mg/L: Hexane extractable

material (HEM): n-Hexane

extraction and gravimetry\42\.

Silica gel treated HEM (SGT-HEM): 1664, Rev. A...................

Silica gel treatment and

gravimetry\42\.

* * * * * * *

--------------------------------------------------------------------------------------------------------------------------------------------------------

Table 1B Notes:

\1\ ``Methods for Chemical Analysis of Water and Wastes'', Environmental Protection Agency, Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-

Ci), EPA-600/4-79-020, Revised March 1983 and 1979 where applicable.

\2\ Fishman, M.J., et al, ``Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments,'' U.S. Department of the Interior, Techniques

of Water--Resource Investigations of the U.S. Geological Survey, Denver, CO, Revised 1989, unless otherwise stated.

* * * * * * *

\35\ Precision and recovery statements for the atomic absorption direct aspiration and graphite furnace methods, and for the spectrophotometric SDDC

method for arsenic are provided in Appendix D of the part titled, ``Precision and Recovery Statements for Methods for Measuring Metals.''

* * * * * * *

\38\ Only the trichlorofluoromethane extraction solvent is approved.

* * * * * * *

\42\ Method 1664, Revision A ``n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractablke Material (SGT-HEM; Non-

polar Material) by Extraction and Gravimetry'' EPA-821-R-98-002, February 1999. Available at NTIS, PB-121949, U.S. Department of Commerce, 5285 Port

Royal, Springfield, Virginia 22161.

* * * * * * *

PART 260--HAZARDOUS WASTE MANAGEMENT SYSTEM: GENERAL

1. The authority for part 260 continues to read as follows:

Authority: 42 U.S.C. 6905, 6912(a), 6921-6927, 6930, 6934, 6935,

6937, 6939, and 6974.

Subpart B--Definitions

2. Section 260.11 is amended by revising paragraph (a)(11) and by

adding paragraph (a)(16) to read as follows:

Sec. 260.11 References.

* * * * *

(a) * * *

(11) ``Test Methods for Evaluating Solid Waste, Physical/Chemical

Methods,'' EPA Publication SW-846 [Third Edition (November 1986), as

amended by Updates I (dated July 1992), II (dated September 1994), IIA

(dated August 1993), IIB (dated January 1995), III (dated December

1996) and IIIA (dated April 1998)]. The Third Edition of SW-846 and

Updates I, II, IIA, IIB, and III (document number 955-001-00000-1) are

available from the Superintendent of Documents, U.S. Government

Printing Office, Washington, DC 20402, (202) 512-1800. Update IIIA is

available through EPA's Methods Information Communication Exchange

(MICE) Service. MICE can be contacted by phone at (703) 821-4690.

Update IIIA can also be obtained by contacting the U.S. Environmental

Protection Agency, Office of Solid Waste (5307W), OSW Methods Team, 401

M Street, SW, Washington, DC, 20460. Copies of the Third Edition and

all of its updates are also available from the National Technical

Information Service (NTIS), 5285 Port Royal Road, Springfield, VA

22161, (703) 605-6000 or (800) 553-6847. Copies may be inspected at the

Library, U.S. Environmental Protection Agency, 401 M Street, SW,

Washington, DC 20460; or at the Office of the Federal Register, 800

North Capitol Street, NW, suite 700, Washington, DC.

* * * * *

(16) Method 1664, Revision A, n-Hexane Extractable Material (HEM;

Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material

(SGT-HEM; Non-polar Material) by Extraction and Gravimetry. Available

at NTIS, PB99-121949, U.S. Department of Commerce, 5285 Port Royal,

Springfield, Virginia 22161.

* * * * *

[FR Doc. 99-12163 Filed 5-13-99; 8:45 am]

BILLING CODE 6560-50-P