Federal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations 26315

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.

SUMMARY: This action approves use of

EPA Method 1664, Revision A: NHexane Extractable Material (HEM; Oil

and Grease) and Silica Gel Treated NHexane 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 (nhexane) 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 qualitybased 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:

Category Examples of potentially regulated

entities

Regional,

State

and

Territorial

Governments

and

Indian

Tribes.

States, Territories, and 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.

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
26316 Federal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations

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 nHexane 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

Solvent

Number

of samples

Mean

(mg/L)

Standard deviation

CFC–113 .... 1,101 11.4 2.1

n-hexane ..... 353 11.4 2.4
Federal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations 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; nonpolar 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 nhexane 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 RCRArelated 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 nhexane 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
26318 Federal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations

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, nhexane 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 noncompliance 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 nhexane 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 (<ML) not

be used in the comparison because it is

desirable to have actual measured

values to test equivalency of results

using the different methods. In the event

that a test result less than the ML is

obtained, the number of tests should be

increased to provide a minimum of

seven paired triplicate results for the

comparison.

Statistical significance should be

tested according to procedures for

development of the root-mean-square

deviation (RMSD) detailed in EPA’s

Freon Replacement Study reports using

results obtained with CFC–113 as the

reference. If the RMSD is within the

acceptance limit, the results obtained

using the different methods are

equivalent.

IV. Timing of Required Use of Method

1664 and Phaseout of Use of CFC–113

EPA proposed to withdraw approved

use of previously approved methods

and require use of Method 1664 on a

date exactly six months after the date of

publication of a final rule. This time lag

was to allow for existing supplies of

CFC–113 to be used, for laboratories to

become familiar with Method 1664, and

for dischargers/generators/industrial

users and regulatory authorities to

determine if a conversion factor based

on a difference in the amount of

material extracted is appropriate.

Commenters suggested alternate dates

for withdrawal, ranging between

‘‘immediate withdrawal of presently

approved methods’’ and ‘‘continue use

of CFC–113 methods indefinitely’’ (see

Section VI below and the detailed

comments and responses in the Docket

for today’s final rule). To accommodate

regulated entities’ concern that the

requirement to change from CFC-based

methods to Method 1664 could result in

non-compliance, and based on an

extension of the time for laboratory use

of CFC–113 to 2005, EPA has decided to

approve use of Method 1664 but not

withdraw approved use of the CFCbased methods.

EPA strongly encourages dischargers/

generators/industrial users to substitute

use of Method 1664 beginning on the

effective date of today’s rulemaking

rather than awaiting reissuance of the

existing permit that currently requires
Federal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations 26319

use of a CFC–113 method. Also, instead

of awaiting permit reissuance, EPA

encourages prompt modification of the

existing permit to specify the use of

Method 1664. To accommodate those

permittees wishing to use Method 1664

once today’s rule becomes effective and

to expedite reduction in CFC–113 use,

EPA will exercise enforcement

discretion with respect to the method

used for compliance. This enforcement

discretion does not extend, however, to

liability for any violation of a permit

limitation or condition, including the

oil and grease limitation, only to a

requirement to use a CFC–113 method

to determine compliance or noncompliance. If non-compliance results

from the use Method 1664, the

permitting authority may establish a

conversion factor, as detailed earlier in

this preamble.

V. Improvements and Changes to

Method 1664 Since Proposal

The Agency has revised Method 1664

(‘‘Method 1664, Revision A’’) to indicate

that it is different from previous

versions. The significant changes

resulting in this revision are the change

of name from ‘‘total petroleum

hydrocarbons’’ to ‘‘non-polar material,’’

the change of the status of the matrix

spike duplicate (MSD) from a

requirement to a suggestion, the change

of an analytical batch to a maximum of

20 samples, and the allowed use of

solid-phase extraction (SPE) without a

demonstration of equivalency.

A. Names and Name Changes

Confusion of the names used for the

analytes determined by Method 1664

prompted EPA to examine these names.

As a result, the name ‘‘n-hexane

extractable material’’ (HEM) has been

retained to be synonymous with ‘‘oil

and grease,’’ but the name ‘‘total

petroleum hydrocarbons (TPH)’’ has

been dropped in favor of ‘‘non-polar

material’’ (NPM) to indicate ‘‘silica-gel

treated n-hexane extractable material’’

(SGT–HEM), as detailed below.

1. Oil and Grease′

The EPA Administrator designated

‘‘oil and grease’’ as a conventional

pollutant under the Clean Water Act

(see 40 CFR 401.16). Oil and grease

consists of those chemical substances

extracted from water or wastes using a

solvent. The nature of the substances

extracted are determined by the

extracting solvent and the extraction

technique. Both CFC–113 and n-hexane

extract many pure materials at nearly

100 percent efficiency. When mixtures

of substances that typically occur in

complex wastewater discharges and in

complex solid and semi-solid wastes are

present, the two solvents may extract

different amounts of material. For most

wastes and wastewaters, materials

commonly extracted are relatively nonvolatile hydrocarbons, vegetable oils,

animal fats, waxes, soaps, greases, and

related materials. Because the nature

and amount of material extracted is

defined by the solvent and, to a lesser

degree, by the details of the procedure

used for extraction, EPA uses the term

‘‘method-defined analyte’’ to identify oil

and grease.

Today’s final rule approves use of

Revision A of EPA Method 1664: nHexane Extractable Material (HEM; Oil

and Grease) and Silica-gel Treated nHexane Extractable Material (SGT–

HEM; Non-polar Material) by Extraction

and Gravimetry, in which n-hexane is

used as the extracting solvent, in

addition to currently approved methods

in which CFC–113 is used as the

extracting solvent. The name ‘‘n-hexane

extractable material’’ (HEM) reflects that

it is the material extracted by normal

hexane (n-hexane) that is being

measured using Method 1664. The

common name ‘‘oil and grease’’ is being

retained because of its familiarity to the

analytical community.

2. Non-Polar Material

At proposal, EPA used the term ‘‘total

petroleum hydrocarbons’’ (TPH) to

designate the substances that remain

after n-hexane extractable material is

exposed to silica gel. Use of the term

‘‘total petroleum hydrocarbons’’ and the

abbreviation TPH was confusing to the

analytical community because the term

is used in other analytical methods that

measure a different property or material,

in some instances by a different

analytical technique. For example, EPA

Method 418.1 and Standard Method

5520 F measure polar materials termed

‘‘petroleum hydrocarbons’’ using

infrared spectroscopy, and certain SW–

846 and State methods measure TPH by

gas chromatography. The term ‘‘nonpolar material’’ (NPM) was chosen for

use in today’s version of Method 1664

to avoid confusion with these uses of

the term TPH.

Silica gel has the property that it

removes ‘‘polar’’ material. Polar material

includes aromatic compounds (those

containing one or more benzene rings),

unsaturated compounds (those

containing one or more double bonds),

and compounds containing atoms other

than carbon and hydrogen (e.g.,

chlorine, oxygen, nitrogen, sulfur), and

other compounds. Polar material also

includes aromatic, phenolic, and

heterocyclic compounds in petroleum

and petroleum products, soaps, and

animal fats. Silica gel adsorbs these

polar materials, so the material that

remains is ‘‘non-polar material.’’ Nonpolar material contains straight and

branched chain hydrocarbons (aliphatic

hydrocarbons) and other chemical

substances in which there are either no

mixture of atoms of different types

(hetero-atoms; e.g., chlorine, oxygen,

nitrogen, sulfur) or these mixtures are

‘‘balanced’’ in the molecule. For

example, the pollutant

hexachloroethane, although containing

chlorine atoms, does not exhibit

sufficient polarity to be adsorbed by

silica gel. As with HEM, the exact

nature and amount of substances that

will be adsorbed by silica gel is defined

by the adsorption process. Therefore, as

with oil and grease (HEM), SGT–HEM

(NPM) is a ‘‘method-defined analyte.’’

B. Other Changes and Improvements

1. Changes to Quality Control (QC)

EPA has made two changes to the QC

in Method 1664 in response to

comments that the QC was onerous to

laboratories: (1) the requirement for a

matrix spike duplicate (MSD) has been

changed to a suggestion; and (2) the size

of an analytical batch has been

increased to a maximum of 20 samples.

This QC is consistent with the QC in

methods for use under the CWA that are

published at 40 CFR part 136, Appendix

A. These methods use a single matrix

spike (termed a ‘‘QC check sample’’ in

those methods) to evaluate matrix

effects and require matrix spikes at a

minimum frequency of five percent (1 in

20) of samples from a given discharge/

waste stream. The on-going precision

and recovery (OPR) sample and blank

are also at a minimum frequency of five

percent (1 in 20). For those laboratories

wishing to evaluate precision with each

analytical batch, an MSD is suggested

but not required.

2. Miscellaneous Changes and

Improvements

Nearly all of the other improvements

to Method 1664 are minor technical

improvements that correct or clarify

language in the Method. Most

improvements were incorporated in

response to a comment or comments.

EPA refers readers to the comments and

responses detailed in the Docket for

additional information. EPA believes

that none of these changes or

improvements or the other changes and

improvements warrant re-proposal of

Method 1664. Miscellaneous changes

and improvements include:

• The hexadecane/stearic acid

standard solution has been diluted by a

factor of 2 and twice as much standard
26320 Federal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations

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°C (¥9 °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 nFederal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations 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 nhexane 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 °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, nhexane-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.
26322 Federal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations

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, solidphase, 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 methoddefined 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
Federal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations 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 nHexane 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-byside 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
26324 Federal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations

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 reevaluated, 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 °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 °C to be consistent with

holding time study data and to allow

storage at 0 °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 nhexane 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 nhexane 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. Methoddefined 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
Federal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations 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 costeffective 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 nonpolar material but does not require its

use. The new approved method uses nhexane 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
26326 Federal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations

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 § 136.3, paragraph (a), Table IB

is amended by revising entry 41 to read

as follows:
Federal Register / Vol. 64, No. 93 / Friday, May 14, 1999 /Rules and Regulations 26327

§ 136.3 Identification of test procedures.

(a) * * *

* * * * *

TABLE IB—LIST OF APPROVED INORGANIC TEST PROCEDURES

Parameter, units and method

Reference (method number or page)

EPA 1, 35

STD methods 18th

ed.

ASTM USGS2 Other

* * * * * * *

41. Oil and grease—Total recoverable, mg/L: Gravimetric (extraction).413.1 ........................ 5520 B38

Oil and grease and non-polar material, mg/L: Hexane extractable

material (HEM): n-Hexane extraction and gravimetry42.

1664, Rev. A.

Silica gel treated HEM (SGT–HEM): Silica gel treatment and gravimetry42.1664, Rev. A.

* * * * * * *

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. 2Fishman, 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.

* * * * * * *

35Precision 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.’’

* * * * * * *

38Only 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:

§ 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, nHexane Extractable Material (HEM; Oil

and Grease) and Silica Gel Treated nHexane 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

FEDERAL COMMUNICATIONS

COMMISSION

47 CFR Part 73

Radio Broadcast Services

CFR Correction

In Title 47 of the Code of Federal

Regulations, parts 70 to 79, revised as of

Oct. 1, 1998, page 193, § 73.624 (c)

introductory text, last sentence, is

corrected by adding ‘‘not’’ after ‘‘shall’’

and before ‘‘be’’.

[FR Doc. 99–55519 Filed 5–13–99; 8:45 am]

BILLING CODE 1505–01–D