99-12163. 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

[Federal Register Volume 64, Number 93 (Friday, May 14, 1999)]
[Rules and Regulations]
[Pages 26315-26327]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 99-12163]

[[Page 26315]]

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ENVIRONMENTAL PROTECTION AGENCY

40 CFR Parts 136 and 260

[FRL-6341-9]
RIN 2040-AC63

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

AGENCY: Environmental Protection Agency (EPA).

ACTION: Final rule.

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SUMMARY: This action approves use of EPA Method 1664, Revision A: N-
Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel
Treated N-Hexane Extractable Material (SGT-HEM; Non-polar Material) by
Extraction and Gravimetry (hereafter Method 1664) for use in EPA's
Clean Water Act (CWA) programs. This action also deletes Method 9070,
adds revised Method 9071B, and incorporates Method 1664 by reference
for use in EPA's Resource Conservation and Recovery Act (RCRA)
programs. Method 1664 is also approved for determination of non-polar
material (NPM) as silica gel treated n-hexane extractable material
(SGT-HEM) to support phaseout of use of CFC-113 for determination of
NPM in EPA's CWA and RCRA programs.
These actions are being taken as a part of EPA's effort to reduce
dependency on use of chlorofluorocarbons (CFCs) to protect Earth's
ozone layer and to meet the CFC phaseout agreed to in the Montreal
Protocol and required by the Clean Air Act Amendments of 1990. Method
1664 uses normal hexane (n-hexane) as the extraction solvent in place
of 1,1,2-trichloro-1,2,2-trifluoroethane (CFC-113; Freon-113), a Class
1 CFC.

DATES: This regulation is effective June 14, 1999. For judicial review
purposes, this final rule is promulgated as of 1:00 p.m. Eastern
Standard Time on May 28, 1999 in accordance with 40 CFR 23.7.
The incorporation by reference of Method 1664 is approved by the
Director of the Federal Register May 14, 1999.

ADDRESSES: Copies of the public comments received, EPA responses, and
all other supporting documents (including references included in this
notice) are available for review at the U.S. Environmental Protection
Agency, Water Docket, 401 M Street SW, Washington, DC 20460. For access
to docket materials, call 202-260-3027 on Monday through Friday,
excluding Federal holidays, between 9:00 a.m. and 3:30 p.m. Eastern
Time for an appointment.
Copies of Method 1664 are available from the National Technical
Information Service (NTIS), 5285 Port Royal Road, Springfield, VA
22161, (703) 605-6000 or (800) 553-6847. The NTIS publication number is
PB99-121949.
Copies of the Third Edition of SW-846 and Updates I, II, IIA, IIB,
and III (document number 955-001-00000-1) are available from the
Superintendent of Documents, U.S. Government Printing Office,
Washington, DC 20402, (202) 512-1800. Update IIIA is available through
EPA's Methods Information Communication Exchange (MICE) Service. MICE
can be contacted by phone at (703) 821-4690. Update IIIA can also be
obtained by contacting the U.S. Environmental Protection Agency, Office
of Solid Waste (5307W), OSW Methods Team, 401 M Street, SW, Washington,
DC, 20460. Copies of the Third Edition and all of its updates are also
available from the National Technical Information Service (NTIS), 5285
Port Royal Road, Springfield, VA 22161, (703) 605-6000 or (800) 553-
6847. In addition, a CD-ROM version of SW-846, Third Edition, as
amended by Updates I through III is available from NTIS (PB97-501928).
In the future, the CD-ROM will be updated by NTIS to include additional
updates, including Update IIIA.
An electronic version of Method 1664 and Method 9071B are also
available via the Internet at http://www.epa.gov/OST.

FOR FURTHER INFORMATION CONTACT: For information regarding Method 1664
and its use in Clean Water Act programs, contact Maria Gomez-Taylor,
Engineering and Analysis Division (4303), USEPA Office of Science and
Technology, 401 M Street, SW, Washington, DC 20460, or call (202) 260-
1639. For information regarding Update IIIA and the use of Method 1664
in the Resource Conservation And Recovery Act programs, contact Gail
Hansen, Office of Solid Waste (5307W), USEPA, 401 M Street, SW,
Washington, DC 20460, or call (703) 308-8855.

SUPPLEMENTARY INFORMATION:

Potentially Regulated Entities

EPA Regions, as well as States, Territories and Tribes authorized
to implement the National Pollutant Discharge Elimination System
(NPDES) program, issue permits that comply with the technology-based
and water quality-based requirements of the Clean Water Act. In doing
so, the NPDES permitting authority, including authorized States,
Territories, and Tribes, make a number of discretionary choices
associated with permit writing, including the selection of pollutants
to be measured and, in many cases, limited in permits. If EPA has
``approved'' standardized testing procedures (i.e., promulgated through
rulemaking) for a given pollutant, the NPDES permit must include one of
the approved testing procedures or an approved alternate test
procedure. Therefore, entities with NPDES permits could be affected by
the standardization of testing procedures in this rulemaking. These
entities may be affected because NPDES permits may incorporate the
standardized testing procedure approved for use in today's rulemaking.
In addition, when a State, Territory, or authorized Tribe provides
certification of federal licenses under Clean Water Act section 401,
States, Territories and Tribes are directed to use the standardized
testing procedures. Under the RCRA program, this method may be required
as part of a hazardous waste delisting petition. Categories and
entities that may ultimately be affected include:

------------------------------------------------------------------------
Examples of potentially
Category regulated entities
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Regional, State and Territorial States, Territories, and Tribes
Governments and Indian Tribes. authorized to administer the
NPDES permitting program;
States, Territories, and
Tribes providing certification
under Clean Water Act section
401; Governmental NPDES
permittees; Regional and State
offices implementing delisting
petitions.
Industry............................... Industrial NPDES permittees;
delisting petitioners.
Municipalities......................... Publicly-owned treatment works
with NPDES permits.
------------------------------------------------------------------------

This table is not intended to be exhaustive, but rather provides a
guide for readers regarding entities likely to be affected by this
action. This table lists the types of entities that EPA is now aware
could potentially be affected by this action. Other types of entities
not listed in the table could also be affected. If you have questions
regarding the applicability of this action to a particular entity,
consult the person listed in the preceding FOR FURTHER INFORMATION
CONTACT section.

Outline of Preamble

I. Authorities
A. Clean Water Act
B. Resource Conservation and Recovery Act
C. Clean Air Act Amendments of 1990
II. Background and History

[[Page 26316]]

A. Regulatory Background
B. Data Gathering
1. EPA's Freon Replacement Studies
2. Water Pollution Performance Evaluation Data
3. Data Received from Commenters
III. Explanation of Today's Action
A. Application of Method 1664 in Clean Water Act Program
1. General Use
2. Search for Other Uses of CFCs in Clean Water Act Program
B. Application of Method 1664 in Resource Conservation and
Recovery Act Program
C. Use of Solid-phase Extraction (SPE)
D. Differences in Results Produced by CFC-113 and n-Hexane and
Determinations of Compliance
IV. Timing of Required Use of Method 1664 and Phaseout of Use of
CFC-113
V. Improvements and Changes to Method 1664 Since Proposal
A. Names and Name Changes
1. Oil and Grease
2. Non-polar Material
B. Other Changes and Improvements
1. Changes to Quality Control
2. Miscellaneous Changes and Improvements
VI. Public Participation and Response to Comments
A. Regulatory Issues
B. Health and Safety Concerns
C. Economic Concerns
D. Solid-phase Extraction (SPE)
1. Comments Supporting Use of SPE
2. Comments Expressing Concern About the Use of SPE
E. Grace period for CFC-113
F. Use of Silica-gel Treated n-Hexane Extractable Material
Procedure
G. Detection and Quantitation
H. Matrix Effects
I. Method Modifications
J. Matrix Spike/Matrix Spike Duplicate
K. Precision and Recovery
L. Differences in Results Produced by n-Hexane and CFC-113
M. Method Validation and QC Acceptance Criteria
N. Quality Control
O. Sample Collection and Preservation
P. Miscellaneous Issues
VII. Regulatory Requirements
A. Executive Order 12866
B. Unfunded Mandates Reform Act
C. Regulatory Flexibility Act
D. Paperwork Reduction Act
E. Submission to Congress and the General Accounting Office
F. National Technology Transfer and Advancement Act
G. Executive Order 13045
H. Executive Order 12805
I. Executive Order 13084

I. Authorities

A. Clean Water Act

These regulations are being promulgated under the authority of
sections 301, 304, and 501(a) of the Clean Water Act (CWA), 33 U.S.C.
1311, 1314(h), 1361(a).

B. Resource Conservation and Recovery Act

These regulations are being promulgated under the authority of
sections 1006, 2002(a), 3001-3007, 3010, 3013-3018, and 7004 of the
Solid Waste Disposal Act (SWDA), as amended by the Resource
Conservation and Recovery Act of 1976 (RCRA), as amended (42 U.S.C.
6905, 6912(a), 6921-6927, 6930, 6934-6930, and 6974).

C. Clean Air Act Amendments of 1990

These regulations are consistent with intent of sections 604, 606,
and 608 of the 1990 Clean Air Act Amendments (CAAA) to phase out
production of Class I CFCs and reduce use and emissions of Class I CFCs
to the lowest achievable level, and with section 613 of CAAA to reduce
the Federal procurement of products and services that employ CFCs.

II. Background and History

A. Regulatory Background

This final rule affects regulations implementing analytical methods
under the Clean Water Act and the Resource Conservation and Recovery
Act. This final rule supports, in part, EPA's Stratospheric Ozone
Protection Program in the Office of Air and Radiation (OAR). The
regulatory background for each of these programs is not given in detail
in this rule; rather, pertinent proposals and rules are referenced, as
follows:
EPA provided a history of analytical methods under 40 CFR part 136
on February 7, 1991 (56 FR 5090) in the proposal of EPA Method 1613.
The Agency presented a brief background on the use of analytical
methods as support for effluent limitations, permit applications, and
compliance monitoring, and a brief description of the alternate test
procedure program (ATP) in the proposal of several new 40 CFR part 136
methods on October 18, 1995 (60 FR 53988). The details of Method 1664
and issues surrounding its use were given at proposal on January 23,
1996 (61 FR 1730).
The EPA Office of Solid Waste gave a brief description of the
regulatory framework for SW-846 methods in a final rule promulgating
the third update to the SW-846 methods on June 13, 1997 (62 FR 32452).
Method 1664 is approved as ``guidance'' under the RCRA programs (see
Section III.B.). Other methods may be used under the conditions stated
in the RCRA regulations (see 40 CFR part 268).
The regulatory background for development of effluent guidelines
and standards is given in proposed and final rules for these guidelines
and standards. See, for example, Section III of the final rule for the
Coastal Subcategory of Oil and Gas Extraction promulgated on December
16, 1996 (61 FR 66086).
The background and history of applicability of EPA's Stratospheric
Ozone Protection Program to analytical methods requiring use of CFCs in
EPA's CWA programs was given in a proposal for an earlier EPA method
for determination of oil and grease on July 3, 1991 (56 FR 30519). The
Montreal Protocol and Section 604 of the Clean Air Act Amendments of
1990 impose limits on the production and consumption of certain ozone-
depleting substances including CFC-113 (see 40 CFR part 82).

B. Data Gathering

Data gathered to support today's final rule were Freon replacement
studies and other data gathered prior to proposal, data collected in
EPA's Water Pollution (WP) Performance Evaluation (PE) Study 038, and
data received from commenters.
1. EPA's Freon Replacement Studies
EPA summarized details of EPA studies that support today's final
rule at proposal (see 61 FR 1730) and presented information in reports
of EPA's Phase I Freon Replacement Study (EPA-821-R-93-011), Phase II
Freon Replacement Study (EPA-820-R-95-003), and Method Validation Study
(821-R-95-036). These reports are included in the Water Docket for the
proposed rule.
2. Water Pollution Performance Evaluation Data
EPA has collected data on the performance of laboratories
conducting routine analyses of wastewaters through water pollution
performance evaluation (PE) studies. For water pollution PE study 038
conducted in late calendar year 1997, EPA accepted data from
laboratories determining oil and grease using either CFC-113 or n-
hexane. The results of this study are summarized in Table 1 and show
that, for this study, CFC-113 and n-hexane extracted identical average
amounts of oil and grease.

Table 1.--Results of Performance Evaluation Study 038 for Determination
of Oil and Grease
------------------------------------------------------------------------
Number
Solvent of Mean (mg/ Standard
samples L) deviation
------------------------------------------------------------------------
CFC-113.................................. 1,101 11.4 2.1
n-hexane................................. 353 11.4 2.4
------------------------------------------------------------------------

[[Page 26317]]

3. Data Received From Commenters
As detailed in other sections of this preamble and in the detailed
comments and responses included in the Docket, EPA utilized data
submitted in response to the proposal of Method 1664 for improvements
included in the version of Method 1664 being approved for use today.
All comments are included in the Water Docket.

III. Explanation of Today's Action

Today's final rule approves Method 1664 determination of n-hexane
extractable material (HEM; oil and grease) and silica-gel treated n-
hexane extractable material (SGT-HEM; non-polar material) in EPA's CWA
and RCRA programs. Today's action has an economic benefit to regulated
entities measuring oil and grease and non-polar material (NPM) in that
the cost of CFC-113 is considerably greater than the cost of n-hexane
as a result of the production phase-out of CFCs and increased tariffs
on their use. The costs for CFCs being phased out can be expected to
rise as production ceases and tariffs increase further. Because n-
hexane is a product of oil refining on a large scale, the impact of the
additional demand for n-hexane is expected to be insignificant. As
pointed out by commenters, however, laboratory use of CFC-113 was small
in comparison to other uses. Indeed, many commenters claimed that
because of safety problems and the disparity in results produced by use
of CFC-113 vs. n-hexane, use of CFC-113 should be continued
indefinitely. Based on these comments and an extension of the
laboratory use exemption to 2005, EPA has decided to allow continued
use of methods that use CFC-113 and to approve use of Method 1664 for
those regulated entities that desire to switch to use of n-hexane.

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

1. General Use
Method 1664 will be used in EPA's wastewater program for regulation
development, permit applications, and compliance monitoring. More than
600 industrial subcategories are regulated under Clean Water Act
pollution control programs (see the rules for these industrial
subcategories at 40 CFR parts 400-510). Nearly all of these regulations
contain nationwide effluent guidelines and standards limiting the
amount of oil and grease that may be discharged from facilities in
these subcategories. EPA estimates that more that 10,000 National
Pollutant Discharge Elimination System (NPDES) permits contain a limit
for oil and grease, potentially necessitating an estimated minimum of
25,000 measurements annually.
2. Search for Other Uses of CFCs in Clean Water Act Program
EPA performed computerized string searches of 40 CFR parts 100-149,
and of Subchapter N, ``Effluent Guidelines and Standards,'' at 40 CFR
parts 400-500 for ``TPH'', ``Freon-113'', ``CFC-113'',
``chlorofluoro'', ``413.1'', and related terms in an attempt to locate
references to CFC-113 and Method 413.1 for determination of oil and
grease. EPA could find no references other than in 40 CFR part 136 and
to the procedure for petroleum hydrocarbons in the Coil Coating
standards at 40 CFR 465.03(c). EPA intends to consider allowing use of
Method 1664 through subsequent rulemaking for the Coil Coating Point
Source Category.

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

Analytical methods found acceptable for testing under Subtitle C of
RCRA are contained in OSW publication SW-846, Test Methods for
Evaluating Solid Waste, Physical/Chemical Methods. Use of some of these
methods is required by some of the hazardous waste regulations under
Subtitle C of RCRA. In other situations, SW-846 functions as a guidance
document setting forth acceptable, although not required, methods to be
implemented by the user, as appropriate, in satisfying RCRA-related
sampling and analysis requirements. As of Update III to SW-846, the two
SW-846 methods for determination of oil and grease have been Method
9070 for waters and aqueous wastes, and Method 9071A for solid and
semi-solid material such as soil, sediment, and sludge. Method 9070 is
virtually identical to presently approved CWA methods for determination
of oil and grease. Method 9071A employs drying of the sample with
magnesium sulfate and Soxhlet extraction with CFC-113 for the
determination. These methods are not specifically required by any RCRA
regulation, although they can be required as part of a hazardous waste
de-listing demonstration.
In today's final rule, SW-846 is being amended further to delete
Method 9070 and to include revised Method 9071B as Update IIIA.
Specifically, Method 9071B addresses the use of n-hexane instead of
CFC-113 as the extraction solvent, in a manner consistent with the use
of n-hexane in Method 1664. In addition, in place of Method 9070, which
uses CFC-113 as the extraction solvent in the testing of waters and
aqueous wastes, the Agency is incorporating by reference Method 1664 in
the RCRA regulations. As part of Update IIIA, SW-846 refers the
regulated community to Method 1664 for testing previously conducted
using Method 9070.
EPA compared results of Soxhlet extraction of solids and sludges
with various solvents, including CFC-113 and n-hexane, in the Phase I
Freon Replacement Study (EPA-821-R-93-011). Results of this study
showed that, as with testing of waters which was described in the Phase
I study report that was included in the Docket at proposal, CFC-113 and
n-hexane extract different amounts of material. However, for petroleum-
based samples, the amount of material extracted by CFC-113 and n-hexane
was not significantly different. This is the same conclusion that was
reached regarding extraction of waters. As a result, and for the other
reasons allowing use of Method 1664 detailed at proposal and in other
sections of this preamble as supported by the information contained in
the Water Docket, EPA believes that changes to SW-846 as a result of
Update IIIA, i.e., the use of Method 1664 in place of Method 9070 and
the addition of Method 9071B to SW-846, are appropriate and logical
outgrowths of the Agency's efforts to reduce dependency on the use of
CFCs.

C. Use of Solid-Phase Extraction (SPE)

SPE uses a cartridge or disk for removal of the oil and grease from
the sample. A detailed description of the SPE technique was provided at
proposal (61 FR 1730). Even prior to proposal of Method 1664, vendors
of SPE devices had requested that SPE be an allowed technique in the
Method. Proposed Method 1664 allowed use of SPE, but required a
demonstration that SPE produced results equivalent to results produced
by the separatory funnel liquid-liquid extraction technique (LLE)
written in Method 1664. Vendors and other commenters objected to this
requirement, claiming that SPE provided sufficient advantages in
solvent reduction, reduced analysis time, reduced emulsion formation,
and other advantages so that its use should be allowed without prior
demonstration of equivalency. EPA discussed the issue extensively at
proposal and in public workshops and meetings, and specifically
solicited data demonstrating equivalency of results produced by SPE and
LLE. Data received were mixed, with some data demonstrating that
results produced are equivalent and other data demonstrating that
results produced are significantly different. EPA reopened the comment
period (61

[[Page 26318]]

FR 26149) to allow submission of further data, and EPA provided a
notice of availability (62 FR 51621) of these and other data so that
EPA could consider these data for today's final rule.
Discussions of the detailed issues on SPE are summarized in Section
VI of this preamble and given in the detailed comments and responses
included in the Docket. Based on comments received and supporting data,
EPA is allowing the use of SPE in the version of Method 1664 being
approved today without a prior demonstration of equivalency. However,
EPA has added a note at the beginning of the extraction procedure
(Section 11.3) in Method 1664 to indicate that it is the discharger/
generator's responsibility to assure that the results produced are
equivalent. If there is doubt about this equivalency, liquid/liquid
extraction is definitive for the measurement.
EPA also acknowledges that if a Region, State, or other permitting
authority has concerns about the difference in results produced by SPE
and LLE, that authority may specify in the permit the use of one of the
two techniques.

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

Since EPA announced results of the Phase I Freon Replacement Study
in 1993, several commenters expressed concerns about the impact of
differences resulting from substitution of CFC-113 with n-hexane on
determinations of compliance under the NPDES program and pretreatment
programs. EPA discussed this issue at proposal (61 FR 1730; January 23,
1996), and discussed the issue in workshops, conferences, and seminars
between proposal and development of today's final rule.
After proposal, EPA received numerous requests from States and EPA
Regions for guidance on implementation of Method 1664. On July 9, 1996,
EPA issued guidance to Pretreatment Coordinators and Regional NPDES
Contacts. A copy of the memorandum is included in the Docket for
today's final rule. In part, this memorandum states the following:

``EPA acknowledges that, due to the diverse nature of
discharges, there may be instances in which n-hexane will extract an
amount of oil and grease greater or less than the amount extracted
by Freon-113. If these instances affect compliance, the permitting
authority may wish to consider establishing a conversion factor,
multiplier, or divisor to account for these differences in the
permit. EPA emphasizes that few, if any, instances will likely be
found in which the differences affect compliance and, therefore,
urges direct substitution of the presently approved methods with
Method 1664 when the date of substitution is announced in the
Federal Register.''

By today's final rule, EPA still believes that the approach
outlined in the memorandum appropriately accommodates any significant
discrepancies that could arise in determining compliance with
limitations or standards for oil and grease using the new method. Based
on the results from the Freon Replacement Studies, EPA found that, on
average, n-hexane extracted approximately 96% of the material extracted
using CFC-113. Therefore, while there may be some effluent matrices
where n-hexane will extract more material than CFC-113, on the whole,
most dischargers would have little risk of a determination of non-
compliance with existing limits. The slightly smaller amount of oil and
grease extracted by n-hexane (96% versus 100% by CFC-113) is not
statistically significant because errors in oil and grease measurement
are in the order of 10 percent relative standard deviation. A coarse
estimate of 95% confidence limits around the 96% recovery by n-hexane
is 96 plus or minus 20%, or the true difference lies somewhere between
76-116%. This encompasses 100% or no difference. Given the lack of
significance of the 4% difference, the measurement error that would be
encountered in the side-by-side comparison (estimated at 10% for each
measurement), the potentially significant cost of a side-by-side
comparison with each discharge and the low anticipated likelihood that
a significant difference would be found (based on EPA's studies), EPA
does not recommend a side-by-side comparison for each discharge.
Instead, EPA continues to recommend a direct replacement of the
approved Freon methods with Method 1664.
However, to accommodate regulated entities concerned about
differences produced, EPA is not withdrawing approved use of methods
employing CFC-113, a Class I ozone depleting substance. If a
discharger/industrial user has concerns about measuring oil and grease,
the discharger/industrial user may choose to perform a side-by-side
comparison of Method 1664 and any of the approved methods that it
previously used to measure compliance with the limitation or standard
for oil and grease. For the side-by-side comparison, EPA suggests, at a
minimum, analysis of three replicates of each sample by each method on
any seven days over a minimum 30-day period, for a total of 42 analyses
(21 by the previously used method and 21 by Method 1664). For this
side-by-side comparison the laboratory should use the LLE procedure
(not the optional SPE procedure) in Method 1664 because of the possible
confounding of results that could occur when two variables (SPE and the
solvent) are changed simultaneously. EPA suggests that all six results
associated with any result less than the minimum level ( The hexadecane/stearic acid standard solution has been
diluted by a factor of 2 and twice as much standard

[[Page 26320]]

is spiked to avoid reported precipitation problems with this standard.
Instructions have been amplified to rinse all glassware
surfaces with solvent after transfer of sample or standards from one
container to another to avoid reported problems that sample and
standards cannot be recovered quantitatively.
Performance data from EPA's validation study have been
added to Section 13.
A procedure was added for drying the sample to constant
weight. The procedure was provided by the American Petroleum Institute.
The section on safety was expanded to address in greater
detail personnel monitoring and the hazards of handling n-hexane.
A requirement was added that certain pieces of equipment
such as the hot plate, centrifuge, and fume hood be specified as
explosion proof.
The QC acceptance criteria have been widened based on
EPA's validation study.
A procedure for collecting four grab samples over the
course of a day for laboratory compositing was added.
The term ``discharge'' was defined to be consistent with
the words ``discharge'' and ``matrix type'' in EPA's Streamlining
Initiative proposed on March 28, 1997 (62 FR 14976).
A suggestion for back-extraction was added to aid in
removal of salt from extracts of produced water samples to address
concerns expressed by the American Petroleum Institute.
References to the solvent removal process were changed
from ``evaporation'' to ``distillation'' to indicate that the process
recovers the solvent. Similarly, the word ``waste'' was changed to
``distillate'' to preclude indications that the distillate may be
hazardous waste.
Use of a greater amount of silica gel is now allowed so
that greater amounts of polar material can be adsorbed in the SGT-HEM
procedure, and the ratio of amount of silica gel to the amount HEM has
been clarified.
The top-loading analytical balance and centrifuge are made
optional because they may not be needed.
A limit has been placed on the amount of spiking solution
that may be added to a sample for the matrix spike and matrix spike
duplicate. The purpose of adding this limit is to preclude adding large
amounts of acetone to the sample, thus possibly allowing the spiking
material to be dissolved in the aqueous phase and not recovered in the
extraction.

VI. Public Participation and Response to Comments

The Agency proposed Method 1664 for use on January 23, 1996 (61 FR
1730). The comment period at proposal closed on March 25, 1996. On May
24, 1996 (61 FR 26149), EPA reopened the comment period for the purpose
of accepting additional data and inviting comments. The reopened
comment period closed on July 23, 1996. EPA continued to receive data
and comments after the close of the reopened comment period. Because
EPA desired to use some of these data to support the information and
decisions in today's final rule, EPA issued a notice of data
availability and request for comment on October 2, 1997 (62 FR 51621).
The comment period on the notice closed on November 3, 1997.
In the proposal and for the reopened comment period, EPA solicited
data comparing various extraction solvents, data comparing use of SPE
with the LLE procedures in Method 1664, and comments on the other
operational aspects of Method 1664. EPA is pleased with the content and
nature of the comments received. Many contained analytical data and/or
constructive comments for improvement of the Method. As a result, EPA
has modified Method 1664, where appropriate, to respond to commenters'
suggestions. Significant comments received are summarized below, along
with EPA's response. To the extent practicable, the comments have been
categorized by subject. Detailed comments and their accompanying
responses are included in the Docket for today's final rule.
EPA thanks commenters for data and constructive suggestions and
believes that the version of Method 1664 being promulgated today will
provide reliable data for compliance monitoring.

A. Regulatory Issues

Comment: Oil and grease is not a viable parameter for National
Pollutant Discharge Elimination System (NPDES) compliance and there is
no objectivity in permitting with an empirically based method.
Response: Oil and grease is a conventional pollutant designated
pursuant to section 304(a)(4) of the Federal Water Pollution Control
Act (FWPCA) and codified at 40 CFR 401.16, and therefore must be
monitored for NPDES compliance under an effluent guideline or when
deemed appropriate by a regulatory authority.
Comment: As with Method 413.1, Method 1664 measures non-oil and
grease substances such as surfactants, soaps, and emulsifiers that will
unduly subject dischargers to continual permitting and compliance
difficulties.
Response: EPA recognizes that it may be inappropriate to include
certain substances in the determination of oil and grease. However,
discharges of pollutants, including surfactants, soaps, emulsifiers,
and other substances, is prohibited under the Clean Water Act unless in
compliance with an NPDES permit. EPA has provided the SGT-HEM (NPM)
procedure in Method 1664 to allow development of effluent guidelines
and in permitting situations for those instances in which removal of
these substances is appropriate, and to allow a regulatory authority to
specify measurement of SGT-HEM for compliance monitoring.

B. Health and Safety Concerns

Comment: n-Hexane is a safety hazard compared to CFC-113. n-Hexane
has a flash point of -23 deg.C (-9 deg.F), has explosive limits in air
in the range of 1.2-6.9 percent, and poses a serious fire risk when
heated or exposed to flame. There are multiple ignition sources in a
laboratory, including Bunsen burners and high temperature furnaces.
Method 1664 should be performed in an explosion-proof hood.
Response: EPA agrees that n-hexane is comparatively more hazardous
than CFC-113. Proposed EPA Method 1664 contained explicit precautions
concerning the handling of n-hexane and the recommendation that
material safety data sheets (MSDSs) be made available to laboratory
personnel. EPA also included references to information on laboratory
safety. EPA has expanded and re-emphasized these precautions in the
version of Method 1664 being approved today.
Comment: EPA needs to modify Method 1664 to give information on the
toxicity of n-hexane and on safety precautions required for safe
handling and storage. n-Hexane is a known neurotoxin.
Response: EPA has expanded the section on safety and the health
effects of n-hexane in the version of Method 1664 being approved for
use in today's final rule.

C. Economic Concerns

Comment: Method 1664 is more complicated and more labor intensive,
requires a greater analysis time, and will be more expensive to
practice.
Response: EPA agrees that Method 1664 will require a somewhat
longer analysis time because of the increase in time required for
extraction, n-hexane evaporation, and QC. However, regulated entities
and their laboratories will benefit from lower costs for the n-

[[Page 26321]]

hexane extraction solvent because CFC-113 is becoming difficult to
obtain as well as expensive. EPA believes that any cost increases will
be small and that the benefit outweighs the cost because it will reduce
the use of ozone-depleting chlorofluorocarbons, thus protecting the
Earth's ozone layer. Further, EPA is not withdrawing allowed use of
methods that employ CFCs. If a regulated entity desires to continue use
of a Freon-based method for economic reasons, the entity may continue
to use that method.
Comment: Disadvantages of using n-hexane include: the lower density
that causes n-hexane to float on the water sample making extraction
more difficult and time consuming than with CFC-113 that sinks; the
higher water solubility of n-hexane requiring more drying agent or use
of phase-separation paper; the greater tendency to form emulsions than
CFC-113; and the higher boiling point of n-hexane requiring an
evaporation time longer than 30 minutes at 85 deg.C.
Response: EPA pointed out the disadvantages of the use of n-hexane,
including some of the disadvantages above, when EPA Method 1664 was
proposed. None of these disadvantages precludes n-hexane from being
used as the extraction solvent in Method 1664. Indeed, and as pointed
out by a commenter, n-hexane was used as the extraction solvent for oil
and grease prior to the advent of CFC-113 in laboratories that were,
undoubtedly, less well equipped to handle toxic and flammable
substances. Tests performed to date using n-hexane in Method 1664
reveal that none of the disadvantages prevent use of this solvent. EPA
agrees that the techniques in Method 1664 and the other methods that
the Agency publishes must be performed carefully in order to ensure
reliable results.

D. Solid-phase Extraction (SPE)

1. Comments Supporting Use of SPE
Comment: Many commenters stated that SPE should be a standard
procedure in Method 1664. Some suggested that SPE should be the
standard procedure and that LLE should be optional.
Response: EPA believes that LLE should remain the standard
procedure because, except for a change necessitated by the change from
CFC-113 to n-hexane, the procedures in Method 1664 are virtually
identical to procedures in existing methods, the equipment used is the
same, and because n-hexane with LLE produced results closest to results
produced by CFC-113 in EPA's Freon replacement studies.
Comment: Method 1664, as proposed, requires a demonstration of
equivalency of SPE and other method modifications on each and every
discharge. This requirement is a barrier in the way of laboratories
that receive samples from different sources and a barrier to use of
innovative technologies on a national level. EPA should allow use of
SPE and other modifications without this demonstration or should allow
nationwide application to the matrices for which applicability has been
demonstrated.
Response: EPA has allowed use of SPE without a required
demonstration of equivalency in the version of Method 1664 approved
today. However, EPA has added a note to Method 1664 that it is the
discharger's responsibility to assure that results produced are
equivalent. Nearly all permits were developed using LLE and CFC-113.
Method 1664 allows the use of SPE. However, two things change when SPE
is used: the solvent and the extraction technique. EPA is concerned
that this double change may cause a discharger to violate a permit
limit simply because the results obtained are not equivalent (i.e., SPE
may produce different results). Therefore, if there is any doubt about
SPE with n-hexane producing results significantly different from
results produced by LLE with n-hexane, dischargers and laboratories
should perform a side-by-side test to demonstrate that equivalent
results are produced.
2. Comments Expressing Concerns about the Use of SPE
Comment: Results produced by SPE and LLE are not equivalent.
Comparisons of results produced by LLE, SPE cartridge, and SPE disk in
our laboratory showed statistically significant differences on 3 of 4
discharges tested. Further, infrared (IR) spectra and gas
chromatography with a flame ionization detector (GC/FID) demonstrate
that different material is being extracted by each of the extraction
techniques.
Response: EPA has seen data that demonstrate differences and other
data that demonstrate equivalence in results produced by LLE and SPE,
and EPA has decided, based on comments and data received, that SPE
should be allowed in the version of Method 1664 approved today.
However, EPA has added the note to Method 1664 that, although SPE may
be used, it is the discharger/industrial user's responsibility to
assure that results produced using SPE are equivalent to results
produced using liquid-liquid extraction (LLE).

E. Grace Period for CFC-113

Comments: Six months is too long to allow existing stocks of CFC-
113 to be used up. Use should cease immediately. Use of CFC-113 should
be allowed until existing stocks are used up, regardless of how long it
takes. Six months is the correct period for stocks of CFC-113 to be
used up. The date of the changeover should be the first day of the
month to simplify compliance monitoring. NPDES permittees should be
given 36 months to determine if they can be compliant with the new
method. Use of Method 1664 should not be required for at least one year
after the method is approved. Method 413.1 should not be withdrawn for
at least two years after the effective date of Method 1664. The
additional time should be used to generate data and establish new
permit limits as needed.
Response: The comments on this issue are diverse but most
commenters supported a grace period for switching to Method 1664. Based
on comments received, on EPA's desire to allow existing stocks of CFC-
113 to be used up, on EPA's desire not to mandate the use of Method
1664 if a CFC-based method is specified in the permit, and on extension
of the laboratory exemption for use of CFCs until 2005, approved
methods employing CFC-113 remain approved.

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

Comment: Hexane-extractable material and silica-gel treated, n-
hexane-extractable material (SGT-HEM) should be better defined.
Response: HEM and SGT-HEM are method-defined analytes, i.e., they
are defined by the procedure used to measure them, in this case Method
1664.
Comment: When will it be necessary to perform the (SGT-HEM)
procedure for total petroleum hydrocarbons (TPH)?
Response: Monitoring of TPH (now SGT-HEM or ``non-polar material;''
NPM) is presently required in the monitoring and reporting requirements
under the Coil Coating point source category at 40 CFR 465.03(c). EPA
intends to consider allowing use of Method 1664 through subsequent
rulemaking for that category and in other categorical effluent
guidelines. In today's rulemaking, EPA is also making the SGT-HEM
procedure available to permitting authorities for instances in which
only the non-polar material component of oil and grease needs to be
monitored. The SGT-HEM procedure allows monitoring of these substances.

[[Page 26322]]

G. Detection and Quantitation

Comment: Many commenters provided MDL data.
Response: The MDLs that the commenters provided and the resulting
MLs are consistent with the range of MDLs and MLs that EPA obtained in
the Agency's MDL studies. The average (mean) of these MDLs is 2.1 mg/L
and the median is 1.4 mg/L. The pooled single-operator MDL, using the
34 MDLs listed above plus the 5 MDLs EPA reported at proposal (61 FR
1736-1737, January 23, 1996), and calculated as the root-mean-square of
the standard deviations multiplied by a student's t value of 2.33 for
234 degrees of freedom, is 2.0 mg/L. These MDLs are all equal or close
to the value of 1.4 mg/L that EPA proposed and support an ML in the
range of 5--10 mg/L. Based on EPA's data and data provided by
commenters, EPA has retained the MDL at 1.4 mg/L and the ML at 5 mg/L
for both HEM and for SGT-HEM in the version of Method 1664 approved for
use in today's final rule.
Comment: Several commenters state that estimates of detection and
quantitation in Method 1664 are one or more of the following: they
cannot be achieved; are scientifically unsound; are neither realistic
nor reproducible; are flawed; were developed in an arbitrary and
capricious manner; use an inappropriate multiplication factor; are
based on spikes into reagent water instead of wastewaters; do not
consider effluent characteristics; were developed using analytical
standards; are based on a protocol that has never been subjected to
peer review and public comment; are not representative of expected
performance by qualified laboratories; represent performance of
``expert'' or ``research-grade'' laboratories; are not a statistical
predictor of laboratory performance; and were not validated on an
interlaboratory basis.
Response: EPA disagrees that the MDLs and MLs in Method 1664 were
developed inappropriately. EPA has received nearly identical sets of
comments from many of the same industry organizations on many recent
methods that EPA has proposed for use in its wastewater programs. (See,
for examples, responses to comments in the final rules promulgating use
of Method 1613 (57 FR 31805, 62 FR 48394) and use of Method 1650 and
1653 (63 FR 18503 )). EPA responds to these comments briefly and
collectively here with the same responses provided in those comments
and responses. Responses to some of the individual issues raised by
commenters are further amplified in other responses.
EPA has used the MDL successfully for estimating the lowest level
at which a substance can be detected since 1984. The MDL procedure was
subjected to peer review when the original article on the MDL was
published in Environmental Science and Technology in 1981 (ES&T 15,
1426-1435). The MDL procedure is subjected to public comment with every
MDL that EPA publishes in test methods proposed in the Federal Register
for use in EPA programs. EPA believes that the MDL procedure is viable
and provides an estimate of the lowest concentration of an analyte that
can be detected. For Method 1664, EPA did not select the lowest or
highest MDL from the five MDL studies that EPA performed prior to
proposal; rather, the Agency selected the central value of the five
MDLs determined, and provided the rationale for this selection process
at proposal (61 FR 1736--1737). This MDL is supported by MDLs in
comments received from laboratories that do not necessarily represent
``expert'' or ``research-grade'' laboratories.
With respect to the comment on lack of interlaboratory validation
of the MDL and ML, EPA performed an interlaboratory validation of
Method 1664 at levels consistent with historical interlaboratory method
validation studies performed by EPA, ASTM, AOAC-International, the
organizations that publish Standard Methods for the Examination of
Water and Wastewater (Standard Methods), and by other organizations
that validate methods. EPA and all of these organizations have not
historically performed interlaboratory studies to estimate detection
and quantitation limits. EPA used data from multiple single laboratory
studies instead to support the MDL and ML. Commenters making this
comment did not perform interlaboratory detection limit studies to
demonstrate that EPA's estimates are flawed.
EPA will continue to examine the issues of detection and
quantitation. The Agency initiated a study recently to evaluate these
concepts and plans to involve the public on these issues.

H. Matrix Effects

Comment: Method 1664 produces severe emulsion problems. These
emulsions were not formed when using Method 413.1. Breaking these
emulsions requires additional handling, increasing the potential for
inaccuracy. Bad emulsions can never be completely broken.
Response: Section 11.3.5 of Method 1664 contains the following
suggestions for overcoming emulsions: ``stirring, filtration through
glass wool, use of solvent phase separation paper, centrifugation, use
of an ultrasonic bath with ice, addition of NaCl, or other physical
methods. Alternatively, solid-phase, continuous, or other extraction
techniques may be used to prevent emulsion formation, provided that the
requirements in Section 9.1.2 are met.''
Comment: EPA must recognize the problems that the high salt content
of produced water creates.
Response: A small amount of water may be soluble in the n-hexane
used as the extracting solvent in Method 1664. In turn, a small amount
of salt may be dissolved in the hexane/water mixture. However, after
extraction, the solution is passed through granular, anhydrous sodium
sulfate to remove all traces of water. In turn, this process should
remove the residual salt. If not, the extract can be back-extracted
with reagent water to remove all traces of residual salt. After back-
extraction, the solution can be again filtered through sodium sulfate
to remove residual traces of water.

I. Method Modifications

Comment: We endorse the concept of performance-based methods to
allow for advances in technology and reductions in the cost of analyses
and encourage EPA to continue to move in this direction.
Response: In response to this and similar requests, EPA proposed an
implementation of a performance-based measurement system (PBMS) in the
Streamlining Initiative on March 28, 1997 (62 FR 14976) and solicited
comment on an alternative PBMS approach on October 6, 1997 (62 FR
52098). The Streamlining Initiative allows modification of a reference
method so long as equivalent or superior performance can be
demonstrated. The alternative PBMS approach allows modification of a
method or use of any other method based on performance demonstrated
equal or superior to a reference method (as with Streamlining) or to a
set of data quality objectives (DQOs). The alternative PBMS approach
does not allow modification of methods for method-defined analytes,
such as oil and grease, because the analyte being measured is defined
by the method used. EPA expects to make a final determination on PBMS
for method-defined analytes in the future, as the Agency gains
experience in dealing with any potential issues, and as comments from
stakeholders on these and other PBMS approaches are received.
Comment: Please clarify the ``specific discharge'' as it relates to
``the

[[Page 26323]]

discharger must demonstrate that the modified method produces results
equivalent to those produced by Method 1664 for each specific
discharge.''
Response: Specific discharge is equivalent to ``matrix type''
defined in the regulatory language proposed in EPA's Streamlining
Initiative (62 FR 14994, March 28, 1997) and means a sample medium with
common characteristics across a given industrial subcategory. Examples
include: C-stage effluents from chlorine bleach mills in the Pulp,
Paper, and Paperboard industrial category; effluent from the continuous
casting subcategory of the Iron and Steel industrial category; publicly
owned treatment work (POTW) sludge; and in-process streams in the
Atlantic and Gulf Coast Hand-shucked Oyster Processing subcategory. For
further explanation of this definition, please see the proposed
Streamlining Initiative.
Comment: Declaring that performance-based modifications can be made
perpetuates the incorrect notion that empirically determined analytes
are not affected when the practice and manner of determining them
changes. When a protocol defines an analyte, deviation from that
protocol should not be permitted.
Response: EPA agrees with this comment, but only in part. The
commenter presumably would not argue that the result of the analysis
will be affected by the size of the funnel that contains the sodium
sulfate used for removal of residual water. In allowing modification of
Method 1664, the Agency identified and distinguished changes that would
not adversely affect method performance (and analyte measurement) from
changes that would. As a result, laboratories may modify extraction and
concentration procedures, but not allow changes to the determinative
technique (gravimetry), provided that equivalent or superior
performance of the modification is demonstrated on a reference matrix
(reagent water) and on the discharge to which the modification will be
applied. EPA believes that this middle ground is the best that can be
done to allow modifications and protect the reliability of the data
produced with a modification.

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

Comment: The relative percent difference criteria for the MS/MSD
are too stringent and do not account for natural variations in grab
samples.
Response: EPA changed the requirement for an MSD to a suggestion
but believes that the MS/MSD will work with flowing streams. In the
Phase I and Phase II studies that EPA performed in support of
development of EPA Method 1664, flowing streams were split using the
procedures given in the note in Section 8.2 of EPA Method 1664 and
provided reliable replicates for testing. For the Phase II study, the
discharge streams sampled were adjusted to provide background
concentrations of oil and grease. No difficulty was encountered
recovering spikes into these samples or achieving precise results with
replicates.
Comment: The requirement for an MS/MSD at a frequency of 10 percent
and per sample batch is excessive and unnecessarily burdensome.
Response: EPA agrees that this requirement is unnecessarily
restrictive and has reduced the frequency of the MS to 5 percent and
has changed the requirement for the MSD to a suggestion.

K. Precision and Recovery

Comment: The precision and recovery criteria are unrealistic and
will not be achievable by most laboratories.
Response: EPA believes that the difficulties in achieving the
precision and recovery criteria in EPA Method 1664 are attributable to
precipitation of hexadecane and stearic acid from the standard solution
and to failure of laboratories to adequately rinse all traces of the
standard from glassware. EPA has modified the version of EPA Method
1664 being approved today to halve the concentration of hexadecane and
stearic acid in the standard solution and require spiking twice as
much. EPA also has noted that the sample container and other surfaces
that the sample contacts must be carefully rinsed with solvent to
effect quantitative transfer of oil and grease and NPM from the sample
to the extract.

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

Comment: Changing to n-hexane may cause dischargers to exceed
permit limitations because the new method may result in higher oil and
grease values. EPA should provide guidance to permit writers and
enforcement staff for dealing with this positive bias.
Response: EPA believes that the possibility that the change in
solvent will result in non-compliance is minimal based on the results
from the Freon Replacement Studies conducted prior to proposal. If a
discharger believes that the change to n-hexane will cause false
readings of noncompliance, the discharger should discuss the situation
with the permitting authority. EPA cautions that to demonstrate that
the noncompliance is the result of the change to n-hexane alone,
comparative data must be obtained using CFC-113 and n-hexane on a
sufficient number of real-world samples and the difference must be
statistically significant. For guidance in this demonstration, the
commenter is referred to Section III.D. of this preamble and the
statistical tests for significance in reports for EPA's Phase I and
Phase II Freon Replacement studies that were included in the Docket at
proposal.
Comment: EPA's proposal to replace previously approved methods with
EPA Method 1664 is arbitrary and capricious and will render obsolete
all effluent limitation guidelines and permit limitations for oil and
grease that were based on the Freon method.
Response: First, EPA is not withdrawing the previously approved
methods in today's rulemaking. Second, as discussed earlier, EPA
believes that the use of n-hexane will generally not affect the oil and
grease results significantly and, therefore, the possibility that the
change in solvent will result in non-compliance is minimal. Third, in
studies comparing different extraction solvents for measurement of oil
and grease, and in the proposal of Method 1664, EPA acknowledged and
again acknowledges that no two extraction solvents will produce exactly
the same results for a method-defined analyte such as oil and grease.
By providing for recalculation of compliance targets based on side-by-
side data, EPA believes that the Agency has taken reasonable steps to
minimize the impact of using Method 1664 rather than the Freon method
in those cases when the difference in results may cause a non-
compliance with a permit limitation.
Comment: Two commenters stated that samples collected and analyzed
under the previously approved methods are used to determine a
discharger's compliance with local and Federal categorical limits and
that it may be appropriate for EPA to re-evaluate all of these limits.
Response: There are more than 600 industrial subcategories and
nearly all contain a limit for oil and grease. Extensive time and
expense would be required for re-evaluation of all limits in all of
these subcategories. EPA conducted side-by-side evaluations on 39
facilities in 24 industrial categories in the Phase I Freon Replacement
Study and on 25 facilities in 16 industrial categories in the Phase II
study. Based on the results from these studies, EPA does not believe
that a re-evaluation of the categorical limits is neccesary at this

[[Page 26324]]

time and supports the use of Method 1664 instead of the Freon method to
determine compliance with the categorical limits. However, EPA
periodically re-evaluates categorical effluent limitations and plans to
use Method 1664 to support this effort. Until each categorical standard
is re-evaluated, EPA has decided to allowed the continued use of the
CFC-113 methods. However, because compliance targets can be adjusted on
a case-by-case basis, EPA encourages the replacement of CFC-113 with n-
hexane consistent with EPA's efforts to reduce dependency on the use of
chlorofluorocarbons.

M. Method Validation and QC Acceptance Criteria

Comment: EPA Method 1664 was not validated properly because
inappropriate sample concentrations of 57 and 170 mg/L were used in the
Twin Cities Round-robin study (TCRR).
Response: EPA disagrees that EPA Method 1664 was validated
improperly. Laboratories that participated in the TCRR study validated
the Method at concentrations of 40 mg/L for HEM and 20 mg/L for NPM in
the initial precision and recovery (IPR) and ongoing precision and
recovery (OPR) tests, and at concentrations of 57 and 170 mg/L for
``real-world'' samples from a petroleum and non-petroleum source,
respectively. It is customary to validate analytical methods at
concentrations in the middle of the concentration range to avoid
attempting to compare results for which HEM is not detected and to
allow lowered recoveries to be measured reliably, should lowered
recoveries occur. For additional information on this issue, see the
response to comments on the detection/quantitation issue.

N. Quality Control

Comment: The QC specified in Section 9 is excessive, especially
for every discharge point.
Response: As stated elsewhere in these comment responses, the
frequency requirement for an MSD has been changed to a suggestion and
the frequency of the MS and OPR have been reduced to a minimum of 5
percent. EPA does not believe that a requirement to assess the
precision and recovery on every 20th sample is excessive.

O. Sample Collection and Preservation

Comment: EPA should add a compositing procedure to EPA Method
1664. Samples can be composited in the laboratory by collecting
individual 250-mL samples over the course of a day, pouring each 250-mL
sample into the separatory funnel, rinsing each of the four bottles
(and caps) sequentially with 30 mL of n-hexane, and using the 30 mL of
n-hexane for the extraction.
Response: EPA has added the above compositing procedure to EPA
Method 1664.
Comment: Change the temperature requirement to 4 2
deg.C with the note that a lower storage temperature may be used so
long as the sample is not frozen.
Response: EPA chose a temperature range of 0-4 deg.C to be
consistent with holding time study data and to allow storage at 0
deg.C.

P. Miscellaneous Issues

Comment: The frequency of verification of balance calibration is
excessive. One commenter suggests verification before and after every
20 samples. Another commenter suggests verification before and after
daily measurements. A third commenter suggests that calibration
verification is unnecessary. A fourth commenter suggests monthly
verification.
Response: Calibration is verified prior to the first batch,
between batches, and after the last batch. EPA does not believe that
this is excessive. (An analytical batch is between 4 and 23
measurements.)
Comment: Method ruggedness has not been established, method
validity has not been confirmed on a wide range of sample matrices, and
the method is still empirical. The method needs further review and
validation on real-world samples.
Response: Based on EPA's Phase II and method validation studies,
and data supplied by commenters, EPA believes that Method 1664 has been
adequately validated and is sufficiently rugged for its intended use.
Method 1664 will always be empirical because oil and grease and NPM are
method-defined analytes.
Comment: The flask used for collection of distillate should be
referred to as a ``distillate collection flask'' rather than a ``waste
collection flask'' because the word ``waste'' can imply hazardous
waste.
Response: EPA agrees and has changed ``waste collection flask'' to
``distillate collection flask''.
Comment: Method 1664 requires that a smaller sample volume should
be extracted when a sample contains >1000 mg/L of oil and grease.
Should the smaller volume be diluted to one liter for extraction, or
should the smaller volume be extracted without dilution?
Response: The smaller volume should be diluted to one liter so
that changes to the Method are minimized. EPA has clarified this
dilution in Method 1664.
Comment: The higher boiling point of n-hexane will cause loss of
the more volatile constituents of oil and grease and therefore produce
greater variability in results.
Response: The average amount of oil and grease determined when
using n-hexane vs CFC-113 (96%), as detailed in other responses to
comments, may be attributable to loss of some volatile constituents.
Comment: What is to be the fate of Method 418.1? Method 418.1 and
SW-846 Method 9071 should not be used if continued use of Method 413.1
is disallowed.
Response: Method 418.1 is a CFC-113/infrared (IR) method for
determination of oil and grease. Although listed in Methods for
Chemical Analysis of Water and Wastes (EPA 600/4-79-020; NTIS PB84-
128677), Method 418.1 has not been approved for use at 40 CFR Part 136.
EPA plans a collaborative study with Canada for development of an IR
method that does not use CFC-113 and may propose an IR method depending
on the outcome of that study.
A solvent change from CFC-113 to n-hexane is being made in SW-846
Method 9071. Method 1664 replaces Method 9070 as the approved SW-846
method for determination of oil and grease in water, as detailed in
section III.B of this preamble.
Comment: EPA should include a thorough discussion of oil and
grease as a ``method-defined analyte'' in the final rule so that all
stakeholders clearly understand the results generated by Method 1664.
Response: EPA explained in section V of the proposal (61 FR 1737,
January 23, 1996) that determination of oil and grease is dependent on
how the measurement is made and cited examples of biochemical oxygen
demand and total suspended solids as other method-defined analytes.
Method-defined analytes are those analytes that are defined by the
procedure used to measure them. For oil and grease, the nature and the
amount of the substances extracted from complex wastewater discharges
and then measured is determined by the extracting solvent and
technique.
Comment: Many commenters suggested that Section 11.4.4 be changed
to require solvent evaporation and desiccation to constant weight. One
commenter suggested specific wording for this change. Another commenter
suggested a desiccation time of 24 hours.
Response: Section 11.4.4 has been changed to the specific wording
suggested by the first commenter but

[[Page 26325]]

has not been modified to include a 24-hour time requirement so that
constant weight achieved in a shorter time can be considered valid.
Comment: It should be EPA's responsibility to certify each
laboratory and not the responsibility of each and every company that
uses the laboratory.
Response: EPA does not certify laboratories under the Clean Water
Act and RCRA analytical programs. The States have this responsibility.
EPA is working with the States and other interested parties under the
auspices of the National Environmental Laboratory Accreditation Program
(NELAP) to accredit laboratory auditing organizations.

VII. Regulatory Requirements

A. Executive Order 12866

Under Executive Order 12866, (58 FR 51735 (October 4, 1993)) the
Agency must determine whether a regulatory action is ``significant''
and therefore subject to OMB review and the requirements of the
Executive Order. The Order defines ``significant regulatory action'' as
one that is likely to result in a rule that may: (1) Have an annual
effect on the economy of $100 million or more or adversely affect in a
material way the economy, a sector of the economy, productivity,
competition, jobs, the environment, public health or safety, or State,
local, or tribal governments or communities; (2) create a serious
inconsistency or otherwise interfere with an action taken or planned by
another agency; (3) materially alter the budgetary impact of
entitlements, grants, user fees, or loan programs or the rights and
obligations of recipients thereof; or (4) raise novel legal or policy
issues arising out of legal mandates, the President's priorities, or
the principles set forth in the Executive Order.''
It has been determined that this rule is not a ``significant
regulatory action'' under the terms of Executive Order 12866 and is
therefore not subject to OMB review.

B. Unfunded Mandates Reform Act

Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), Pub.
L. 104-4, establishes requirements for Federal agencies to assess the
effects of their regulatory actions on State, local, and tribal
governments and the private sector. Under section 202 of the UMRA, EPA
generally must prepare a written statement, including a cost-benefit
analysis, for proposed and final rules with ``Federal mandates'' that
may result in expenditures to State, local, and tribal governments, in
the aggregate, or to the private sector, of $100 million or more in any
one year. Before promulgating an EPA rule for which a written statement
is needed, section 205 of the UMRA generally requires EPA to identify
and consider a reasonable number of regulatory alternatives and adopt
the least costly, most cost-effective or least burdensome alternative
that achieves the objectives of the rule. The provisions of section 205
do not apply when they are inconsistent with applicable law. Moreover,
section 205 allows EPA to adopt an alternative other than the least
costly, most cost-effective or least burdensome alternative if the
Administrator publishes with the final rule an explanation why that
alternative was not adopted. Before EPA establishes any regulatory
requirements that may significantly or uniquely affect small
governments, including tribal governments, it must have developed under
section 203 of UMRA a small government agency plan. The plan must
provide for notifying potentially affected small governments, enabling
officials of affected small governments to have meaningful and timely
input in the development of EPA regulatory proposals with significant
Federal intergovernmental mandates, and informing, educating, and
advising small governments on compliance with the regulatory
requirements.
Today's final rule contains no Federal mandates (under the
regulatory provisions of Title II of UMRA) for State, local, or tribal
governments or the private sector. EPA has determined that this rule
contains no regulatory requirements that might significantly or
uniquely affect small governments. This rule would impose no
enforceable duty on any State, local or Tribal governments or the
private sector, nor would it significantly or uniquely affect them.
This rule makes available an additional testing procedure which would
merely standardize the procedures when testing is otherwise required by
a regulatory agency. Therefore, today's rule is not subject to the
requirements of sections 202, 203 and 205 of UMRA.

C. Regulatory Flexibility Act

Under the Regulatory Flexibility Act (RFA), 5 U.S.C. 601 et seq.,
as amended by the Small Business Regulatory Enforcement Fairness Act
(SBREFA), EPA generally is required to conduct a regulatory flexibility
analysis describing the impact of the regulatory action on small
entities as part of rulemaking. However, under section 605(b) of the
RFA, if EPA certifies that the rule will not have a significant
economic impact on a substantial number of small entities, EPA is not
required to prepare a regulatory flexibility analysis. Pursuant to
section 605(b) of the Regulatory Flexibility Act, 5 U.S.C. 605(b), the
Administrator certifies that this rule will not have a significant
economic impact on a substantial number of small entities. This
regulation merely approves an additional testing procedure for the
measurement of oil and grease and non-polar material but does not
require its use. The new approved method uses n-hexane which has a much
lower cost than Freon-113, which is used in the currently approved
methods.

D. Paperwork Reduction Act

This rule contains no information collection requirements.
Therefore, no information collection request has been submitted to the
Office of Management and Budget (OMB) for review and approval under the
Paperwork Reduction Act of 1980, 44 U.S.C. 3501 et seq.

E. Submission to Congress and the General Accounting Office

The Congressional Review Act, 5 U.S.C. section 801 et seq., as
added by the Small Business Regulatory Enforcement Fairness Act of
1996, generally provides that before a rule may take effect, the agency
promulgating the rule must submit a rule report, which includes a copy
of the rule, to each House of the Congress and to the Comptroller
General of the United States. EPA will submit a report containing this
rule and other required information to the U.S. Senate, the U.S. House
of Representatives and the Comptroller General of the United States
prior to publication of the rule in the Federal Register. A major rule
cannot take effect until 60 days after it is published in the Federal
Register. This rule is not a ``major rule'' as defined by 5 U.S.C.
section 804(2). This rule will take effect on the effective date shown
at the beginning of this preamble.

F. National Technology Transfer and Advancement Act

Under Section 12(d) of the National Technology Transfer and
Advancement Act (NTTAA), the Agency is required to use voluntary
consensus standards in its regulatory activities unless to do so would
be inconsistent with applicable law or otherwise impractical. Voluntary
consensus standards are technical standards (e.g., materials
specifications, test methods, sampling procedures, business practices,
etc.) that are developed or adopted by voluntary consensus standards
bodies. Where

[[Page 26326]]

available and potentially applicable consensus standards are not used
by EPA, the Act requires the Agency to provide Congress, through the
Office of Management and Budget (OMB), an explanation of the reasons
for not using such standards. EPA's search of the technical literature
has revealed that there are no consensus methods for determination of
hexane extractable material (HEM) and silica gel treated hexane
extractable material (SGT-HEM), although the American Society of
Testing and Materials (ASTM) is in the process of developing an
analytical method for the determination of HEM. If ASTM or another
voluntary consensus standard body approves such a method and EPA
believes that the method is suitable for compliance monitoring and
other purposes, EPA will promulgate the method in a subsequent rule.

G. Executive Order 13045

The Executive Order, ``Protection of Children from Environmental
Health Risks and Safety Risks,'' (62 FR 19885), applies to any rule
initiated after April 21, 1997, or proposed after April 21, 1998, that:
(1) is determined to be ``economically significant'' as defined under
E.O. 12866, and (2) concerns an environmental health or safety risk
that EPA has reason to believe may have a disproportionate effect on
children. If the regulatory action meets both criteria, the Agency must
evaluate the environmental health or safety effects of the planned rule
on children, and explain why the planned regulation is preferable to
other potentially effective and reasonably feasible alternatives
considered by the Agency.
This regulation is not subject to the Executive Order because EPA
published a notice of proposed rulemaking before April 21, 1998 and
further because this is not an economically significant rule as defined
under E.O. 12866. However, EPA's policy since November 1, 1995, has
been to consistently and explicitly consider risks to infants and
children in all risk assessments generated during its decision making
process including the setting of standards to protect public health and
the environment.
EPA's Office of Water has historically considered risks to
sensitive populations (including fetuses, infants, and children) in
establishing risk assessments for setting health or safety standards.
This regulation does not involve the development of a standard to
mitigate environmental health or safety risks. This regulation instead
approves an additional analytical method for compliance monitoring.
However, because the extraction solvent used in Method 1664, n-hexane,
has been associated with neurotoxic effects, EPA investigated the
available health information to determine whether the fetus may be
adversely affected as a result of pregnant women being exposed to n-
hexane in the laboratory environment. Based on animal studies, the
available information on developmental effects does not indicate any
potential risks to the fetus due to exposure to n-hexane.

H. Executive Order 12875

Under Executive Order 12875, ``Enhancing the Intergovernmental
Partnership,'' EPA may not issue a regulation that is not required by
statute and that creates a mandate upon a State, local or tribal
government, unless the Federal government provides the funds necessary
to pay the direct compliance costs incurred by those governments, or
EPA consults with those governments. If EPA complies by consulting,
E.O. 12875 requires EPA to provide to the Office of Management and
Budget a description of the extent of EPA's prior consultation with
representatives of affected State, local and tribal governments, the
nature of their concerns, any written communications from the
governments, and a statement supporting the need to issue the
regulation. In addition, Executive Order 12875 requires EPA to develop
an effective process permitting elected officials and other
representatives of State, local and tribal governments ``to provide
meaningful and timely input in the development of regulatory proposals
containing significant unfunded mandates.''
Today's rule does not create a mandate on State, local or tribal
governments. The rule does not impose any enforceable duties on these
entities. This rule makes available an additional testing procedure
that would merely standardize the procedures when testing is otherwise
required by a regulatory agency. Accordingly, the requirements of
section 1(a) of Executive Order 12875 do not apply to this rule.

I. Executive Order 13084

Under Executive Order 13084, ``Consultation and Coordination with
Indian Tribal Governments,'' EPA may not issue a regulation that is not
required by statute, that significantly or uniquely affects the
communities of Indian tribal governments, and that imposes substantial
direct compliance costs on those communities, unless the Federal
government provides the funds necessary to pay the direct compliance
costs incurred by the tribal governments, or EPA consults with those
governments. If EPA complies by consulting, Executive Order 13084
requires EPA to provide to the Office of Management and Budget, in a
separately identified section of the preamble to the rule, a
description of the extent of EPA's prior consultation with
representatives of affected tribal governments, a summary of the nature
of their concerns, and a statement supporting the need to issue the
regulation. In addition, E.O. 13084 requires EPA to develop an
effective process permitting elected and other representatives of
Indian tribal governments ``to provide meaningful and timely input in
the development of regulatory policies on matters that significantly or
uniquely affect their communities.''
Today's rule does not significantly or uniquely affect the
communities of Indian tribal governments. Further, this rule does not
impose substantial direct compliance costs on tribal governments. This
rule makes available an additional testing procedure which would merely
standardize the procedures when testing is otherwise required by a
regulatory agency. Accordingly, the requirements of section 3(b) of
Executive Order 13084 do not apply to this rule.

List of Subjects

40 CFR Part 136

Environmental protection, Analytical methods, Incorporation by
reference, Monitoring, Reporting and recordkeeping requirements, Waste
treatment and disposal, Water pollution control.

40 CFR Part 260

Environmental protection, Administrative practice and procedure,
Analytical methods, Confidential business information, Hazardous waste,
Incorporation by reference, Reporting and recordkeeping requirements.

Dated: May 7, 1999.
Carol M. Browner,
Administrator.
For the reasons set out in the preamble, title 40, chapter I of the
Code of Federal Regulations, is amended as follows:

PART 136--GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS
OF POLLUTANTS

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

Authority: Secs. 301, 304(h), 307, and 501(a) Pub. L. 95-217, 91
Stat. 1566, et seq. (33 U.S.C. 1251, et seq.) (the Federal Water
Pollution Control Act Amendments of 1972 as amended by the Clean
Water Act of 1977.)

2. In Sec. 136.3, paragraph (a), Table IB is amended by revising
entry 41 to read as follows:

[[Page 26327]]

Sec. 136.3 Identification of test procedures.

(a) * * *
* * * * *

Table IB--List of Approved Inorganic Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
Reference (method number or page)
--------------------------------------------------------------------------------------------------------------------
Parameter, units and method STD methods 18th
EPA ^1, ³⁵ ed. ASTM USGS\2\ Other
--------------------------------------------------------------------------------------------------------------------------------------------------------

* * * * * * *
41. Oil and grease--Total 413.1.......................... 5520 B\38\
recoverable, mg/L: Gravimetric
(extraction).
Oil and grease and non-polar 1664, Rev. A...................
material, mg/L: Hexane extractable
material (HEM): n-Hexane
extraction and gravimetry\42\.
Silica gel treated HEM (SGT-HEM): 1664, Rev. A...................
Silica gel treatment and
gravimetry\42\.

* * * * * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1B Notes:
\1\ ``Methods for Chemical Analysis of Water and Wastes'', Environmental Protection Agency, Environmental Monitoring Systems Laboratory-Cincinnati (EMSL-
Ci), EPA-600/4-79-020, Revised March 1983 and 1979 where applicable.
\2\ Fishman, M.J., et al, ``Methods for Analysis of Inorganic Substances in Water and Fluvial Sediments,'' U.S. Department of the Interior, Techniques
of Water--Resource Investigations of the U.S. Geological Survey, Denver, CO, Revised 1989, unless otherwise stated.

* * * * * * *
\35\ Precision and recovery statements for the atomic absorption direct aspiration and graphite furnace methods, and for the spectrophotometric SDDC
method for arsenic are provided in Appendix D of the part titled, ``Precision and Recovery Statements for Methods for Measuring Metals.''

* * * * * * *
\38\ Only the trichlorofluoromethane extraction solvent is approved.

* * * * * * *
\42\ Method 1664, Revision A ``n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated n-Hexane Extractablke Material (SGT-HEM; Non-
polar Material) by Extraction and Gravimetry'' EPA-821-R-98-002, February 1999. Available at NTIS, PB-121949, U.S. Department of Commerce, 5285 Port
Royal, Springfield, Virginia 22161.

* * * * * * *

PART 260--HAZARDOUS WASTE MANAGEMENT SYSTEM: GENERAL

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

Authority: 42 U.S.C. 6905, 6912(a), 6921-6927, 6930, 6934, 6935,
6937, 6939, and 6974.

Subpart B--Definitions

2. Section 260.11 is amended by revising paragraph (a)(11) and by
adding paragraph (a)(16) to read as follows:

Sec. 260.11 References.

* * * * *
(a) * * *
(11) ``Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods,'' EPA Publication SW-846 [Third Edition (November 1986), as
amended by Updates I (dated July 1992), II (dated September 1994), IIA
(dated August 1993), IIB (dated January 1995), III (dated December
1996) and IIIA (dated April 1998)]. The Third Edition of SW-846 and
Updates I, II, IIA, IIB, and III (document number 955-001-00000-1) are
available from the Superintendent of Documents, U.S. Government
Printing Office, Washington, DC 20402, (202) 512-1800. Update IIIA is
available through EPA's Methods Information Communication Exchange
(MICE) Service. MICE can be contacted by phone at (703) 821-4690.
Update IIIA can also be obtained by contacting the U.S. Environmental
Protection Agency, Office of Solid Waste (5307W), OSW Methods Team, 401
M Street, SW, Washington, DC, 20460. Copies of the Third Edition and
all of its updates are also available from the National Technical
Information Service (NTIS), 5285 Port Royal Road, Springfield, VA
22161, (703) 605-6000 or (800) 553-6847. Copies may be inspected at the
Library, U.S. Environmental Protection Agency, 401 M Street, SW,
Washington, DC 20460; or at the Office of the Federal Register, 800
North Capitol Street, NW, suite 700, Washington, DC.
* * * * *
(16) Method 1664, Revision A, n-Hexane Extractable Material (HEM;
Oil and Grease) and Silica Gel Treated n-Hexane Extractable Material
(SGT-HEM; Non-polar Material) by Extraction and Gravimetry. Available
at NTIS, PB99-121949, U.S. Department of Commerce, 5285 Port Royal,
Springfield, Virginia 22161.
* * * * *
[FR Doc. 99-12163 Filed 5-13-99; 8:45 am]
BILLING CODE 6560-50-P

Visit the Official Version

Document Information

Effective Date:: 6/14/1999
Published:: 05/14/1999
Department:: Environmental Protection Agency
Entry Type:: Rule
Action:: Final rule.
Document Number:: 99-12163
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.
Pages:: 26315-26327 (13 pages)
Docket Numbers:: FRL-6341-9
RINs:: 2040-AC63: Guidelines Establishing Oil and Grease Test Procedures for the Analysis of Pollutants Under the Clean Water Act
RIN Links:: https://www.federalregister.gov/regulations/2040-AC63/guidelines-establishing-oil-and-grease-test-procedures-for-the-analysis-of-pollutants-under-the-clea
PDF File:: 99-12163.pdf
CFR: (2): 40 CFR 136.3; 40 CFR 260.11