[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
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                                            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