Monday
January 23, 1989
Part II
Environmental
Protection Agency
40 CFR Parts 260, 261, 262, 264, 265, 268
and 270
Hazardous Waste Management System;
Testing and Monitoring Activities;
Proposed Rule
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3212 Federal Registec://V^l. .54; No. ,13 /Monday. January 23.--1989/'Proposied Rules
ENVIRONMENTAL PROTECTION
AGENCY
40 CFR Parts 260,261,262,264,265,
268 and 270
[FRL-3394-4]
Hazardous Waste Management
System; Testing and Monitoring
Activities
AGENCY: Environmental Protection
Agency (EPA).
ACTION: Proppsed rule. • ,
SUMMARY: The Environmental Protection
Agency (EPA) is today proposing to
revise certain testing methods that are
approved or required under Subtitle C of
the Resource Conservation and '
Recovery Act (RCRA). EPA is also
proposing to add several new testing
methods that can be used to comply
with the requirements of Subtitle C of
RCRA. These new and revised methods
are found in the Third Edition of "Test
Methods for Evaluating Solid Waste,
Physical/Chemical Methods," SW-846
and the first update package to this
Third Edition of SW-846. The Agency is
also proposing to make specified
Quality Control (QC) procedures
mandatory for all testing conducted
under the hazardous waste regulations
of RCRA. These Quality Control
procedures are also found in the Third
edition of SW-846. Some modifications,
have also been made to Chapter One of
the manual to provide clarification of
definitions. The modified sections of
Chapter One are found in the first
update package to the Third Edition of
SW-846, which is also being proposed in
today's rule. The revisions to Chapter
One contained in this first update
package are given in Appendix A of this
proposed rule. The appendix has been
added to this proposed rule in order to
provide the public with the specific
language that will be substituted for the
language currently found in Chapter
One of the SW-848 manual. Today's
action is necessary to provide better and
more complete analytical test methods
for RCRA-related testing and to
document the quality of the data
gathered for complying with the RCRA
hazardous waste regulations. This
proposed rule will provide more reliable
analytical data and promote consistency
In the analytical test methods used for
sompliance with RCRA and the
Comprehensive Environmental
Response, Compensation, and Liability
<\ct (CERCLA).
3ATE: Comments on this proposed rule
nust be submitted on or before March 9,
1989.
ADDRESS: The public should submit an
original and two copies of their •• ,•
comments on this proposed rule,to:
Docket Number F-89-WTMP-FFFFF,
EPA RGRA Docket, OS-305 (Room SE-
205), U.S. Environmental Protection
Agency, 401M Street SW., Washington,
DC 20460. Please place Docket number
on all comments. The EPA RCRA .
Docket is located in the sub-basement at
the above address and is open from 9:00
a.m. to 4:00 p.m., Monday through
Friday, except Federal holidays. The
public must'make an appointment to
review docket materials by calling (202) •
475-9327. The public may copy 100
pages of material from any one .
regulatory docket at no cost;, additional
copies cost $0.15 per page.
Copies of the Third Edition of SW-846
and of the proposed first update to the •
Third Edition are available from the .
Government Printing office, , . ...
Superintendent of Documents,
Washington, DC 20402, (202) 783-3238. .
The document number is 955-001-00000-,
1 and the cost is $110.00 for the four-
volume set plus updates. Update • . ,
packages will be automatically mailed
to all subscribers. Non-subscribers may .:
order the proposed first update package
by calling the RCRA Hotline at (SOO)1 ;
424-9346 (toll free) or (202) 382-3006,:br
by writing the Communications and :.
Training Section, U.S. Environmental
Protection Agency, 401M Street, SW.,
Washington, DC 20460. The. requester V..
must specify the appropriate document ,
title; document number and "First , .•; :
Update Package." ' .,.'''.•"'.,
Copies of the Second Edition of SW-
846 are available.from the National
Technical Information Service (NTJS),.
5285 Port Royal Road, Springfield, VA
22161, (703) 487-4600. The document
number is PB87-120-291 and the cost is
$48.95 for paper copies and $13.50 for
microfiche. '
FOR FURTHER INFORMATION CONTACT:
For general information contact the
RCRA Hotline at (800) 424-^348 (toll
free) or (202) 382-3000. For Information
on the technical aspects of this proposed
rule contact Charles Sellers, Office of
Solid Waste, OS-331, U.S.
Environmental Protection Agency, 401 M
Street, SW., Washington, DC 20460,
(202) 382-3282. .
SUPPLEMENTARY INFORMATION:
Index
Part I. Background
Part II. Proposal
(A) Methods Substitutions
(B) Methods Format
• (C) Regulatory Status of the third Edition
(D) Quality Control
1. Field Quality Control • • '-•
2. Analytical Laboratory Quality Control
(E) Methods Inclusion and Exclusion
, Part III. State Authority .
(A) Applicability of Rules in Authorized
States
(B) Effect on State Authorization
Part IV. Economic and Regulatory Impacts
(A) Regulatory Impact Analysis
(B) Regulatory Flexibility Act
(C) Paperwork Reduction Act
I. Background
On October 1,1984 (49 FR 33786-
33812), EPA proposed several changes to
. the RCRA hazardous waste regulations.
These proposed changes included the •
following elements: •
(1) Addition of new methods to SW-
846. .
(2) Mandatory adherence to the
procedures and methods in SW-846 for
all RCRA testing.
(3) Elimination of requirements to test
for certain compounds when conducting
ground water monitoring.
(4) Use of screening tests when
monitoring ground water for hazardous
constituents.
(5) Use of the Hierarchical Analysis
Procedure for ground water screening.
Many comments were received on the
^proposal. The Agency evaluated these
comments and, as a result, decided not
to promulgate the October 1,1984,
; • proposal. 'Instead, the Agency revised
SW-846 to incorporate many of the ;
suggestions made in the^coniments and
undertook other actions to address
changes to the ground water monitoring.
regulations. On March 16,1987, EPA
announced the. availability of the Third
Edition of SW-846 in the Federal
Register (50 FR 8072). The Third Edition
contains 72 methods that are new to
SW-846. Of these, 43 will be finalized in
a soon to be released rulemaking and
will be acceptable for use, where
, required in 40 CFR Parts 260 through
270, in conjunction with, or in addition
to, the Second Edition of SW-846 as
amended by Updates I and II. These 43
methods were first proposed in the 1984
Notice of Proposed Rulemaking (NPRM),
and are not being reproposed in today's
rulemaking. However, of the remaining
methods, 28 methods not previously •
proposed for RCRA testing are being
proposed, and one other method is being
reproposed by the Agency in today's
rulemaking.
Upon review and following comments
and questions received from the public,
it was determined that several errors
existed in the manual. Comments also
indicated the need to provide additional
and improved analytical test methods
for RCRA-related testing. To alleviate
confusion arising from errors or
confusing language in the test methods,
an update package with-revisions and
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Federal Register / Vol. 54, No. 13 / Monday, January 23, 1989 /• Proposed Rules
3213
clarifications was deemed necessary.
Thus, the Agency is also proposing the
use of the first update package to the
Third Edition, along with the Third
Edition in today's rulemaking. The first
update package contains revisions to
methods in the Third Edition, asrwell as
14 methods that are new to SW-846. Of
these, four will be finalized in a soon to
be released rulemaking and will be
acceptable for use, where required in 40
CFR Parts 260 through 270, in
conjunction with, or in addition to, the
Second Edition of SW-848 as amended
by Updates I and II. These four methods
were first proposed in the 1984 NPRM,
and are not being reproposed in today's
rulemaking. However, the remaining ten
methods not previously proposed for
RCRA testing, are being proposed by the
Agency in today's rulemaking.
, Promulgation of this proposal will
allow the use of the Third Edition.as
revised by the first update package for
all testing for which the Second Edition
methods are mandated by current RCRA
regulations (see PROPOSAL, Regulatory
Status of the Third Edition} and will
mandate certain Quality Control
procedures detailed in Chapter One of
the Third Edition and revised in the first
update. '
II. Proposal .
A. Methods Substitutions
The Agency is today proposing to,
replace the S W-846 Second Edition
methods with the versions contained in
the Third Edition and the first update
package. These replacements will allow
the Third Edition as revised by the first
update to be used for all RCRA testing.
The Agency is making this substitution
because it believes that the Third
Edition and first update methods are
improvements on those in the Second
Edition. (See the Background Document
included in the docket to this proposal
for a specific discussion of these
changes and why they are
improvements.) . •
B. Methods Format
Comments on the October 1,1984,
Federal Register .proposal also indicated •
that the Second Edition method formats
.were inconsistent and difficult to follow.
The Agency agreed with these
comments, and made changes
accordingly. The methods were
reviewed by a work group composed of
technical experts from within EPA and
state hazardous waste testing programs;
One of the aims of their efforts was to
edit the text for technical clarity. The
method formats, were revised and
standardized into the following format:'
.' 1.0. Scope and Application. -
2.0 Summary.
3.0 Interferences. • '
4.0 Apparatus and Materials.
5.0 Reagents.
• 6.0 Sample Collection, Preservation,
and Handling.-.- '.:- -
7.0 Procedure. . • • , <
8.0 Quality Control.
9.0 , Method Performance.
10.0 References..
Section 9.0, Method Performance, is
new to the Manual. It contains available
method precision and accuracy data.
Such data are not available for all
methods; however, the Agency is
continuing its data gathering effort and
will provide the data as they become
available in future updates.
Comments also noted that detailed
procedures and instrument calibration
procedures were not consistent between
the EPA solid waste management
programs (i.e., RCRA and CERCLA),
even when essentially identical methods
were used. The Office of Solid Waste
(OSW), therefore, worked with the
CERCLA program to make the methods
used in the two programs as consistent
as possible. Particularly, OSW changed
standards and surrogates, calibration
procedures, and gas chromatographlc
(GC) analysis conditions of the gas
chromatographic/mass spectrometric
(GC/MS) methods.
In order to 'save space and eliminate
duplication of information, each group of
methods that applies to a specific class
of analytes or concerns a general
analytical technique (e.g., atomic
absorption spectroscopy) is preceded by
a general method that contains common
information and analytical guidance.
Thus, information is not repeated in the
detailed directions for each analyte.
The comments also contained many
requests for additional guidance on
method selection. EPA responded by
including a hew chapter in the Third
Edition. This chapter, "Choosing the
Correct Procedure," aids the analyst in
choosing appropriate methods for
samples based on sample matrix,
properties to be measured, and the .
regulations requiring the analysis. For
example, an analysis scheme is
presented for determining Appendix IX
analytes in ground water. It give advice
on suitable, cost-effective SW-846
methods for the volatile and semi-
volatile organic analytes, taking into
account the sample matrix and the >.
' regulatory requirements.
C. Regulatory Status of The Third
Edition
The hazardous waste regulations '
under Subtitle C of RCRA require that
specific testing methods described in the
Second Edition of SW-846 be employed
for certain applications. The following
sections of 40 CFR require the. use of
SW-S46 methods: ;
(1) Section 260.22(d)(l)(i)—Submission
of data in support of petitions to exclude
a waste produced at a particular facility.
(2) Section 261.22(a)—Evaluation of
wastes against the Corrosivity
Characteristic.
(3) Section 261.24(a>—Evaluation of
wastes against the Extraction-Procedure
Toxicity Characteristic.
(4) Sections 264.314(a) and
, 265.314(d)—Evaluation of wastes to
determine if free liquid is a component
of the waste. .
(5) Section 270.62(b)(2)(i}(C)—
Analysis of wastes prior to conducting a
trial burn in support of an application ;
for a hazardous waste incineration
permit... ' . ' .' '
The Agency is today proposing to
replace the Second Edition methods
with the Third Edition methods as
revised by the first update package to
.the Third Edition for the reasons
discussed previously (see" PROPOSAL,
Methods Substitutions).
D. Quality Control .
EPA is today proposing to make
selected Quality Control (QG)
procedures in Chapter One of SW-846
(specifically Sections 1.2-and 1.3 and
procedures referenced therein)
mandatory for all RCRA testing. .Chapter
One has been modified in order to
provide consistency and clarification of
definitions within the regulatory •
community as well as the SW-846 .
manual. These modifications are
contained in the first update to'the Third
Edition, also proposed in.today's rule
and- are republished in Appendix A of
this Federal Register Notice.
Appendix A has been added to this
proposed rule in order to provide the
public with the specific language that
will be substituted for the language
found in Chapter One of the Third
Edition of the SW-846 manual.
Additional information regarding the
rationale for the first update's revisions
to Chapter One proposed in today's rule
and published in Appendix A of this
Federal Register notice, is included in
the docket to this proposed rule. These
QC procedures are proposed to be
mandatory for all chemical analyses'
required under RCRA regulations
codified in 40 CFR Parts 260, 261.262,
264, 265, 268, and 270 regardless of
whether or not SW-4346 analytical •
methods are used. Thus, the QC
procedures are proposed to be •
mandatory for required RCRA analyses
under these-Parts whea SW-846 '
analytical methods are used, whether or
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3214 FederalRegister/ Vol. 54, Mo. 13 /Monday. January 23, 1989 / Proposed Rules
not use of these methods are mandatory
under the applicable RGRA regulations
and where a method other than an SW-
848 method is used. The Agency thus
intends to document the quality of data
generated to determine compliance with
the RCRA hazardous waste regulations.
EPA is proposing to mandate the QC
procedures which are contained in
Section 1.2, (which discusses field and
analytical laboratory QC), and Section
1.3 (which discusses method detection
limits), as well as the procedures
referenced in these two sections. •
The other sections of Chapter One (1.1
Introduction, 1.4 Data Reporting, 1.5
Quality Control Documentation, and 1.6
References) do not contain QC
procedures. They are included for
completeness but are offered only as
guidance. Many of the proposed
mandated QC procedures listed in
Section 1.2 and 1.3 are described more
fully in Section 8.0 of the applicable
SW-846 method located in later
chapters of the manual. For example,
while instrument calibration is
mandated in Section 1.2.2.3.2, the ,
diversity of calibration techniques
which are peculiar to specific
instruments and procedures, precludes
the incorporation of all the calibration
techniques described in the different
methods set forth in Chapters Three
through Eight and Ten of SW-846.
Therefore, the reader is referred by ,
Sections 1.2 and 1.3 to the applicable QC
procedures contained in Section 8.0 of
the applicable RCRA test method in
these chapters of SW-846. These
referenced procedures found hi Section
8.0 of each test method shall also be
mandatory when an SW-848 method is
used. When an SW-^846 method is not
used, the referenced procedures located
in Section 8.0 of the methods shall, of
course, not be mandatory, QC sections
in Chapter One, other than Sections 1.2
and 1.3 and those in 'other parts of the
manual are offered only as guidance.
The Agency's philosophy is that a QC
program must begin at the1 inception of a
project, continue through collection'and
storage of samples, include all phases of
chemical analyses, and extend through
the interpretation and compilation of
data results; Two basic concepts-used in
a QC program are to: (1) Control errors,
and (2) verify that the entire analytical
method is operating within acceptable
performance limits. Use of qualified
personnel, reliable and well-maintained
equipment, appropriate calibrations and
standards, and close supervision of all
operations are important components of
the QC system.
Some aspects of such a QC program
are to: (1) Use matrix spikes and ';
surrogates to provide a means for
generating accurate analytical data of
documented quality to determine that
the required sensitivity is being
achieved; (2) use duplicates to indicate
the existence of gross errors; (3) use
field QC to show that the sample is free
from contamination errors introduced in
sampling and handing; (4) use standard
curves and check samples to indicate
proper instrument calibration; and (5)
use detection and quantification limit
criteria to show that the method
detection limit was adequate to detect
analytes at or below a regulatory
threshold and assist in the identification
,of possible sources of error and
laboratory problems. A quality-control
program can be divided into two main
categories: (1) Field Quality Control and
(2) Laboratory Quality Control.
1. Field Quality Control
It is the intention of the Agency to
mandate the QC procedures in Section
1.2.1 of SW-846 in order to eliminate
improper sampling and handling
• techniques and, thus, minimize potential
errors that could skew data results.
Areas of concern in field QC include
sampling techniques; documentation of
pre-field, field,-and post-field activities;
and generation of QC samples such as
field duplicate samples (taken from the
same sampling point to the field), trip .
blanks, field blanks and equipment
blanks. Quality control in these areas is
necessary to document that sampling
equipment is properly calibrated,
containers are appropriately prepared,
representative samples are taken, and
proper shipping procedures are
followed.
This section of SW-846 mandates, that
documentation of compliance with the
requirements for field activities be
maintairied and made available upon
request.
2. Analytical Laboratory Quality Control
Section 1.2.2 discusses analytical
laboratory QC procedures. The QC
procedures described are intended to be
applied to all chemical analytical
procedures. The purpose of laboratory
QC is to provide information about the
quality of the data as-they are being
produced. Data quality, is usually
expressed in terms of accuracy,
precision, and detection limit of the
analytical method. Accuracy is a
measurement of the closeness of an
individual measurement, or an average
of a number of measurements to the true
value. Accuracy is generally represented
as percent recovery.
Precision is defined as a measure of
reproducibility among individual -
measurements of the same arialyte
under specified conditions. Instrument
and overall method precision are often
expressed as the coefficient of variation,
standard deviation, percent difference,
and/or relative standard deviation. The
sections on precision are currently
included in the interest of completeness.
The Agency is not seeking to mandate
the determination of precision in this
rulemaking since significant precision
data cannot be obtained from the
analysis of one replicate or duplicate as
proposed here. The Agency is soliciting
comment on appropriate ways to
determine method precision in the
sample matrix", especially when the •
number of samples in the batch is.
limited.
More accurate results may be
obtained by instituting a QC program
which demands that the degree of
variability of all operating parameters
that are under the control of the analyst
be kept within the control limits.
However, the QC system does not
ensure this. Results from QC procedures
. are used to document data quality, to
verify that the analytical system is
working well on a given matrix/analyte
combination, to indicate whether
instruments are operating properly, and
to indicate when additional sample
cleanup or other corrections need to be
made. The QC data are indicators, but
themselves do not change the quality of
the analytical data.
Table 1 contains analytical QC
requirements and their frequency of
application. It also clarifies some of the
terms used in Sections 1.2 and 1,3 of
Chapter One. The QC requirements in
Table 1 will produce qualitative and
quantitative information about the
generated data. If the QC data indicate
that any aspect of the system is out of
control, measures must be taken to bring
it back into control. The Agency is
considering including the use of control
charts in the QC requirements and
invites comments. . :
Standard:curves covering the .
analytical range of interest for
calibrating analytical instruments are
required to define the linear calibration
range which can be used for
environmental sample analyses.
GC/MS Quality Control presents
slightly expanded method-specific
requirements that are necessary to '
guarantee proper determination and
identification of the analytes. This
involves special instrument tuning,
verification of retention times, mass
spectral correlation with an authentic
standard of a particular analyte, and the
use of surrogates. These QC procedures
are found in the individual methods.
All QC data must be recorded and
maintained by the laboratory for later
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Federal Register / Vol. 54, No. 13 / Monday, January 23, 1989 / Proposed Rules
3215
verification and must be available upon request for a period of 3 years from the date the data are reported.
;.• = •: TABLE 1^QC REQUIREMENTS AND FREQUENCY OF APPLICATION
QC Parameter
Frequency
Comments
Matrix spikes
Replicates (See
Figure 1). •
Blanks..
Field duplicates
(See Figure
Check standard..
Surrogates .........
Column check
sample.
Column check
sample blank.
Standard
curves.
GC/MS ,
instrument
performance
' check. '.
One per analytical batch per matrix-or every 20 samples.
whichever is greater. . ' •> ......'..
One per analytical batch per 'matrix'or every 20 samples,
- whichever is1 greater. • :•-. ••;
One per analytical batch per matrix or every 20 samples,
whichever is greater. ' . ,
One per analytical batch per matrix or every 20 samples,
whichever is greater.
One per analytical batch or every 20 samples, whichever is
greater. "
Add prescribed surrogates to every blank, standard, sample and
QC sample. .;
One per batch of adsorbent
One per batch of adsorbent ...:..
Refer to specific method for necessary periodic calibration......;
Initial 5-point calibration is to- be verified with' a single point
calibration once every 12 hrs of instrument operation and H
the sensitivity and linearity criteria are not met, a new 5-ppint
initial calibration must be generated.
Replicate samples are separate aliquots taken from the same sample container
in the laboratory and analyzed independently. Evaluation of replicate data can
.indicate the existence of• gross errors in the analysis. In cases where
. aliquoting is impossible (i.e., volatiles), duplicate samples must be taken for
replicate analysis.
Field duplicate samples are two separate samples taken from the same
sampling point in the field (i.e., in separate containers and analyzed independ-
ently). Evaluation of duplicate data can indicate the existence of gross errors
in the sampling technique.
Only for volatile and semi-volatile organics and pesticides.
Applies to adsorbent chromatography and back extractions of organic corn-
pounds. .
Applies to adsorbent chromatography and back extractions of ,organlc com-
pounds. ••.'•.., .
As prescribed by specific methods.
Performed to meet tuning criteria of the instrument as specified in the GC/MS
methods. Organic analytes shall be checked with a 4-bromofluorobenzene
(BFB) for determination of volatiles .and with decafluorotriphenylphosphine
(DFTPP) for determination of semi-volatiles.
BILLING CODE 6560-50-M
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3216
Federal Register / VoL 54, No. 13 / Monday, January 23,1989 / Proposed Rules
SAMPLING POINT
OR
SOURCE IN THE FIELD
FIELD; DUPLICATE I
FIELQ: DUPLICATE I!
REPLICATE IA
REPLICATE IB
REPLICATE IIA
REPLICATE IIB
Figure 1. Sampling Chart for Field Duplicates and Replicates.
Collected 1n the field
Analyzed 1n the laboratory
-16-
BILUHQ CODE 4560-50-C
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Federal Register / Vol. 54, No. 13 / Monday, January 23, 1989 / Proposed Rules
3217
When the analytical data are used to
demonstrate compliance-with a
regulation, Data Quality Objective, or
other study objective, any and all values
reported as less than a specified
regulatory threshold must be verified. If,
no regulatory threshold is mandated for .
the analyte of interest, any and all
values'reported as less than the method
. detection limit must be verified. The
analyst must demonstrate the method's.
ability to detect the analyte of concern
, in the sample matrix. This is
accomplished using a "clean" sample;
for example, tint base would be a
suitable "clean" representative matrix
when testing paint waste; or upgradient
ground water (from the same aquifer) .
could be a suitable "clean"
i representative matrix when testing
monitoring well samples. • • •
EJ Methods Inclusion and Exclusion
The majority of the methods proposed
for addition to SW-846 on October 1,
1984, are included in the Third Edition of
.SW-846. Some proposed methods and
:some methods in the Second Edition are
not. included becausei problems were
encountered during their evaluation.'
Data generated by .the public and by
EPA demonstrated that the methods
could not be used in their published1
form for the purpose stated in the
method. These methods are listed in
Table 2. More detailed information can
be found in the technical support
document, which is located in the EPA
RCRA'Docket F-89-WTMP-FFFFF.,
TABLE 2.—METHODS NOT INCLUDED IN THE THIRD EDITION OF SW-846
Method
Title
Comments
1120
3560
7551
8320
8330
8410.
8411
6600
8610
8620
8630
9011
9037
Electrochemical Corrosion ....;.
Reverse Phase Cartridge Extraction.,
Osmium (AA; Furnace Technique)
Miscellaneous Compounds by HPLC
Thioureas..
Formaldehyde, Basic and Acidic Medium..
Heirarchical Analysis Protocol..*...'.................., '.
Total Aromatics by Ultraviolet Spectrpscopy..-
Total Nitrogen-Phosphorous Gas Chromatographabie. Com-
,. pounds.. " '•-.'''•.'' : "'•'.'. :. ' ,
Derivatizatioii Procedure for Appendix VIII Compounds....:......:......
Photodegradable Cyanides..........; !..'. '. *.!:
Sulfate, Gravimetric...:...... ...„..,.. :.... ......
Method not equivalent to reference method. • ,
Lack of sufficient data on column pre-treatment and conditioning, elution sequences,
elution volumes, and the effect of the loading of organic compounds on the column to
permit method to be adequately defined. , ' " . •
EPA study indicates accuracy problems. •
Np supporting data on effectiveness of cleanup procedures and HPLG to determine the
analytes. Questionable precision and accuracy.'. ' .•:'••. -\
No supporting data on effectiveness of cleanup procedures and HPLC to determine the
analytes. Questionable precision and accuracy.
Too .susceptible to interferences, for application to ground water and solid waste
matrices. ,.;•,, .
Method not sensitive enough for its intended purpose. .
Method not sensitive enough for ife intended purpose. ' ' .'•
Method not sensitive enough for its intended purpose. • '/.-'••-
Method not sensitive enough for rts intended purppse, . . *"'/'.'' • ' ';
Uncertain how test and results'relate to the environment arid the.'regulations.- • -
Precision and sensitivity not adequate, Interferencerprone and therefore not-appropriate
for environmental assay. . ,,/,.,..
The methods described in SW-846 are
not mandatory for all testing under
RCRA. Currently, only §§ 260.22(d)(l)(i),
261.22(a), 261.24(a), 264.314(c},
265.314(d), and 270.62(b)(2){i){CJ.of 40
CFR require use of SW-846 methods.
The proposed Third Edition will not
alter the current testing requirements.
The Third Edition contains 72
methods that are new to SW-846 and
are listed in Table 3. Of these, 43 will be
finalized in a soon to be released
"rulemaking, and will be acceptable for
use, where required in 40 CFR Parts 260
through 270, in conjunction with, or in-
addition to, the Second Edition of SW-
846 as amended by Updates -I and II.
, Data generated by the public and by
EPA for the 43 methods have
demonstrated that the method precision
and accuracy are adequate for the :
purpose stated. Although listed in Table
3, the Agency is not reproposing these 43
methods in today's rule. These methods
are listed in Table 3 solely to notify the
public that these methods are appearing
for the first time in the Third Edition of
SW-846. The Agency is today proposing
the remaining 29 methods found in
Table 3 for public comment/Of these 29
methods, some were extracted and
reformatted from earlier methods. For
example, some of the organic .
procedures in the Second Edition were
made up of several methods (i.e.,
separation/extraction, cleanup, and •
determinative methods). Several.of ,.
these procedures Were divided and the
component methods given individual
numbers. Thus, these methods listed in
Table 3 are not new to SW-846, but are
simply appearing independently under a
new number. Finally, one method,
. Method 9090, is being reproposed. This.
method was extensively revised since it •
was- first proposed on October 1,1984; .
The Agency seeks comment on this
revised version and, therefore, decided
to repropose this method rather than to
finalize it.
TABLE 3..—NEW METHODS INCLUDED IN THE THIRD EDITION OF SW-846
Method
0010"
0020s
0030"
1320«
1330"
3005
3500
Title
Modified Method 5 Sampling Train
Source Assessment Sampling System..
Volatile Organic Sampling Train...
Multiple Extraction Procedure
Extraction Procedure for Oily Wastes ,
Acid Disgestion of Waters for Total Recoverable or Dissolved
Metals for Analysis by Flame Atomic Absorption or ICP Spec-
troscopy.
Organic Extraction and Sample .Preparation
Comments
Stack sampling method for semi-volatile compounds.
Stack sampling method for semi-volatile compounds. . .
Stack sampling method for organic compounds.
Extraction procedure used for delisting wastes that are stabilized, encapsulated, or'
chemically fixed. • .
Extraction procedures for removal of oil or grease that may interfere with the EP test.
Provides digestion technique for dissolved metals in a water matrix.
Serves as an introduction to 35XX series methods dealing wjih quantitative extraction of
volatile and semivolatile organic compounds from various sa-nple matrices.
-------
3218
Federal Register / Vol. 54, No.'13 / Monday, January 23, 1989'/Proposed Rofes
TABtE 3.—NEW MiETHODS INCLUDED IWTHE TfHffiO EDITION' OF SW-84&—Continued1
Method
Title
Comments
3580
3600
3610"
3611*
3620*
3630*
3640*
36SO«
3660
3810
3820
5040*
6010*
7000
7028
7090*
709t»
7140
7198*
7200
7201
7310*
7380"
7450
7460"
7480
748t
7550
7770*
7840"
7841*
7870
7910*
7911*
7950*
8000
8280
0012
8022*
8035"
9036*
9038*
9041
9045
9050
9060*
9065*
9066*
9067*
9070*
9071*
9080*
9081*
9090*
9100*
3131*
9232*
9200*
9250*
9251*
9252*
9310*
9315*
9320*
Waste Dilution...
Alumina Column Cleanup..-
Alumina Column Cleanup and Separation of Petroleum Wastes....
Ftorisir Cokimn Cleanup..................... i,
Silica Gel Cleanup...
Gel-Permeation Cleanup
Actd-Baso Partition Cleanup
Sulfur Cleanup.....
Hcadspace
Hexadecane Extraction and Screening of Purgeable Organics ........
Protocol for Analysis of Sorbent Cartridges- from Volatile Organic
SampHng Train.
Inductively Coupled* Plasma Atomic Emission Speetroscopy ............
Atomic Absorption Methods ................. ».....»..»«.......» ..... . ..... ...... ...... «.
Afumkiura (AA, Direct Aspiration}...- ......................... . __________ ............ .
Beryllium (AA, Direct' Aspiration).. ....... _ ..... „. ....... _ ...... ..„ ................ ....
BofyWunr. (AA, Furnace Technique}-. ______________ ....... ---------- . ......... .-.,
Calcium (AA, Direct Aspiration) ....... » ____ ...... .......... . ..... «.« .................. ,
Chromium, Hexavatent (Differential: Pulse Polargraphy) .............. ......
Cobalt (AA, Direct Aspiration)...... ............. ~ ...... -» .................... . ......... -.
Cobalt (AA, Furnace Technique)-. ------------------ .......... - ................ .....
Copper (AA, Direct Aspiration)- ..... ______ .................... ; ............ _ ..............
Iron (AA, Direct Aspiration) ....................................... »..„ ...................... .
Magnesium (AA, Direct Aspiration) ........................................... „ ......... ,
Manganese (AA, Direct Aspiration)'. ......... „ ...........................................
Molybdenum (AA, Direct Aspiration)-. [[[
Melybdenum- (A*, Furnace Technique) ._ ............................................ ,
Osmium (AA, Direct Aspiration) ..................................... .. ............ .• ________
Potassium- (AA, Direct Aspiration).: [[[
Sodium (AA\ Direct Aspiration) ................................................ . .............
Thallium (AA, Direct Aspiration) ............... .*. ..........................................
Thaltkim (AAv Ftirnaes Technique). -------- .
Tin. (AA, Direct AsplrationJ. ___ -•_.. ..... .
Vanadium (AA, Direct Aspiration) —
Vanadium (AA, Furnace' Technique)-. .......... _,...
SBC (AA, Direct AspfraHonr
The Analysis of Polychlorihafed Dibenzo-fHjioxins and Pojychlo-
rtnatect Dfbtnzorurans.
Total tnd Amenable Cyanidea ..„._... ...... _....„ ............. _ ....... ........ ......
Tola! Organic Halides (TOX>by Neutron Activation Analysis ._ _______
'
Eutfate-.
pH Paper Method.
SotlpH~ „ „ „
Specific Conductenca— '.
Phenolics.™
Total Recoverable Oil and Grease ..... -------- ..................
Oil and Grease Extraction Method (or Sludge Samples
Cation-Exchange Capacity of Soite. ------ . ------- ....... — ..
Cation-Exchange Capacity, of Soils -------------- ......... -------
Compatability Test for Wastes and Membrane Liners ....... ........ . ......
Saturated Hydraulic Conductivity* Saturated. Leachate Conductivi-
ty, and Intrinsic Permeabilty. .
Conform.
Coliform.
Nitrate....
Chloride
Solvent dilutions procedure foe npnaqueous waste samples nonaqueous. waste, samples,
prior to cleanup and/or analysis.
Serves as an introduction to 36XX series methods which diminish, or eliminate extrane-
ous materials from the waste sample.
Separation of analytes of a narrow polority range from interfering peaks of a different
polarity. .
Prowes a cleanup technique- for oily matrices.. Proposed) as. Method 3570..
Separation of analytes of a narrow polarity range from interfe'rihg peafcs of a different
polarity. :
Separation- of analytes of a narrow polarity range tern interfering peaks of a different
polarity. ,
Separation of high molecular weight material from sample analytes.
Separation of base/neutral organic extractable fraction from the acid organic extractable
fraction.. .
Elimination of sulfur (which may cause peaks) from sample extracts.
Formerly Second Edition Method 5020. It is now approved only as a screening
technique because of- problems with precision and. accuracy; •
Qualitative screening procedure for use with purge-and-trap GC or GC/MS.
Provides quantitative analysis method following VOST colleetiort. Proposed- as; Method
3720; . • • ; '
General method for multiple element determination.
Serves as an introduction to 7XXX series methods dealing with quantitative analysis, of
metals. .
Flame AA method: . :
Flame AA method.
Graphite fumaee AA method. •• i •
Flame AA metthod. ' .
Differential1 pulse polarogyap'ny method'. ,
Flame AA method. •
Graphite fumaee XvA methodl
Rame AA method,
Rame AA metliod.
Flame AA method.
Rame AA .method;
Frame AA method; '
Graphite furnace /tA method: '
Flame- AA method.
Flame AA method.
Flame AA method. ,
Flame AA method. , • •
Graphite furnace AA method.'
Flame -AA metbod;.
Flame AA method..
Graphite furnace AV\ method:
Flame.- AA method;.
Serves, as an- jntredueiipr* to' 8KXX series methods stealing wife quantaa«\» analysfe of
organic analytes.
Betermination of tetra-penta-,, hepta-, hexay,. and octachlorinated iSbenzo-p-dteina
(peDDs)-and dibenzofurans. (PCDFs) in chemical wastes.
Automated quantitative analytical method.
Neutron activation adds alternate' analytical technique. ,
Automated «hloranilata colorimetnG method,
Automated methyHhymbl blue, autoanalyzer II colorimetric method-
Turbidirnetfic method.
Paper method' adds alternate analytical technique
Analytical' technique- to> determine p'H in solid; matrices.
Analytical techniqiie to, determine conductivity.
Infrared determination of carbon, dioxide.
Manual; *-AAP with distillation spectrophotdmetric method;
Automated 4-AAP' with-' distillation1 spectrophotometie method;
MBTH: vniih, distillation sp8ctrop}ioionnetric method •
Total oil and grease for liquids. Gravimetric, separatory funnel extraction.
Total oil and grease for solids.
So* Hnef evaluation using iammonium aeetate.
Soil liner evaluation using, sodium acetate.,
U'ner compatability test for flexible membrane liners.
General' methods- for- hydraulic conductivity and liner psaneabHity. -
Mullipla tube fermentation technique. ,
IMembrane filter, technique; "
Chorida :.
Chotidtt,
Gross Alpha and-Bete-.
Alpha-Emitting Radium Isotopes...;....'.. — _ —•_..
Radtum-228 « « « « -
Aotomated^ferricyanide autoanalyzer l-colorimetrie mschod:
Automated* ferricyanide autoanalyzer II colorimetric method.
Mercune nitrate1 titrtmetric method;
Senoral. radioactivity method., .
Total radium meth-pk ' ! . • '
Radium 228 method.
•Those methods, wilt be- finalized in a soon to- be teleasedi ratemakiirg, and, thus, are not being proposed in today's rule. They are, however, new to the- Third
EditSon oJ SW-846. ' ^
> Tnosa methods were formerly sections within the SOOO method series in the Second Edition of SW-846.
«.This method was formerly Method 3530 in the Second Edition of SW-846. . . .
-------
3219
Information on method precision,
accuracy and a more detailed
explanation of the Agency's, rationale
for the deletions and inclusions listed in
Tables 2 and 3 can be found in the
Technical Support Document, which is
located in the EPA RCRA Docket F-89-
WTMP-FFFFF.
Guidance methods issued by EPA on
July 12,1985, for the determination of
reactive cyanides and sulfides in wastes
have been included in the Third Edition
for the convenience of persons
evaluating wastes. These methods may
be used for assessing whether a waste is
a reactive waste by reason of toxic gas
generation (reactivity), pending
development and proposal of more
accurate tests.
Table 4 summarizes the revisions
included in the first update for the Third
Edition of the methods manual and '
proposed today for public comment.
These revised methods are being issued
to subscribers in the first update
package. More detailed information on
these changes can be found in the
Technical Support Document available
in the RCRA docket.
TABLE 4.—REVISIONS INCLUDED IN UPDATE t, SW-846, THIRD EDITION
Method
Chapter 1 .„
Chapter 2 .. .. . • .
Chapter 4 . .
Chapter 7 ,
1310— EP TOX Test Method „.;
1330 — Extraction Procedure for Oily Wastes _ „
3005 — Acid Digestion of Waters (or Total Recoverable or Dissolved
Metals for Analysis by FLAA or ICP.
3010 — Acid Digestion of Aqueous Samples and Extracts for Total
Metals for Analysis by FLAA or ICP.
3020— Acid Digestion of Aqueous Samples and Extracts for Total
Metals for Analysis by GFAA.
3050— Acid Digestion of Sediments, Sludges, and Soils
3510 — Separatory Funnel Liquid-Liquid Extraction _ :
3520— Continuous Liquid-Liquid Extraction ._. .'.
3540— Soxhlet Extraction- '_. - _ . „ „
3600 — Cleanup _^ ._ „ . •
3650— Acid-Base Partition Cleanup _ „
5030 — Purge-and-Trap ._ ... _.-. _
6010— Inductively Coupled Plasma Atomic Emission Spectroscopy
7000— Atomic Absorption Methods. _ ..._ „ _'
7061— Arsenic (AA, Gaseous Hydride)......
7196— Chromium, Hexavalent (Cotorimetric) „ „.
7760— Silver (AA, Direct Aspiration)
8000 — Gas Chromatography „...„.„..„....„ „ „.
8010— Halogenated Volatile Organics
8015 — Non-halogenated Volatile Organics „ . „
8030 — Acrolein, Acrylonitrile, Acetonitrile
8040— Phenols..: _ :
81 20— Chlorinated Hydrocarbons .
8150— Chlorinated Herbicides „ .-.
8240— GO/MS for Volatile Organics „... .....'..„.
8250— GC/MS for Semivolatile Organics: Packed Column Tech-
nique.
8270— GC/MS for Semivolafile Organics; CapBlary Column
9010— Total and Amenable Cyanide _ „_ „
9030— Acid-Soluble and Acid-Insoluble Sulfides _ .....
9090 — Compatibility Test for Wastes and Membrane Liners
Indication of change
Partial revision . ....
.do
„.;. do -
do
do .__..
do _
......do .....v
... do ... ..
do
.... do
do
... do
do
do
Total Revision
Total Revision
.. do ._..._ - . .
do
Partial Revision "'
.... do-
do '
do .
do _ _
do ...
do
•„. do . _ _
.... do .
do ...
Total Revision . .
do..~ _
. • . • Reason for change
Clarification of the definitions
additions and deletions to analyte lists.
Change in soil/sediment and concentrated waste holding time
Revision and clarification of reactive cyanide procedure.
Addition of reference to Chapter 7.
Revision to procedure and calculation formula.
Revision to list of applicable metals; clarification of appropriate
determinative procedure.
Revision to list of applicable . metals* clarification of procedure
Revision to fist of 'applicable methods.
Do
Clarification In procedure.
Clarification in procedure.
Clarification specifies cycles/hr
•Clarification in procedure •
Clarification irt procedure* addition of Table of Anatytes.
errors. ,
Deletion of non-applicable steps; addition of metals.
Revision of quality control procedures.
Revision of calibration standard and spike concentration.
Revision of calculation formula.
Deletion of analytes f rorri Table 1 ; clarification H*r procedure.
POL1 listed for all matrices
Deletion of analytes from Table 1 .
Addition of waste preparation step* addition of operational param-
eters; correction of errors.
Addition of other operational parameters; additional solvents for
. waste; correction of errors. • " .
Text correction in matrix spikes.
Addition of other operational parameters; correction of errors.
Addition of semi-quantitative • method for acid insoluble sulfides;
additional performance data.
1 Practical Quantitation Limit.
The first update to the Third Edition
contains 14 methods that are new to
SW-846 |nd are listed in Table 5. Of
these, foufi will be finalized in a soon to
be releasffl rulemaking, and will be
acceptabj|rfor use, where required in 40
CFR Paulf 260 through 270, in
conjundpm with, or in addition to, the
SeconePEdition of SW-846 as amended
,by Updates I and II. Although listed in
Table 5, the Agency is not reproposing
these four methods in today's rule.
These methods are listed in Table 5
solely to notify the public that these
methods are appearing for the first time
in the Third Edition of SW-846. The
Agency is today proposing the
remaining ten methods found in Table 5
for public comment. These new methods
are being issued to subscribers in the
first update package. More detailed
information on these new methods can
be found in the Technical Support
Document available in the RCRA
docket.
-------
3220
Federal Register / Vol. 54, No. 13 / Monday, January 23, 1989 / Proposed Rules
TABLE 5.—NEW METHODS INCLUDED IN UPDATE I, SW-846, THIRD EDITION
Method
Reason for inclusion
••7081—Barium (AA. furnace technique)
•7211—Coppaf (AA, fumaca technique) »•
•7381—Iron (AA. fumaco technique)
7430—UthkMTi (AA, direct aspiration) •
•7461—Manganesa (AA, furnace technique) >.
"7761—Silver (AA, furnace technique)
7780—Strontium (AA, direct aspiration) .- '. •• -
•7S51—Zinc (AA, furnace technique) <•••
8011—1,2-Dibromoothans and 1,2-Dtt>romo-3-chloropropane in Water by Micro-
extraction and Gas Chromatography.
8021—Violates In Water by Purge and Trap Capillary Column GO with PID and
ELCD hi Series. .
6070—Nitrosamlnes :
8110-Hatoethers.,. ~ •-•• ••
8141—Orflanophosphorus Pesticides -
8260—GC/MS for Volatile) Organfcs: Capillary Column Technique
8021—Purgeabte Organic HalWes
8031-ExtractaWe Sulfkjes .......
Provides lower detection limit and analytical flexibility. '
Provides lower detection limit and analytical flexibility.
Provides lower detection limit and analytical flexibility.
No previous determinative method; needed to support incineration regulations.
Provides lower detection limit and analytical flexibility.
Provides lower detection limit and analytical flexibility.
No previous determinative method.
Provides lower detection limit and analytical, flexibility.
Determines compounds not listed in any other SW-846 method. '
Offers lower detection limit and improved resolution; allows concurrent analysis of
aromaties and halocarbons. -
No previous determinative method. ' .
No previous 'determinative method.
Capillary column technique; additional performance data for soil samples.
Determines volatile organics using GC/MS capillary (as opposed to packed)
column technique.
Provides quick screening procedure; eliminates need for carbon adsorption.
Includes additional matrices. •
•Thesa methods will be finalized in a soon to be released rulemaking. They are, however, being ^submitted to subscribersi for thefirst timein this update.
"These methods were finalized in the Second Edition of SW-846. They were inadvertently omitted from the Third Edition and are not being proposed as new.
III. State Authority
A. Applicability of Rules in Authorized
States
Under section 3006 of RCRA, EPA
may authorize qualified States to
administer and enforce the RCRA
program within the State. (See 40 CFR
Part 271 for the standards and
requirements for authorization.)
Following authorization, EPA retains
enforcement authority under sections •
3008, 7003 and 3013 of RCRA,-although
authorized States have primary
enforcement responsibility.
Prior to the Hazardous and Solid
Waste Amendments of 1984 [HSWA), a
State with final authorization
administered its hazardous waste
program entirely in lieu of EPA.
administering the Federal program in
that State. The Federal requirements no
longer applied in the authorized State,
and EPA could not issue permits for any
facilities in the State which the State
was authorized to permit. When new,
more stringent Federal requirements
were promulgated or enacted, the State
was obliged to enact equivalent
authority within specified time frames.
New Federal requirements did not take
effect in an authorized State until the
Slate adopted the requirements as State
law.
In contrast, under section 3006(g) of
RCRA, 42 U.S.C. 6926(g), new
requirements and prohibitions imposed
by the HSWA take effect in authorized
States at the same time that they take
effect in nonauthorized States. EPA is
directed to carry out those requirements
and prohibitions in authorized States,
including the issuance of permits, until
the State is granted authorization to do
so. While States must still adopt
HSWA-related provisions as State law
to retain final authorization, the HSWA
applies in authorized States in the
interim. . .
B. Effect on State Authorizations
Today's rule proposes standards that
would not be effective in authorized
States since the requirements would not
be imposed pursuant to the Hazardous
and Solid Waste Amendments of 1984.
Thus, the requirements will be
applicable only in those States that do
not have interim of final authorization.
In authorized States, the requirements
will not be applicable until the State
revises.its program .to adopt equivalent
requirements under State law.
40 CFR 271.21(e)(2) requires that
States that have final authorization must
modify their programs to reflect Federal
program changes and must subsequently
submit the modifications to EPA for
approval. The deadline by which the
State must modify its program to adopt
this proposed regulation will be
determined by the date of promulgation
of the final rule in accordance with
§ 271.21(e). These deadlines can be
extended in certain cases (40 CFR
271.21(e)(3)). Once EPA approves the
modification, the State requirements
become Subtitle C RCRA requirements.
States with authorized RCRA
programs may already have
requirements similar to those in today's-
rule. These State regulations have not
been assessed against the Federal
regulations being proposed today to
determine whether they meet the tests
for authorization. Thus, a State is not
authorized to carry out these
requirements in lieu of EPA until the
State program modification is submitted
to EPA and approved. Of course, States
with existing standards may continue to
administer and enforce their standards
as a matter of State law.
- States that submit their official
application for final authorization Jess
than 12 months after the effective date
of these standards are not required to
include standards equivalent to these
standards in their application. However,
the State must modify its program by the
deadlines set forth in § 271.21(e). States
, that submit official applications for final
authorization 12 months after the ;
effective date of those standards must
include standards equivalent to these
standards in their application. 40 CFR
271.3 sets forth the requirements a State
must meet when submitting its final
authorization application.
IV. Economic and Regulatory Impacts
A. Regulatory-Impact Analysis
Under Executive -Order 12291, EPA
must determine whether a regulation is
"Major", and, therefore, subject to the
requirement of a Regulatory Impact
Analysis. The total additional
annualized cost for substituting the
Second Edition of SW-846 with the
Third Edition of,SW-846 and for
mandating specified Quality Control -
procedures for all testing conducted
under the hazardous waste
identification and management
regulation of RCRA has been
conservatively estimated at $60 million,
'which is well below the $100 million that
constitutes a major regulation. EPA has.
also determined that this proposed rule
will not cause a major increase in
prices, and will not have a significant
adverse effect on competition or the
ability of U.S. enterprises to compete
with foreign enterprises. Increased costs
*;
-------
13 ^ opda'an"ary 23' 1989 ^ Proposed Rules
3221.
could result from the minimal additional
quality control compliance and
recordkeeping involved in implementing
this proposed rule. Since the procedures
mandated by these rules are those
already performed by reputable
laboratories, few laboratories are likely
to be significantly impacted by this rule.
Detailed information on the costs of the
proposal and a brief regulatory impact
analysis can be found in the background
document located in EPA RCRA Docket
F-89-WTMP^FFFFF.
B. Regulatory Flexibility Act
Pursuant to the Regulatory Flexibility
Act (5 U.S.C. 601-6*2, Pub. L. 96-354,
September 19,1880), whenever an
agency is required to publish a general
notice of rulemaking for any proposed or
final rule, it must prepare and make
available for public comment a
regulatory flexibility analysis (RFA) that
describes 'the impact of the rule on small
entities (i.e., small businesses, small
organizations, and small governmental
jurisdictions}. No regulatory flexibility
analysis is required, however, if the
head of the agency certifies that the rule
will have a significant impact on a
substantial number of small entities.
This rule will not require the purchase
of new instruments or equipment. The
proposed Quality Control is basic and
the Agency believes that most
laboratories have already implemented
the use of these QC procedures. The
regulation requires no new reports
beyond those now required. The
analytical techniques approved here can
either be handled by small facilities, or
are widely "available by contract at a
reasonable price. EPA is certifying that
this proposed rule, if promulgated, will
not have a significant economic impact
on a substantial number of small entities
(as defined by the RFA). Thus, the
proposed regulation does not require a ,
RFA. Therefore, in accordance with 5
U.S.C. 605(b), I hereby certify that 1his
rule will nqt have a significant adverse
economic impact on a substantial
number of small facilities.
C. Paperwork Reduction Act
, The information collection
requirements in this proposed rule have
been submitted for approval to the
Office of Management and Budget
(OMB) under the Paperwork Reduction
Act, 44U,S.G. 3501 et seq. An
Information Collection Request
document has been prepared by EPA
(ICR No. 1485) and a copy may be •
obtained from Richard Westlund,
Information Policy Branch, PM-223, U.S^
Environmental Protection Agency, 401M
St., SW.» Washington, DC 20460, or by
calling (202) 382-2745.
Public reporting burden-for this
collection of information is estimated to
average 0.5 hour per response, including
time for reviewing instructions,
searching existing data sources, •
gathering and maintaining the data
needed, and completing and reviewing
the collection of information.
Send comments regarding the burden
estimate or any other aspect of this
collection of information, including
suggestions for reducing this burden, to
Chief, Information Policy Branch, PM-
223, U.S. Environmental Protection
Agency, 401 M St., SW., Washington, DC
20460; and to the Office of Information
and Regulatory Affairs, Office of
Management and Budget, Washington,
DC 20503, marked "Attention: Desk
Officer for EPA." The final rule will
respond to any OMB or public
• comments on the information collection
requirements contained in this proposal.
List of Subjects in 40 CFR Parts 260,261,
262,264,265,268, and 270
Chemical, physical and biological
treatment. General facility standards,
Ground water monitoring, Hazardous
waste, Hazardous waste incinerator
permits, Incinerators, Intergovernmental
regulations, Interim status standards for
owners and operators, of hazardous
waste treatment facilities, Landfills,
Land treatment. Reporting and
reeordkeeping requirements, Storage
and disposal facilities, Surface
impoundment, Thermal treatment,
Waste piles, Waste treatment and
disposal. , .
Dated: December 14,1988. •
Lee M. Thomas,
Administrator.
For the reasons set out in the
.preamble, it is proposed that Chapter I- •
of Title 40 of the Code of Federal
Regulations be amended as follows: ,.' .
PART 260—HAZARDOUS WASTE
MANAGEMENT SYSTEM: GENERAL
The authority citation for Part 260
continues to read as follows:
Authority: 42 U.S.G. 6905,6912(a), 6921
through 6927, 6930, 6934, 6935, 6937, 6938,
6939, and 6974.
Subpart A—General
2. Section 260.1 is amended by adding
(c) to read as follows .-
§280.1
*',*-
(c) In all cases, the sampling and
analytical determinations performed to
meet the requirements of Part 260 must
• comply with the quality control'
procedures specified in Sections 1.2 and
1.3, and, where an SW-846 method is
used, the additional procedures set forth
in Section 8.0 of the methods contained
in Chapters Three through Eight and Ten
which are referenced therein, of Chapter
One of "Test Methods for Evaluating
Solid Waste, Physical/Chemical
Methods", EPA Publication SW-846, as
incorporated by reference in § 260.11.
These quality control procedures must
be followed when using any SW-^46
method, whether mandatory or not
mandatory, and when using any other .
analytical method.
Subpart B—Definitions
3. Section 260.11 is amended by
revising the fourth reference in
paragraph (a) to read as follows:
§260.11 References
(a) * * * "Test Methods for Evaluating
Solid Waste, Physical/Chemical
Methods", EPA Publication SW-846,
Third EditiOnf 1987, as amended by
Update I. This document is available as
document number 955-001-00000-1 from
the Superintendent of Documents, U.S.
Government Printing Office,
Washington, DC 20402, (202) 783-3238,
on a subscription basis. Future updates
will automatically be mailed to the
. subscriber. •
Subpart C—Rtitentakirtg Petitions
4. Section 260.22 is amended by
adding paragraph (a)(3) to read as
follows: . . . .
§ 260.22 Petitions to amend Part 261 to
exclude a waste produced at a particular
facility.
(a)***
(3) Information submitted under
paragraphs, (a) (1) and (2) of this section
must be based on appropriate test :
methods prescribed in Appendix III of
Part 261. The test methods must follow
the quality control procedures specified
.in Sections 1.2 and 1.3, and procedures
set forth in Section 8.0 of the methods
contained in Chapters Three through
Eight and Ten which are referenced
therein, of Chapter One of "Test ,-
Methods for. Evaluating Solid Waste,
Physical/Chemical Methods", EPA
Publication SW-846, as incorporated by
reference,in §.260.11. The testing and
quality control requiremesats of this
section also apply to § 260.22 (b), (c), (d),
and (e) below.
-------
3222
Federal Register / Vol. 54, No. 13 / Monday, January 23. 1989 / Proposed-jgules^
PART 261—IDENTIF1CATION AND
LISTING OF HAZARDOUS WASTE
5. The authority citation for Part 261
continues to read as follows:
Authority: 42 U.S.C. 6905, 6912(a), 6921. ahd
C922.
Subpart A— General
6. Section 281.1 is amended by adding
paragraph (d) to read as follows:
§ 262.1 Purpose and scope.
(d) In all cases, the sampling and
analytical determinations performed to
meet the requirements of Part 261 must
comply with the quality control
procedures specified in Section 1.2 and
1.3 and, when an SW-846 method is
used, those procedures set forth in -
Section 8.0 of the methods contained in
Chapters Three through Eight and Ten
which are referenced therein, of Chapter
One of "Test Methods for Evaluating
Solid Waste, Physical/Chemical
Methods", EPA Publication SW-846, as
Incorporated by reference in § 260.11.
These quality control procedures must
be followed when using any SW-846
method, whether mandatory or not
mandatory, and when using any other
analytical methods.
Appendices
7. Appendix III of Part 261 is revised
to read as follows:
Appendix HI — Chemical Analysis Test
Methods
Tables 1, 2, and 3 specify the appropriate
analytical procedures described in "Test
Methods Tor Evaluating Solid Waste,
Physical/Chemical Methods", incorporated
by reference in § 260.11 that shall be used to
determine whether a sample contains a given
Appendix VII or VIII toxic constituent
Tublo 1 identifies each Appendix VII or
VJ11 organic constituent along with the
approved measurement method. Table 2
identifies the corresponding methods for
inorganic species. Table 3 summarizes the
contents of SW-840 and supplies the specific
section and method number for sampling and
analysis methods.
Prior to final sampling and analysis method
selection, the analyst should consult the
specific section or method described in SW-
840 for additional guidance on which of the
approved methods should be employed for a
specific sample analysis situation. In all
cases, the sampling and analytical
determinations must comply with quality
control procedures specified in Sections 1.2 ,
and 1.3, and those procedures set forth in
Section 8.0 of the methods contained in
Chapters Three through Eight and Ten which
are referenced therein, of Chapter One of
"Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods"; EPA
Publication SW-8-16, incorporated by
reference in § 260.11.
These quality control procedures must be
followed when using any SW-846 method,
whether mandatory or not mandatory, and
when using any other analytical method.
TABLE 1.— ANALYSIS METHODS FOR OR-
GANIC CHEMICALS CONTAINED IN SW-
846 -
Compound
Acetonltrile -
Acetophenone
Acrolein .'.
Aldrin
4-Aminobipheny)
Benzal chloride
Benzene : ....
Benzo(j)fluoranthene.....
Benzyl chloride ;
Bis(2-chloroethoxy)methane........
Bis(2-ch!oroethyl)ether .'. ,
Bis(2-chloroisopropyl)ether
4-Bromophenyl phenyl ether .......
' Chlorinated dibenzo-p-dloxins
Chlorinated dibenzofurans :
Chlorobenzene
2-ChtoroethyI vinyl ether
Chloromethane
Chloromethylmethyl ether
2-Chloronaphthalene
Cresol(s)
Creyslic acid(s)
4 4'-DDE
4 4'-DDT
Dibenz(a h)acridin0
Dibenz(a,j)acn'dine
Dibenz(a.h)anthracene
7H-Dibenzo(c,g)carbazole.....
Dibenzo(a,h) pyrene •.
Dl-n-butylphthalate
Dich!orobenzene(s)
Methodfs)
8030, 8240
8250, 8270 .
8030, 8240
8015 . ,
8030, 8240
8080, 8250, 8270
8250,8270
8250, 8270
8120
8020, 8021, 8240,
8260
8250, 8270
8100, 8250, 8270,
8310
8100, 8250, 8270,
8310
8100
8100, 8250, 8270,
8310
8120
8010, 8120, 8240
8010,8110,8250,
8270
8110,8250,8270
8010,8110,8250,
8270
8060, 8250, 8270
8010,8021,8240,
8260
8110,8250,8270
8250, 8270
8240
8010, 8021, 8240,
8260
8080, 8250, 8270
8080
8280
8280
8250, 8270
8010. 8020, 8021,
8240, 8260
8010,8240
8010,8021,8240,
8260
8010, 8021, 8240,
8260
8010
8120,8250,8270
8040, 8250, 8270
8100, 8250, 8270,
8310
8100, 8250, 8270
8040
8040. 8250, 8270
8150
8080, 8250, 8270
8080, 8250, 8270
8080, 8250, 8270
8100
8100, 8250, 8270
8100, 8250. 8270,
8310
8100
8100, 8270
8100
8100
8060, 8250, 8270
8010, 8020, 8021,
8120,8220,
8250, 8260
8250, 8270
TABLE 1.— ANALYSIS METHODS FOR OR-
GANIC CHEMICALS CONTAINED: IN §W-
846— Continued
Compound
Dichlorodifluoromethane
Dichloroethane(s)1...,
1,1-Dichloroethylene
1,2-bichloroethylene.....
Dichloromethane...;
2,6-Dlchlorophenol
1 ,2-Dichloropr'oparie
trans-1.,3-Dichlorophr6pyJene.......
Dichloropropene(s)..
Dieldrin .'.
biethyl phthalate
4-Dimethylaminoazobenzene
7,12- .
Dimethy]benz(a)anthracene.
alpha-.alpha-
Dimethylpheriethylamine.
2,4-Dimethyrphenol ..'....'».» ...
Dimethyl phthalate
Dinitrobenzene(s). :.....
2,4-Dinitrophenol ;
2,4-Dinitrotoluene
2,6-Dinitro toluene •• ••
1,2-Diphenylhydrazine
Endosulfan(l & II) .-
Endrin., >
Ethyl ether >•••
Endrin metabolites
Ethyl methanesulfpnate
Fluoranthene.....
Heptachlor ....
Hexachlorobenzene
Hexachlorobutadiene i ,
Hexachlorocyclopentadiene.......
Hexaohloroethane
lndeno(1,2,3^cd)pyrene
Ltndane
Maleic anhydride
Methoxychtor •••
. 3-Methylcholanthrene
Methyl ethyl ketone ...
Methyl isobuty) ketone ..:.
Methylmethanesulfonate
Naphthalene :
Naphthoquinone..,.. ,
1 -Naphthylamine ...,....*..
2-Naphthylamiha ....
Nitrobenzene •;
4-Nitrophenol .«
N-Nitrosodibutylamine...:..'i....;...
N-NitroSodimethylamirie ............
N-Nitrosopiperidine ................;....
Paraldehyde (trimer of acetal-
dehyde). ,
Pentachlorobenzene. — :...»
Pentachloronitrobenzene ..........
Pentachlorophenol,, , ,-
Phenol :....(.,'.: ; ••.-
Phorate ; ....>..„....
Phthalic anhydride.............:........
Method(s).
8010, 8021, 8240,
8260
8010,8021.8240,
- 8260
8010 ,
8010, 8240
8010
8040, 8250, 8270
8040, 8250, 8270
8010,8021,8240,
8260
8010
8240
8080, 8250, 8270
8060, 8250, 8270
8250, 8270
8250, 8270
8250, 8270 . '
8040, 8250, 8270
8060, 8250, 8270
8090,8270
8040, 8250, 8270
8090, 8250, 8270
8090, 8250, 8270
8150,8260
8060
8256, 8270
8250, 8270
8140,8270
8080, 8250, 8270
8080, 8250, 8270
8015
8080, 8250, 8270
8250, 8270
8100, 8250, 8270,
8310
8080, 8250, 8270
8080, 8250, 8270
8120,8250,8270
8021,8120,8250,
8260,8270
8210, 8250. 8270
8120,8250,8270
8100, 8250, 8270,
8310
8080
8250, 8270
8080, 8250, 8270
8100, 8250, 8270
8015
8015,8240:
8250,8270 .
8021,, 81 00, 8250,
8270,8310:
8090, 8270
8250.8270
8250.8270
8250,8270 .'.
8090, 8250,' 8270,
8040, 8250, 8270
8250, 8270 v
8250,8270
•8250, 8270 •:
8015; '-...
8140, 8141, 8270
8250, 8270
8250, 8270 : ,
8,040. 8250, 8270
8250, 8270
8040,' 8250, 827.0
r»t40,8141- ' :
82«s,-, . .-. • :'..
8*4C. 8250, 8270
8250,8276
-------
Federal Register / Vol. 54, No. 13 / Monday, January 23, 1989 / Proposed Rules
TABLE 1.— ANALYSIS METHODS FOR OR-
GANIC CHEMICALS CONTAINED IN SW-
846— Continued
Compound
Tetrachloroethane(s) :
Tetrachlorophenol.....
Toluene ;
Toxaphene '.
1,2,4-Trichlorobenzene
Trichloroethane(s)
Trichlorofluoromethane
Triohloropropane
Vinyl chloride .'. .-..„;.
Xylene(s) .'.
^
Method(s)
8120, 8250, 8270
8010, 8021, 8240,
8260
8010,8021,8240,
8260
8040, 8250; 8270
8020,8021,8240,
8260
8080, 8250. 8270
8021,8120,8250,
8260, 8270
8010,8021,8240
8010, 8021, 8240
8010, 8021, 8240
8040, 8250, 8270
8010, 8021, 8240
801 Q; 8021, 8240,
• 8260
8020,8021,8240,
8260 '
1 Analyze for phenanthrene and carbazole; if
these are present in a ratio between 1.4:1 and 5:1
creosote should be considered present.
TABLE 2— ANALYSIS METHODS FOR INOR-
GANIC CHEMICALS AND MISCELLANEOUS
. GROUPS OF ANALYTES CONTAINED IN
SW-846
'Compound
Aluminum
Antimony '.:
Arsenic
Barium
Beryllium „.
Cadmium ,
Calcium
Chromium :
Chromium, Hexavalent
Cobalt. ;
Lead
Lithium.:;
Magnesium....
Manganese
Mercury ..
Molybdenum
Nickel
Osmium
Phosphorus...
Silver
Sodium „.
Strontium..;
Thallium
Tin
Vanadium..
Zinc
Cyanide
Total Organic Halogen
Purgeable Organic
Sulfide
Sulfate
Total Organic Carbon
Phenolics.. .:..:.
Oil and Grease
Total.Coliform.. ;
Nitrate..
Chloride '.
Method(s)
6010, 7020'
6010, 7040, 7041
6010, 7060, 7061
6010, 7080. 7081
. 6010, 7090. 7091
6010, 7130, 7131
6010, 7140
' 6010,7190,7191
7195,7196,7197,7198
6010,7200,7201
6010.7210,7211
6010, 7380, 7381
6010, 7420, 7421
6010, 7430
.6010,7450
6010, 7460. 7461
7470, 7471
6010, 7480, 7481
,6010,7520
7550
6010
. 6010, 7610
6010, 7740, 7741
6010, 7760; 7761
6010, 7770
6010, 7780
6010, 7840, 7841
7870
6010,7910,7911
,6010, 7950, 7951
'9010, 9012
9020, 9022 ,
9021
9030, 9031
9035, 9036, 9038
9060
9065, 9066, 9067
9070. 9071
9131, 9132
•9200
9250, 9251, 9252
TABLE 2— ANALYSI
GANIC CHEMICAL
GROUPS OF AN
SW 846 Contir
s METHODS FOR INQR-
s AND MISCELLANEOUS
ALYTES CONTAINED IN
lued
Compound Method(s)
' Gross Alpha and Gross
Beta ;;
Alpha-Emitting Radium
Isotopes....
'9310
9315
9320
TABLE 3.— SAMPLING AND ANALYSIS
METHODS CONTAINED IN SW-846
- Title
Quality control
Method detection
limit
Quality 'control
documentation........
References
Choosing the correct
procedure
Purpose
Required information.
Implementing the
guidance.....
Characteristics
Ground water....
References
Metallic analytes
Sampling
, considerations
Sample preparation
methods
Acid digestion of
waters for total
recoverable or
dissolved metals
for analysis by
flame AAS or
ICP
Acid digestion of
aqueous
samples and
extracts for total
metals for
analysis by
, flame AAS or
ICP....
Acid digestion of
aqueous
samples and
extracts for total
metals for
analysis by .
furnace AAS
Dissolution
procedure for
oils, greases, or
. waxes.;........:
Acid digestion of
.sediments,
sludges and
soils.........
Methods for the
determination of
Inductively
coupled plasma
atomic emission
spectroscopy
Atomic absorption
methods
Chapter No.
^
1.0
1.1
1.2
1.3
• 1.4
1.5
1.6
: 2.0
2.1
2.2
2.3
2.4
2.5
'2.6
3.0
3.1
3.2
3.2
3.2
3.2
3.2
3-2
3.3
' 3.3
3.3
Method No.
3005
3010
3020
3040
V
3050
6010
7000
TABLE 3.— SAMPLING AND ANALYSIS
METHODS CONTAINED IN SW-846—
Continued
Title
Aluminum, flame
AAS
'Antimony, flame
AAS
Antjmony, furnace
AAS
Arsenic, furnace
AAS
• Arsenic, gaseous
hydride AAS
Barium, flame AAS
Barium, furnace
AAS
Beryllium, flame
AAS
Beryllium, furnace
AAS'
Cadmium, flame
AAS
Cadmium, furnace
AAS
Calcium, flame
AAS
Chromium, flame
AAS....
Chromium, furnace
AAS
. Chromium,
hexavalerit, .
coprecipitation ....
Chromium,
hexavalent,
colorimetric
Chromium,
hexavalent,
chelation/
extraction
Chromium,
hexavalent,
differential pulse
polarpgraphy
Cobalt, flame AAS..
Cobalt, furnace
AAS
"Copper, flame
AAS
Copper, furnace
• AAO
Iron, flame AAS
Iron, furnace AAS ...
Lead, flame AAS
Lead, furnace AAS..
Magnesium, flame
AAS
Manganese, flame
AAS. „.
Manganese,
furnace AAS
Mercury in liquid
waste, manual
cold vapor
technique
Mercury in solid or
semisolid waste,
manual cold-
vapor technique...
Molybdenum,
flame AAS
Molybdenum,
furnace AAS
Nickel, flame AAS...
Osmium, flame'
Potassium, flame
Selenium, furnace *
AAQ
Chapter No.
3.3
3.3
3.3
3.3
3.3
3.3
3.3
3.3
. 3-3
3.3
3.3
3.3
3.3
3.3
-3.3
3.3
3.3;
3.3
3.3
3.3
3.3
3.3
3.3
.3,3
• 3:3'
3.3
3.3
3.3
3.3
' 3.3
3.3
3.3
3:3
• • 3,3
• 3.3
-3.3
3.3
Method No.'
7020
7040 '
7041
7060
7061
7080
7081
7090
7091
7130
7131
7140
7190
7191
. 7195
7196 '
7197
7198
7200
' 7201
' . 7210
7211
7380
7381
7420
7421
7450
7460
7461
7470
7471
- .7480
7481
• 7520
7550
7610
7740
-------
3224
Federal Register/Vol; 54, No. 13 /.Monday, January 23, 1989 / Proposed Rules
TABLE 3.— SAMPLING AND ANALYSIS
METHODS CONTAINED IN SW-846—
Continued
Title '
Selenium, gaseous
hydride AAS
Stiver, llama AAS....
Stiver, fumaca
AAS
Sodium, flame
AAS
Thallium, llamo
AAS,
Thallium, fumaca
AAS
Tin, flame AAS
Vanadium, llama
AAS..™,™™™...™,,
Vanadium, furnace
AAS..™.....
Zinc, flame AAS ......
Zinc, fumaca AAS...
Organic anafytos™
Sampling
considerations
Sampla preparation
methods
Extraction and
Organic extraction
and sample
preparation
Separately funnel
liquid-liquid
extraction..™
Continuous HquW-
Kqufd extraction...
Soxhlot extraction™
Ultrasonic
extraction
Waste dilution..™
Purge-and'trap
Protocol for
analysis of
sorbent
cartridges from
VOST
Cleanup
Cleanup ...™ ™..
Atumma column
cleanup
Alumina column
cleanup and
soparalion.ol
potioloum
wastes ™.......
Flofisil column
cleanup...
SKca gel cleanup....
Gol-potmcatton
cleanup....*™.
Acid-base partition
cleanup.....™
• Sulfur cleanup
, Determination of
organic analytos —
Gas
chromatographic
methods
Gas
chromalogra-
ptw t<11OT (lll
Halogo rated
volants
organlcs
EDBandDBCP...
Nonhatogenated
volatilo
ixganics
Aromatic votatila
organics....™.....
Chapter No.
3.3
33
3.3
3.3
3.3
3.3
3.3
3.3
3.3
3.3
3.3
4.0
4.1
4.2
4.2.1
4.2.1
4.2.1
4.2.1
-4.2.1
4.2.1
' 4.2.1
4.2.1
4.2.1
4.2.2
4.2.2
4.2.2
4.2.2
4.2.2
4.2.2
4.2.2
4.2.2
42.2
4.3
4.3.1
4.3.1
4.3.1
4.3.1
4.3.1
' 4.3.1
Method No.
7741
7760
, 7761
7770
7840
7841
7870
7910
7911
7950
7951
3500
3510
3520
'3540
• 3550
3580
5030
5040
3600
3610.
3611
3620
3630
3640
3650
3660
8000
6010
6011
8015
8020
TABLE , 3.— SAMPLING AND' ANALYSIS
METHODS - CONTAINED JN SW-846 —
Continued
Title ,
Volatile-organic
compounds in
water by
• purge-and-
trap capillary
column GC
with PID and
electrolytic
conductivity
detector in
series -
Acrolein,
•• acrylonitrile,
acetonitrile
Phenols
Phthalate esters..
Nitrosamines
Organo'chlorine
pesticides and
RGBs as
aroclors
Nitroaromatics
and cyclic
Polynuclear
aromatic •
hydrocarbons...
Haloethers :.
Chlorinated
hydrocarbons...
Organophos-
' phorous
pesticides
Organophos-
phorus
pesticides:
capillary
column .'
Chlorinated
herbicides
Gas
chromatogra-
phic/mass
spectroscopic
methods
• GC/MS volatiles..
GC/MS
semh/olatiles,
packed
column
GC/MS for
volatiles
capillary
column
GC/MS
semh/olatiles,
capillary
column
Analysis of
chlorinated
dioxins and -
dibenzofurans ..
High performance
liquid
chromatographic
methods (HPLC)..
Polynuclear
aromatic
hydrocarbons...
Miscellaneous
screening
methods ...
Headspace
Chapter No.
4.3.1
4.3.1
4.3.1
4.3.1
4.3.1
4.3/t
4.3.1
4.3.1
4.3.1
4.3.1
4.3.1
f
4.3.1
4.3.1
4.3.2
4.3.2
4.3.2
4.3.2
4.3.2
4.3.2
4.3.3
4.3.3
4.4
4.4
Method No.
8021
8030
8040 '
8060
8070
8080
8090
8100
.8110
8120 .:
8140
8141
8150
8240
8250 :
8260
8270 '
8280 j
8310
3810
TABLE 3.— SAMPLING AND ANALYSIS
METHODS CONTAINED IN SW-846—
Continued
. • :. Title.
Hexadecane
extraction and
screening Of
pufgeable
. organics
Miscellaneous test
Total, and amenable
cyanide
(colorimetric,
manual)
Total and amenable
. cyanide
(colorimetric,
.automated)
. Total organic halides
(TOX)
Purgeable organic
halides (POX)
Total organic halides
(TOX) by neutron
activation analysis...
Acid-soluble and '
acid-insoluble
Extractabla sulfides ....
Sulfate (colorimetric
automated, >
chloranitate) ...
Sulfate, (colorimetric
automated,
rnethylthymol blue,
AA II) ...
Sulfate,
(turbidimetric)
Total organic carbon ..
Phenolics
(spectrophotomet-
rte, manual 4-
AAP)
Phenolics
(colorimetric
automated, 4-
AAP)
Phenolics
(spectrophotomet-
ric, MBTH)
Total recoverable oil ,
and grease
(gravimetric,
separatory funnel
OH and grease
• extraction method
for sludge samples .
Total coliform:
multiple tube
fermentation
Total Coliform:
membrane filter
Nitrate......
. Chloride (colorimetric
automated,
ferricyanide AAI)....l.
Chloride (colorimetrie
automated,
ferricyanide A All)
Chloride (titrimetric,
mercuric nitrate)......
Multiple extraction
Extraction procedure
for oily wastes
pH electrometric
measurement
pH paper method
Chapter No. '•
L
4.4
5.0 ;
5.0.
5.0
5.0
5.0
5.0
5.0
5.0.
S;0
5.0
-5.0
5.0
5.0 '
5.0
5.0'
5,0 '•
5.0,
5.0 ,
5JO,
5.0 i
' 1
.5.0 \
SJO':
•5.0 '.
6.0 ,
&0'
6,0
&.0,
8.0
Method No.
3820
9010
9012
9020
8023
9022
9030
,9031
9035
9036
9038
9060
9065
9066
9067
9070
9071
9131
9132
92GO
9250
9251
.9252
13SO
1339
S040
®041
-------
Federal Register / Vol. 54, No.. 13 / Monday, January 23, 1989 / Proposed -Rules-
3225
TABLE. 3.—SAMPLING AND ANALYSIS
METHODS CONTAINED IN SW-846—
Continued :
Title
Soil pH ..
Specific
conductance..:.........
Cation-exchange
capacity of soils
(ammonium
acetate) ..•
Cation-exchange
capacity of soils
(sodium acetate) .....
Compatibility test for-
wastes and
membrane liners
Paint filter liquids
test ' ; '
Saturated hydraulic
conductivity,
saturated leachate
conductivity, and
intrinsic
permeability
Gross alpha and
gross beta.. . . .. '
Alpha-emitting
radium isotopes
Radium-228....
Introduction and
regulatory definitions ..
Ignitability
Corrosivity ...... .....
Reactivity „.
Test method to
determine
hydrogen
cyanide
released from
Test method to
determine
hydrogen sulfide
released from
wastes ...
Extraction procedure
toxicity . .
Methods for
determining
characteristics
Ignitability ... .
Pensky-Martens
closed-cup
method ..".
Setaflash closed-
cup method
Corrosivity toward '
steel ......
Reactivity
Extraction
procedure (EP)
toxicity test
method and
structural
integrity test
Sampling plan
Design and
development
Implementation...........
Sampling methods
Modified method 5
sampling train,
appendix A and B ..
Source assessment
sampling system
(SASS) :.
Volatile organic
sampling train
Chapter No.
• 60
6.0
60
6.0
6.0
60
60
60
6.0
6.0
7.0
7.1
7.3
• ' •''• ' 73'
. 73
. - ' 7.3
74
8.0
81
8.1
8.1
82
8.2
8.3
84
8.4
9.0
9.1
9.2
10.0
10.0
10.0
10.0
Method No.
9045
9050
9080
9081
9090
9095
9100
9310
9315
9320
1010
1020
1110
1310
0010
0020
" 0030
TABLE 3.—SAMPLING AND ANALYSIS
METHODS CONTAINED IM SW-846—
Continued
Title
Ground water
monitoring
Background and
Relationship to the
regulations and to
other documents.....
. Revisions and ."
additions
Acceptable designs
Unacceptable
designs and
Land treatment
monitoring
Background
Treatment zone
Regulatory definition...
Monitoring and
sampling strategy....
Analysis
References and
bibliography..
Incineration.
Introduction...1 ;
Regulatory definition...
Waste
characterization
strategy. ..... ..
Stack-gas effluent
characterization ,
strategy.
Additional effluent
characterization
strategy.....1 :...'...-...
Selection of specific
sampling and
analysis methods ....
References
Chapter No.
110
111
11.2
11.3
11 4
11 5
12.0
12.1
12.2
12.3
12.4
12.5
12.6
13.0
13.1
13.2
.. 13.3
13.4
13.5 '
13.6
137
Method No.
Subpart C—-Characteristics of
Hazardous Waste
8. Section 261.22 is amended by
revising paragraphs (a)(l) and (2) to
read as follows: .
§261.22 Characteristic of Corrosivity.
(a) * * *
(1) It is aqueous and has a pH less
than or equal to 2 or greater than or
equal to 12.5, as determined by a pH
meter using either an EPA test method
or an equivalent test method approved '
by the Administrator under the
procedures set forth in § § 260.20 and
260.21. The EPA test method for pH is
specified in "Test Methods for
Evaluating Solid Waste, Physical/
Chemical Methods", EPA Publication
SW-846, as incorporated by reference in
§ 260.11. In all cases, the sampling and
analytical determinations must comply
with the quality control procedures
specified in Sections 1.2 and 1.3, and
where an SW-846 method is used, those •
procedures set forth in Section 8.0 of the
methods contained in Chapters Three
through Eight andTen which are *
referenced therein, of Chapter One of
SW-846.
(2) It is a liquid and corrodes steel
(SAB 1020) at a rate greater than 6.35
mm (0.250 inch) per year at a test
temperature of 55° C (130° F) as
determined by the, test method specified
in NACE (National Association of -
Corrosion Engineers) Standard TM-01-
69. as standardizedin "Test Methods for
Evaluating Solid Waste, Physical/
Chemical Methods", EPA Publication :
SW-846, as incorporated by reference in
§ 260.11, or an equivalent test method
approved by the'Administrator under,
the procredures set forth in §§ 260.20
and 260.21. In all cases, the sampling '
and analytical determinations must
comply with the quality control
procedures specified in Sections 1.2 and
1.3, and, where an SW-846 method is
used, those procedures set forth in
Section 8.0 of .the methods contained in
Chapters Three through Eight and Ten
which are referenced therein, of Chapter
One of SW-846. -.'••'
* * • *. * *
9. Section 261.24 is amended by
revising paragraph (a) to read as
follows:
§251.24 Characteristic of EP tOMicity.
" (a) A solid waste exhibits the
characteristic of EP toxicity if, using the
test methods and procedures described
in Appendix II or equivalent methods "
approved by the Administrator under •
the procedures set forth in § § 260.20 and
260.21, the extract from a representative
sample of the waste contains any of the ,
contaminants listed in Table 1 at a
concentration equal to or greater than
the respective value given in that table.
Where the waste contains less than 0.5
percent filterable solids, the waste itself,
after filtering, is considered to be the
extract for the purposes of this section.
In all cases, the determinations must
comply with the quality control
procedures specified in Sections 1.2 and
1.3, and, where an SW-846 method is
used, those procedures set forth in .
Section 8.0 of the methods contained in
Chapters Three through Eight and Ten
which are referenced therein, of Chapter
One of 'Test Methods for Evaluating
Solid Waste, Physical/Chemical
Methods", EPA Publication SW-846 as
incorporated by reference in § 260.11. '.
PART 262-^-STAKSDARDS APPLICABLE
TO GENERATORS OF HAZARDOUS-
WASTE ., • .' •
10. The authority citation for Part 262
continues to read as follows:
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3226
Federal Register / Vol., 54, No. 13 / Monday, January 23. 1989 / Proposed Rules
Authority: 42 U.S.C. 6906,6912. 6922. 6923.
6024.6925, and 6937.
Subpart A—General
11. Section 262.11 is amended by
adding, paragraph (e) to read as follows:
§ 262.11 Hazardous waste determination.
« * « * ° *
(c) In all cases, the sampling and
analytical determinations performed to
meet the requirements of Part 262 must
comply with the quality control
procedures specified in Sections 1.2 and
1.3, and. where the SW-846 methods are
used, those procedures set forth in
Section 8.0 of the methods contained in
Chapters Three through Eight and Ten
which are referenced therein, of Chapter
One of "Test Methods for Evaluating
Solid Waste. Physical/Chemical
Methods", EPA Publication SW-846, as
incorporated by reference in § 260.11.
These quality control requirements must
be followed when using any SW-846 ,
method, whether mandatory or not
mandatory, and when using any other
analytical method.
PART 264—STANDARDS FOR
OWNERS AND OPERATORS OF.
HAZARDOUS WASTE TREATMENT,
STORAGE, AND DISPOSAL
FACILITIES
12. The authority citation for Part 264
continues to read as follows:
Authority; 42 U.S.C. 6905,6912(a), 6924, and
0825.
Subpart A—General
13. Section 264.1 is amended by
adding (i) to read as follows:
§ 264.1 Purpose, scope, and applicability.
* * * * * .
(i) In all cases, the sampling and
analytical determinations performed to
meet the requirements of Part 264 must
comply with the quality control
procedures specified in Section 1.2 and
1.3, and, where SW-846 methods are
used, those procedures set forth in
Section 8.0 of the methods contained in
Chapters Three through Eight and Ten
which are referenced therein, of Chapter
One of "Test Methods for Evaluating ,
Solid Waste. Physical/Chemical
Methods", EPA Publication SW-846, as
incorporated by reference in § 260.11.
These quality control procedures must
be followed when using any SW-846
method, whether mandatory or not
mandatory, and when using any other
analytical method.
Subpart N—Landfills
14. Section 264.314 is amended by
revising-paragraph (c) to read as
follows:
§ 264.314 Special requirements for bulk-
and containerized liquids.
*******
(c) To demonstrate the absence or.
presence of free liquids in either a
containerized or a bulk waste, the
following test must be used: Method
9095 (Paint Filter Liquids Test) as
described in "Test Methods for
Evaluating Solid Wastes, Physical/
Chemical Methods", EPA Publication ,
SW-846, as incorporated by reference in
§ 260.11. The sampling and analytical
determinations performed to
demonstrate the absence or presence of
free liquids in a containerized or bulk
waste must comply with the appropriate
quality control procedures specified in
• Section 1.2, and those procedures set
forth in Section 8.0 of Method 9095
referenced therein, of Chapter One of
1 "Test Methods for Evaluating Solid
Waste, Physical/Chemical Methods",
EPA Publication SW-846, as
incorporated by reference in § 260.11
PART 265—INTERIM STATUS ,
STANDARDS FOR OWNERS AND
OPERATORS OF HAZARDOUS WASTE
TREATMENT, STORAGE, AND
DISPOSAL FACILITIES
15. The authority citation for Part 265
continues to read as follows:
Authority: 42 U.S.C. 6905, 6912(a), 6924,
6925, and 6935.
Subpart A—General
16. Section 265.1 is amended by
adding paragraph (f) to read as follows:
§265.1 Purpose, scope, and applicability.
* * * * *
(f) In all cases, the sampling and
analytical-determinations performed to
meet the requirements of Part 265 must
comply with the quality control
procedures specified in Sections 1.2 and
1.3, and, where SW-846 methods are
•used, those procedures set forth in
Section 8.0 of the methods contained in
Chapters Three through Eight and Ten
which are referenced therein, of Chapter
One of "Test Methods for Evaluating
Solid Waste, Physical/Chemical
Methods", EPA Publication SW-846, as
incorporated by reference in § 260.11.
These quality control procedures must
be followed when using any SW-846
method, whether mandatory or not
mandatory, and when using any other
analytical method.
Subpart N—Landfills
17. Section 265.314 is amended by ,
revising paragraph (d) to read as
follows:,
§ 265.314 Special requirements for bulk
and containerized liquids.
*" * * * " *
(d) To demonstrate the absence or
presence of free liquids in either a
containerized or a bulk waste, the
following text must be used: Method
9095 (Paint Filter Liquids Test) as ,
described in "Test Methods for
Evaluating Solid Wastes, Physical/
Chemical Methods", EPA Publication
SW-846, as incorporated by reference in
§ 260.11. The sampling and analytical
determinations performed to
demonstrate the absence or presence of
free liquids in a containerized or bulk
waste must comply with the appropriate
. quality control procedures specified in
Section 1.2, and those procedures set
forth.in Section 8.0 of Method 9095
referenced therein, of Chapter One of
"Test Methods for Evaluating Solid ,
Waste, Physical/Chemical Methods",
EPA Publication SW-846, as
incorporated by reference in § 260.11.
PART 268—LAND DISPOSAL
RESTRICTIONS .
18. Thfe authority citation for Part 268
continues to read as follows:
Authority: 42 U.S.C. 69Q5, 6912(a), 6921 and
6924. . ,
Subpart A—General
19. Section 268.1 is amended by .
adding paragraph (e) to read as follows:
§ 268.1 Purpose, scope and applicability.
*' * * * * .
(e) In all cases, the sampling arid;
analytical determinations performed to
meet the requirements of Part 268 must
comply with the quality control
procedures specfied in Sections 1.2,and
1.3, and those additional procedures set
forth in Section 8.0 of the methods ,'•
contained in Chapters Three through
Eight and Ten which are referenced
therein, of Chapter One of "Test
Methods for Evaluating Solid Waste,
Physical/Chemical Methods", EPA
Publication SW-846, as incorporated by
reference in § 260.11. These quality
control procedures must be followed
when using any SW-846 method,
whether mandatory or not mandatory,
and when using any other analytical •
method.
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t€!f
54' NO. 13 / Monday. January 23, 1989 / Proposed Rules
3227
PART 270—EPA ADMINISTERED
PERMIT PROGRAMS: THE
HAZARDOUS WASTE PERMIT
PROGRAM
20. The authority citation for Part 270
continues to read as follows:
Authority: 42 U.S.C. 6905. 6912, 6925, 6927,
6939, and 6974.
Subpart A—General Information
21. Section 270.1 is amended by
adding paragraph (d) to read as follows:
§ 270.1 Purpose and scope of these
regulations.
*****
(d) In all cases, the sampling and
analytical determinations performed to
meet the requirements of Part 270 must
comply with the quality control
procedures specified in Sections 1.2 and
1.3, and those procedures set forth in
Section 8.0 of the methods contained in
Chapters Three through Eight and Ten
which are referenced therein, of Chapter
One of "Test Methods for Evaluating
Solid Waste, Physical/Chemical
Methods", EPA Publication SW-846, as
incorporated by reference in § 270.8.
. These quality control procedures must
be followed when using any SW-846
method, whether mandatory or not
mandatory, and when using any other
analytical method.
22. Section 270.6 is amended by
revising the first reference In paragraph
(a) to read as follows:
§ 270.8 References.
(a)* * * "Test Methods for
Evaluating Solid Waste, Physical/
Chemical Methods", EPA Publication
SW-846, Third Edition, 1987, as
amended by Update I. This document is
available as document number 955-001-
OOOOft-1 from the Superintendent of
-Documents, U.S. Government Printing
Office, Washington, DC 20402, {202) 783-
3238, on a subscription basis.-Future
updates will automatically be mailed to
the subscriber. •
Subpart F—Special Forms of Permits
23. Section 270.62 is amended by
revising paragraph (b)(2){i)(C) to read as
follows:
§ 270.62 Hazardous waste incinerator
permits. .-."-;•
* * * * *
(b) * * *
(2) * * *
{i) , * *
(C) An identification of any hazardous
organic constituents listed in Part 261,
Appendix VIII of this chapter, which are
present in the waste to be burned,
except that the applicant need not
analyze for constituents listed in Part
261, Appendix VIII, of this chapter.
which would reasonably not be
expected to be found in the waste. The
constituents excluded from analysis
must be identified, and the basis for the
exclusion stated. The waste analysis
must rely on analytical techniques
specified in "Test. Methods for
Evaluating Solid Waste, Physical/
Chemical Methods", EPA .Publication
SW-846, as incorporated by reference in
§ 270.6, or theuvequivalent In all cases,
the sampling and analytical
determinations performed to meet the
requirements of this Part must comply
with the quality control procedures
specified hi Sections 1.2 and 1.3, and,
where an SW-^846 method is used, those
procedures set forth in Section 8.6 of the
methods contained hi Chapters Three .
through Eight and Ten which are
referenced therein, of Chapter One of .
"Test Methods fpr Evaluating Solid
Waste, Physical/Chemical Methods",
EPA Publication SW-846, as :
incorporated by reference in § 570.6.
These quality control procedures must
be followed when using any SW-646
method, whether mandatory or not
mandatory, and when using any other
analytical method,
* * . * * * ;
Editorial Note: This appendix will not
appear in the Code of Federal Regulations.
Appendix A—Chapter One Changes in
SW-846, Third Edition
Page No. in Chapter One •.
1. ONE-7—In section 1.1.8, revise the
definition of ACCURACY to read as follows:
Accuracy is the nearness of ,a measurement
or the mean (x) of a set of measurements to
the true value. Accuracy is assessed by
means of reference samples and percent
recoveries.
2. ONE-7—Add this sentence after the last
sentence.in the present definition of
ANALYTICAL BATCH:
Analytical batch: "* * .* Samples in each
batch should be of similar composition (e.g.
ground water, sludge, ash, etc.) ,
3. ONE-7—Replace present definition for
BLANK with the following: Blanks:
ONE-7— Calibration blank: Usually an
organic or aqueous Solution that is as free of
analyte as possible and prepared with the
same volume of chemical reagents used in the
preparation of the calibration standards and
diluted to the appropriate volume with the
seme solvent (water or organic] used .in the
preparation of the calibration standard. The
calibration blank is used to give the null
reading for the instrument response versus
concentration calibration curve. One
.calibration blank should be analyzed with
each analytical batch or every 20 samples,
whichever is greater.
ONE-8—Equipment blank: Usually an
organic or aqueous solution that is as free of
analyte as possible,and is tranported to the
site, opened in the field, and poured over or
through the sample collection device,
collected in a sample container, and returned
to the laboratory. This serves as a check on
sampling device cleanliness. One equipment
blank should be analyzed-with each
analytical batch or every 20 samples,
• whichever is greater. •
ONE-8—Field blank: Usually an organic or
aqueous solution that is as free of analyte as
possible and is transferred from one vessel to
another at the sampling site and preserved
with the appropriate reagents. This serves as
a check on reagent and environmental
contamination. One field blank should be
analyzed with each analytical batch or every
20 samples, whichever is greater.
ONE-S—Reagent blank: Usually an organic
or aqueous solution that is as free of analyte
as possible and contains all the reagents in
the same voluine as used in the processing of
the samples. The reagent blank mast be
carried through the complete sample
preparation procedure and contains the same
reagent concentrations in the final solution as
in the sample solution used for analysis. The
reagent blank is used to correct for possible
contamination, resulting from the preparation
or processing of the sample. One reagent
blank should be prepared for /every analytical
batch or for every 20 samples, whichever is
greater.
ONE-&~Trfp blank: Usually an organic or
aquecms solution that, is as free of analyte as
possible and is transported to the sampling
site and returned to •me laboratory without
being opened.-This serves as a check on
sample contamination originating from
sample transport, shipping, and from the site
conditions. One trip blank should be
• analyzed with each analytical batch or every
20 samples, whichever is greater.
4. ONE-8-iDelete CALIBRATION CHECK
: and" insert the following:
Check standard: A material of known
composition that is analyzed-concurrently
with test samples to evaluate a measurement
process. An analytical standard that is
analyzed to verify the calibration of the
analytical system. One check standard
should be analyzed with each analytical
batch or every 20 samples, whichever is
greater. . .
:5. ONE-8—Add the definition of MATRIX
SPIKE as follows:
Matrix spike; A matrix spike is employed
to provide a measure of accuracy for the
method used ia a given matrix, A matrix
spike analysis is performed by adding a
predetermined quantity of stock solutions of .
. certain analytes to a sample matrix prior 'to
sample extraction/digestion and analysis.
The concentration of the spike should be at
the, regulatory standard level or the PQL for
the method. When the concentration of the
analyte in the sample is greater than 0.1%, no
spike of the analyte is necessary.
. 6. ONE-S—Delete MQL and insert.the
fallowing:
MDL: The methoddetection limit (MDL) is
defined as the minimum concentration of a
substance that can be measurad and reported
with 99% confidence that the analyte
concentration is greater than zero and is
-------
3228
Federal^Register / Vol. 54, No.13 /Monday, January 23, 1989 / Proposed Rules
determined from analysis of a sample in a
given matrix containing the analyte.
7. ONE-8—Revise the definition of
PRECISION to read as follows:
Precision Is the agreement between a set of
replicate measurements without assumption
or knowledge of the true value. Precision is
assessed by means of duplicate/replicate
mimplo analysis.
8. ONE-9—Add the heading SAMPLES.
with the following definitions:
ONE-9—Delete MATRIX SPIKE/
DUPLICATE ANALYSIS and insert the
following: ' '•
Duplicate samples: Duplicate samples are
two separate samples taken from the same
source (i.e. in separate containers and
analyzed independently).
ONE-10—Delete CHECK SAMPLE and
insert the following:
Quality control reference sample: A
sample prepared from an independent
standard at a concentration other than that
used for calibration, but within the
calibration range. An independent standard
Is defined as a standard composed of the
analylc(s) of interest from a different source
than that used in the preparation of
standards for use in the standard curve. A
quality control reference sample is intended
as an Independent check of technique,
methodology, and standards and should be
run with every analytical batch or every 20
samples, whichever is greater. This is
applicable to all organic and inorganic
analyses. .' . t
ONE-10—Replace the definition of
REPLICATE SAMPLE with the following:
/ieplicale Samples: Replicate samples are
two allquots taken from the same sample
container and analyzed independently. In
cases where allquoting is impossible, as in
the case of volatiles. duplicate samples must *
bo taken for replicate analysis. '
9. ONE-10—Replace the definition of '
STANDARD CURVE with the following:
Standard curve: A standard curve is a
curve which plots concentrations of known
nnnlyte standards versus the instrument
response to the analyte. Calibration
ntandards are prepared by diluting the stock
(inalyto solution in graduated amounts which
cover the expected range of the samples . .
being analyzed.'Standards should be
prepared at the frequency specified in the
(ippropriatc section. The calibration
stundurds must be prepared using the same
Ijpe of acid or solvent and at the same
concentration as will result in the samples
following sample preparation. This is •
applicable to organic and inorganic chemical
tmuljscs.
10. ONE-10—Replace the definition of
SURROGATE with the following:
Surrogate: Surrogates are organic
compounds which are similar to analytes of
Interest in chemical composition, extraction,
and chromatography, but which are not
normally found in environmental samples.
These compounds are spiked into all blanks,
calibration and check standards, samples
(Including duplicates and QC reference
samples} and spiked samples prior to
analysis. Percent recoveries are calculated
for each surrogate. ..
11. ONE-11—Replace the definition of
WATER with the following:
Water: Any reference to water in a Chapter
or Method refers to ASTM Type II reagent
water (unless otherwise specified) which is
free of contaminants that may interfere with
the analytical test in question.,
12. ONE-11—In section 1.2.1, revise FIELD
QUALITY CONTROL to read as follows:
1.2.1 Field Quality Control'"' * '.Quality
Assurance Project Plan (QAPP) shall include
as appropriate:"
• 13. ONE-11—In section 1.2.2 revise
Analytical Quality Control by deleting the
last sentence in the second paragraph:
"The frequencies of these procedures shall
be as stated below or at least one with each •
analytical batch." . , l
14. ONE-12—Replace section 1.2.2.1.1 with
the folowing: '
' 1.2.2.1.1 Matrix Spiked Sample: A matrix
spiked sample shall be analyzed with every
analytical batch or every 20 samples,
whichever is greater. The sample shall be
spiked with the analyte(s) of interest (see the
appropriate method). The sample to be
spiked should be typical or representative of
the batch. Ideally, it should be an
intermediate between the cleanest and the
most contaminated samples based on the
best information available. It is
recommended that the spike be made in a
replicate of the field duplicate samples. This
is applicable to all organic or inorganic •
chemical analyses..
15. ONE-12—Add section 1.2.2.1.2-to read
as follows: '
Field Duplicate Samples shall be analyzed
with every analytical batch or every 20
samples, whichever is greater. This procedure
js applicable to all organic and inorganic ,
chemical analyses.
16. ONE-12—Add the following sentence to
the discussion under section 1.2.2.1.4, FIELD
SAMPLES/SURROGATE'COMPOUNDS,
delete the term "Field Samples" from the
heading, and replace check sample with the
following: •
1.2.2.1.4 Surrogate Compounds:
"* * * evaluation of analytical quality then
will rely on the quality control embodied in
the quality control reference sample and
spiked and duplicate samples. This is
applicable to organic analyses only."
17. ONE-12—In section 1.2.2.1.5,,the term
CHECK SAMPIE has been changed to
QUALITY CONTROL REFERENCE SAMPLE
and the definition rewritten as follows:
1.2.2.1.5 Quality Control Reference
Sample: A quality control reference sample is
a sample prepared from an independent
standard at a concentration other than that
used.for calibration, but within the
calibration range. An independent standard
is defined as a standard composed of the
analytes of interest from a different source ''
than that used in the preparation of
standards for use in the standard curve. A
quality control reference sample is intended
as an independent check of technique,
methodology, and standards and should be
run with every analytical batch or every 20
samples, whichever is greater. This is
applicable to all organic and inorganic
analyses.
18. ONE-13—Insert section 1.2.2.1.6,
CHECK STANDARD, to read as follows;
1.2.2,1.6 Check Standard: A standard of,
known concentration prepared by the analyst
to monitor and verify instrument performance
on a daily basis.
19. ONE-13—In section 1.2.2.2, add the
following sentence at the end of the
discussion on CLEAN-UPS:
"This is applicable to organic analyses
only."
20. ONE-13—In section 1.2.2.2.1, add the
following sentence at the end of the
discussion on Column check Sample:
"This is applicable to organic analyses
only."
21. ONE-13—In section 1.2.2.2.2, remove
"sample" from the heading for COLUMN
CHECK SAMPLE BLANK, delete the present
discussion, and insert the'foliowing:
1.2.2.2.2 Column Check Blank:"* * * The
column check blank shall be run after
activating or deactivating a batch of
adsorbent. This is applicable to organic
analyses only."
22. ONE-13—In section 1.2.2.3.1, add the
following sentence to INSTRUMENT
ADJUSTMENT: TUNING, ALIGNMENT,
ETC. and alter the heading as follows:
1.2.2.3.1 Instrument Adjustment, Tuning,
and Alignment: "* * 'appropriate
procedures. This is applicable to all organic
and inorganic analyses."'
23. ONE-14—In section 1.2.2.3.2, revise
CALIBRATION to read as follows:
"* * * procedures employed. Methods 6010,
7000, and 800° as well as the appropriate
analytical procedure ***" - :
24. ONE-14—In section 1:2.2.3.3, revise
ADDITIONAL QC REQUIREMENTS FOR
'INORGANIC ANALYSIS to read as follows:
"Standard curves derived from data
consisting of one calibration blank and three
concentrations * * *" •
25. ONE-16—In section 1.3, rvise METHOD
DETECTION LIMIT to read as follows:
For. operational purposes, when it is
necessary to determine the method detection .
limit in the sample matrix, the MDL defined
in One-9 shall be determined by multiplying
by 7 the standard deviation obtained from the
triplicate analyses of a matrix spike
containing the analyte of interest at a'
concentration three to five times the
estimated .MDL.
. • Determine the estimated MDL as follows:
• Obtain the concentration value that
corresponds to:
• a) an instrument signal/noise ratio
within the range of 2.5 to 5.0, or
• b) the region of the standard curve where
there is a significant change in sensitivity,
i.e., a break in the slope of the standard
curve.
• Determine the variance (S2) for each
analyte as follows:
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Federal Register / Vol. 54, No. 13 / Monday, January 23, 1989 / Proposed Rules 3229
• Determine the standard deviation (S) for
each analyte as follows: S = (S 2)I/2
• Determine the MDL for each analyte as
follows: MDL = t
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