[Federal Register Volume 80, Number 156 (Thursday, August 13, 2015)]
[Notices]
[Pages 48522-48528]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 2015-20030]
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ENVIRONMENTAL PROTECTION AGENCY
[EPA-HQ-RCRA-2012-0072; FRL-9929-37-OSWER]
Waste Management System; Testing and Monitoring Activities;
Notice of Availability of Final Update V of SW-846
AGENCY: Environmental Protection Agency (EPA).
ACTION: Notice.
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SUMMARY: The Environmental Protection Agency (EPA or Agency) is
providing notice of the availability of ``Final Update V'' to the Third
Edition of the manual, ``Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods,'' EPA publication SW-846. Final Update V
contains analytical methods, of which 8 are new and 15 are revised. The
methods in Update V may be used in monitoring or complying with the
Resource Conservation and Recovery Act (RCRA) hazardous waste
regulations. This action includes revisions to the methods in response
to comments received on a Notice published in the Federal Register on
October 23, 2013 and finalizes the methods and guidance. In addition,
the Agency is also finalizing revisions to Chapters One through Five of
SW-846 and an Office of Resource Conservation and Recovery (ORCR)
policy statement in the SW-846 methods compendium. The Agency is
issuing this Update as guidance since the changes in this document to
the SW-846 analytical methods are not required by RCRA's hazardous
waste regulations. Any required analytical methods have not been
changed.
FOR FURTHER INFORMATION CONTACT: Kim Kirkland, Office of Resource
Conservation and Recovery (5304P), Environmental Protection Agency,
1200 Pennsylvania Avenue NW., Washington, DC 20460-0002; telephone
number: (703) 308-8855, fax number: (703) 308-0509, email address:
[email protected].
SUPPLEMENTARY INFORMATION:
I. General Information
A. Does this action apply to me?
This notice is directed to the public in general. It may, however,
be of particular interest to those conducting waste sampling and
analysis for RCRA-related activities. This universe might include any
entity that generates, treats, stores, or disposes of hazardous or
nonhazardous solid waste and might also include any laboratory that
conducts waste sampling and analyses for such entities.
B. How can I get copies of Final Update V and other related
information?
1. The Agency has established a docket for this action under Docket
ID No. EPA-RCRA-2012-0072; FRL-9901-86-OSWER and FRL-9929-37-OSWER.
Publicly available docket materials are available either electronically
through www.regulations.gov or in hard copy at the OSWER RCRA Docket in
the EPA Docket Center (EPA/DC), EPA West, Room 3334, and 1301
Constitution Ave. NW., Washington, DC. The EPA Docket Center Public
Reading Room is open from 8:30 a.m. to 4:30 p.m., Monday through
Friday, excluding legal holidays. The telephone number for the Public
Reading Room is (202) 566-1744, and the telephone number for the OSWER
RCRA Docket is (202) 566-0270.
C. How can I get copies of the Third Edition of SW-846 its updates?
The Third Edition of SW-846, as amended by Final Updates I, II,
IIA, IIB, III, IIIA, IIIB, IVA, IVB, and V, is available in pdf format
on the Internet at http://www.epa.gov/SW-846.
D. How is the rest of this Notice organized?
Sections:
II. What is the subject and purpose of this Notice?
III. Why is the Agency releasing Update V to SW-846?
IV. What does final Update V contain?
V. What revisions are discussed in this Notice?
VI. Summary
II. What is the subject and purpose of this Notice?
The Agency is announcing publication of Final Update V to ``Test
Methods for Evaluating Solid Waste, Physical/Chemical Methods,'' EPA
publication SW-846, which is now part of the SW-846 methods compendium.
Specifically, Update V of SW-846 contains revisions to the first five
chapters of SW-846 and 23 new and modified analytical methods that the
Agency has evaluated, and/or revised and determined to be appropriate
and may be used for monitoring or complying with the RCRA hazardous
waste regulations. Eight of the 23 methods are new methods that have
been fully validated, i.e., they have completed technical and Agency
workgroup review and approval. In addition these eight new methods are
being announced in the Federal Register through this notice. Since the
methods have completed the approval process, they will be removed from
the ``Validated Methods'' link at: http://www.epa.gov/epawaste/hazard/testmethods/sw846/new_meth.htm and incorporated in the SW-846 methods
compendium at: http://www.epa.gov/epawaste/hazard/testmethods/sw846/online/index.htm.
The 15 revised methods have replaced the previous versions in the
final update package and will also be placed into the SW-846 methods
compendium. Because the RCRA hazardous waste regulations do not require
the analytical methods contained in Update V, the Agency is issuing
this update as guidance. This guidance does not add or change the RCRA
regulations, and does not have any impact on existing rulemakings
associated with the RCRA program. To date, the Agency has finalized
Updates I, II, IIA, IIB, III, IIIA, IIIB, IVA, and IVB to the SW-846
manual, which can be found on the Agency's ORCR Web page at: http://www.epa.gov/SW-846.
III. Why is the Agency releasing final Update V to SW-846?
SW-846 is revised over time as new information and data become
available. The Agency continually reviews advances in analytical
instrumentation and techniques and periodically incorporates such
advances into SW-846 as method updates by adding new methods to the
manual, and replacing existing methods with revised versions of the
same method. On October 23,
[[Page 48523]]
2013, the Agency published a FR Notice (78 FR 63185), announcing the
availability of Update V to SW-846. When the comment period closed on
January 23, 2014, the Agency received a total of 111 technical and
general comments on the Update. The Agency revised the methods and
chapters based on comments received, when it was appropriate to do so.
Revisions made were either editorial for clarity or technical for
accuracy. A summary of significant changes are noted in Appendix A of
each revised method.\1\ In addition, significant revisions to the
chapters are discussed in Section V of this Notice. These methods can
be used for any RCRA applications, other than those specifically
required by regulation. In cases that the regulation does not specify
the method, the analyst should select an appropriate method in which
the performance can be demonstrated and meet project-specific Data
Quality Objectives (DQOs). On a related matter, the Agency is also
finalizing an ORCR Policy Statement that responds to concerns the
Environmental Laboratory Advisory Board (ELAB) has expressed regarding
the official version and status of various methods. ELAB is a committee
established under the Federal Advisory Committee Act (FACA) that
advises the Agency on measurement, monitoring, and laboratory science
issues. The ELAB contacted the Agency's Forum on Environmental
Measurements (FEM) \2\ with several issues regarding the use of SW-846,
specifically seeking clarification about which versions of a revised
method are recommended, and seeking clarification in defining
terminology used to identify the category of methods.
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\1\ Specifically, this summary of significant changes (Appendix
A) is included in each newly-revised method referenced in this
notice, to assist users in identifying changes from the prior
version of the method. EPA also intends to include such summaries in
future method revisions.
\2\ The FEM is a standing committee of senior EPA managers
established in 2003 to promote consistency and consensus within the
EPA on measurement issues, and provide an internal and external
contact point for addressing measurement methodology, monitoring,
and laboratory science issues with multi-program impacts.
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The Agency did not receive any comments regarding the content of
the ORCR Policy Statement and has finalized it without change. As a
reminder, the Agency strongly recommends the use of the latest version
of an SW-846 method. The Agency, however, is not imposing restrictions
on the use of earlier versions of non-required SW-846 methods or
precluding the use of previous guidance, if such use is appropriate.
For example, earlier versions of an SW-846 method may be more
appropriate for regulatory purposes (e.g., for compliance with an
existing permit or consent decree), or when new method versions may be
more costly to run or perform, than necessary for meeting project-
specific objectives.
IV. What does final Update V contain?
Final Update V contains revisions to Chapters One through Five of
EPA's publication SW-846. As noted above, no changes are made to Method
Defined Parameters (MDPs), which are required by the RCRA regulation
and must be followed prescriptively. Also, no changes were made to
general sections of SW-846 to the extent they apply to MDPs. The
analytical methods in Update V are considered guidance, provide a basic
standard operating procedure, and may be modified where appropriate.
In addition, included in the original Update V Notice, was ``The
ORCR Policy Statement,'' which was developed as a result of
stakeholders' discussions regarding a need for clarification of the
status and definitions (e.g., validated, final, superseded) of methods
in SW-846. For example, the policy statement is clear that ``the most
recent version'' of an approved method in SW-846, should be used,
unless an existing permit, consent decree, etc.) This policy statement
appeared in the original Update V Federal Register Notice. See: October
23, 2013 (78 FR 63188-63190), and has been inserted in SW-846 in the
table of contents after the Preface. For more information on the policy
statement see: http://www.epa.gov/wastes/hazard/testmethods/sw846/online/index.htm. The Agency further notes that its Quality Assurance/
Quality Control (QA/QC) guidance (e.g., lower limit of quantitation
(LLOQ), relative standard error (RSE), initial demonstration of
proficiency (IDP), etc.), while it appears in Chapter One, is also
discussed in appropriate sections of the individual methods. Updated V
documents are dated July 2014, even though this Update is announced
publicly in this 2015 Federal Register Notice. The July 2014 documents
are identified as ``Update V'' in the document footer.
Table 1 provides a listing of the five revised chapters and 23
methods in this Update V.
Table 1--Final Update V
[Methods, Chapters and Guidance]
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Analytical method No. Method or chapter title
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Table of Contents.
Chapter One--Quality Control.
Chapter Two--Choosing the
Correct Procedure.
Chapter Three--Inorganic
Analytes.
Chapter Four--Organic Analytes.
Chapter Five--Miscellaneous
Test Methods.
1030................................... Ignitability of Solids.
3200 *................................. Mercury Species Fractionation
and Quantification by
Microwave-Assisted Extraction,
Selective Solvent Extraction
and/or Solid Phase Extraction.
3511 *................................. Organic Compounds in Water by
Microextraction.
3572 *................................. Extraction of Wipe Samples for
Chemical Agents.
3620C.................................. Florisil Cleanup.
4025 *................................. Screening for Polychlorinated
Dibenzodioxins and
Polychlorinated Dibenzofurans
(PCDD/Fs) by Immunoassay.
4430 *................................. Screening for Polychlorinated
Dibenzo-p-Dioxins and Furans
(PCDD/Fs) by Aryl Hydrocarbon
Receptor PCR Assay.
4435 *................................. Method for Toxic Equivalent
(TEQS) Determination for
Dioxin-Like Chemical Activity
With the CALUX[supreg]
Bioassay.
[[Page 48524]]
5021A.................................. Volatile Organic Compounds in
Various Sample Matrices Using
Equilibrium Headspace
Analysis.
6010D.................................. Inductively Coupled Plasma-
Atomic Emission Spectrometry.
6020B.................................. Inductively Coupled Plasma-Mass
Spectrometry.
6800................................... Elemental and Speciated Isotope
Dilution Mass Spectrometry.
8000D.................................. Determinative Chromatographic
Separations.
8021B.................................. Aromatic and Halogenated
Volatiles by Gas
Chromatography Using
Photoionization and/or
Electrolytic Conductivity
Detectors.
8111................................... Haloethers by Gas
Chromatography.
8270D.................................. Semivolatile Organic Compounds
by Gas Chromatography/Mass
Spectrometry.
8276 *................................. Toxaphene and Toxaphene
Congeners by Gas
Chromatography/Negative Ion
Chemical Ionization Mass
Spectrometry (GC-NICI/MS).
8410................................... Gas Chromatography/Fourier
Transform Infrared
Spectrometry for Semivolatile
Organics: Capillary Column.
8430................................... Analysis of Bis(2-
Chloroethyl)Ester and
Hydrolysis Products by Direct
Aqueous Injection.
9013A.................................. Cyanide Extraction Procedure
for Solids and Oils.
9014................................... Titrimetric and Manual
Spectrophotometric
Determinative Methods for
Cyanide.
9015 *................................. Metal Cyanide Complexes by
Anion Exchange Chromatography
and UV Detection.
9320................................... Radium 228.
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* New Method
V. What revisions are discussed in this notice?
A. SW-846 Chapters One Through Five and QA/QC Guidance
SW-846 contains the following 13 chapters, which provide additional
guidance when conducting sample collection, preparation, treatment and
disposal. The first five chapters were revised and/or updated in
accordance with Update V method revisions. All the chapter titles for
SW-846 are listed in Table 2.
Table 2--SW-846 Chapters
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CHAPTER ONE....................... QUALITY CONTROL.
CHAPTER TWO....................... CHOOSING THE CORRECT PROCEDURE.
CHAPTER THREE..................... INORGANIC ANALYTES.
CHAPTER FOUR...................... ORGANIC ANALYTES.
CHAPTER FIVE...................... MISSCELLANEOUS TEST METHODS.
CHAPTER SIX....................... PROPERTIES.
CHAPTER SEVEN..................... CHARACTERISTIC INTRODUCTION AND
REGUALTORY DEFINITIONS.
CHAPTER EIGHT..................... METHODS FOR DETERMINING
CHARACTERISTICS.
CHAPTER NINE...................... SAMPLING PLAN.
CHAPTER TEN....................... SAMPLING METHODS.
CHAPTER ELEVEN.................... GROUND WATER MONITORING.
CHAPTER TWELVE.................... LAND TREATMENT MONITORING.
CHAPTER THIRTEEN.................. INCINERATION.
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The date that the technical workgroup officially updated the
methods is also displayed in the footer of Update V methods and
chapters. Specifically, discussion of the comments and the Agency's
responses follow:
Chapter One (Quality Control)
The Agency received 20 comments on Chapter One. Most comments were
favorable. For those that were not, the comments mainly focused on the
interpretation of terminology used (e.g., Field Blank, Sensitivity,
Limit of Quantitation (LOQ), Reproducibility, etc.). Changes to this
terminology have been added to the glossary section. The Agency has
revised Chapter One for clarity of terminology. The final guidance is
more user friendly and more consistent with the Agency's official
guidance on QA/QC implementation and procedures (e.g., Quality
Assurance Project Plans (QAPPs), DQOs, and the Flexible Approach to
Environmental Measurement), located at: http://www.epa.gov/quality/qa_docs.html#noneparqt. Revisions were also made to improve and clarify
the language on LLOQ and blank contamination. In addition, EPA added
and revised several QA/QC concepts in Chapter One. The concepts are now
included in Chapter One (Quality Control) and individual methods where
appropriate. These changes are described below:
Lower Limit of Quantitation (LLOQ)--The Agency received 35 comments
on the LLOQ concept. Most comments were favorable. As discussed in the
October 2013 Federal Register notice, the Agency recommends
establishing the LLOQ as the lowest point of quantitation, which in
most cases is the concentration of the lowest calibration standard in
the calibration curve that has been adjusted for the preparation mass
and/or volume. The LLOQ value is a function of both the analytical
method and the sample being evaluated.
The Method Detection Limit (MDL) procedure in 40 CFR part 136,
Appendix B, for the determination of MDLs developed for the Clean Water
Act (CWA) program uses a clean matrix (i.e., reagent water for
preparing ``spiked'' samples, or samples with known constituent
concentrations). Analytical laboratories often have difficulty
demonstrating they can meet
[[Page 48525]]
the MDL established using Part 136 when evaluating complex matrices,
such as wastes (e.g., soils, sludges, wipes, and spent materials). This
MDL approach generally yields unrealistic and/or unachievable method
detection limits for these complex matrices. Since the current Part 136
procedure is generally not suitable for RCRA wastes or materials
encountered under the RCRA program, the Agency has chosen to finalize
the LLOQ for SW-846. The procedure outlined in Part 136 is currently
under review and is being revised for consideration in a future
rulemaking effort. The LLOQ considers the effect of sample matrix
(e.g., components of a sample other than the analyte) by taking the
LLOQ sample through the entire analytical process, including sample
preparation, clean up (to remove sample interferences), and
determinative procedures. Lastly, results above the LLOQ are
quantifiable within acceptable precision and bias. Thus, the LLOQ
approach better suits the needs of the RCRA program, because it
provides reliable and defensible results, especially at the lower level
of quantitation, and can be reported with a known level of confidence
for the complex matrices being evaluated. The Agency uses MDLs in some
of the MDPs and understands that other Agency programs may continue to
use MDLs to meet their program use and needs (e.g., the National
Pollutant Discharge Elimination System (NPDES) permit program).
Since the current MDL procedure is not suitable for complex
matrices found in RCRA waste, references to the MDL have been replaced
with the LLOQ for non-regulatory methods (guidance). As the regulations
are revised, the RCRA program will remove the MDL reference from the
MDPs and replace it with the LLOQ concept where appropriate.
The Agency refined the procedure for establishing the LLOQ. This
refinement considers sample matrix effects; includes a provision to
verify the reasonableness of the reported quantitation limit (QL); and
recommends a frequency of LLOQ verification (found in Chapter One and
each method) to be balanced between rigor and practicality.
The Agency understands that previous versions of methods published
in SW-846 may contain the MDL reference and as methods are updated, the
Agency will remove references to the MDLs. The Agency will also remove
MDL references in older methods that have not yet been updated, as time
and resources allow. References in MDPs will be revised in a future
effort since they can only be revised through a notice and comment
rulemaking effort. The Agency recommends the use of LLOQ, as
appropriate, for the non-MDP methods that have not yet been updated.
See Section 9.8 in Method 6020B for Inorganic analytes and Section 9.7
in Method 8000 for Organic analytes on LLOQ for further information on
implementation. Also, if method users choose to run the LLOQ sample, it
must be run with each batch to see if it meets the established
acceptance criteria. Lastly, results above the LLOQ are quantifiable
within an acceptable precision and bias. Thus, the LLOQ approach better
suits the needs of the RCRA program, because it provides reliable and
defensible results, especially at the lower level of quantitation, and
can be reported with a known level of confidence for the complex
matrices being evaluated. Various programs use SW-846 methods in
implementing different statutes, including RCRA, the Comprehensive
Environmental Response, Compensation, and Liability Act (CERCLA), the
Toxic Substances Control Act (TSCA), the Oil Pollution Act, Homeland
Security Presidential Directives and Presidential Policy Directives,
for waste and materials characterization, compliance testing, site/
incident characterization and extent of contamination, risk assessment,
and remediation for protection of human health and the environment, and
better management and use of wastes and materials, for a wide range of
difficult matrices. The Agency believes that the LLOQ approach is an
important improvement and supports the essential need to provide data
that are verified to meet the precision and accuracy requirements of
the RCRA program.
Establishing the LLOQ for Inorganic Analytes--When performing
methods for inorganic analyses, the LLOQ should be verified by the
analysis of at least seven replicate samples (prepared in a clean
matrix or control material) and spiked at the LLOQ and processed
through all preparation and analysis steps of the method. The mean
recovery and relative standard deviation (RSD) of these samples provide
an initial statement of precision and bias at the LLOQ. In most cases,
the mean recovery should be no more than 35% of the true
value and the RSD should be <=20%. Ongoing LLOQ verification, at a
minimum, is on a quarterly basis to validate quantitation capability at
low analyte concentration levels. This verification may be accomplished
either with clean control material (e.g., reagent water, method blanks,
Ottawa sand, diatomaceous earth, etc.) or a representative sample
matrix free of target compounds. Optimally, the LLOQ should be less
than the desired regulatory action levels based on the stated project-
specific requirements. For more information, please see the individual
methods (e.g., Methods 6010 and 6020) and Chapter One of SW-846.
Establishing LLOQ for Organic Analytes--When performing methods for
organic analyses, the LLOQ should be verified using either a clean
control material (e.g., reagent water, method blanks, Ottawa sand,
diatomaceous earth, etc.) or a representative sample matrix free of
target compounds. Optimally, the LLOQ should be less than the desired
regulatory action levels based on the stated project-specific
requirements.
For organic analyses, the acceptable recovery ranges of target
analytes will vary more than for other types of analyses, such as
inorganics. The recovery of target analytes in the LLOQ check sample
should be within established limits, or other such project-required
acceptance limits, for precision and bias to verify the data reporting
limits. Until the laboratory has sufficient data to determine
acceptance limits statistically, the laboratory control sample (LCS)
criterion, +20% (i.e., lower limit minus 20% and upper limit plus 20%)
may be used for an acceptable range for the LLOQ. This approach
acknowledges the poorer overall response at the low end of the
calibration curve. Historically based LLOQ acceptance criteria should
be determined as soon as practical once sufficient data points have
been acquired.
In-house limits (which a laboratory establishes) for bias (e.g., %
Recovery) and precision (e.g., Relative Percent Difference (%RPD)) of
the LLOQ for a particular sample matrix may be calculated when
sufficient data points exist. The laboratory should have a documented
procedure for establishing its in-house acceptance ranges. Sometimes
the laboratory instrument and/or analyst performance vary or test
samples cause problems with the detector (e.g., samples may have
interferences; may clog the instruments cells, wall or tube; may cause
contamination; etc.). Therefore, a laboratory establishes the limits of
acceptance (for precision and bias) with sufficient data to demonstrate
that they can report down to the LLOQ with a certain level of
confidence. As an alternative, a QAPP may include the acceptance limits
(for precision and bias) for LLOQ at the project level through the DQOs
it includes. The
[[Page 48526]]
frequency of the LLOQ check is not specified for organic analytes.
Note: The LLOQ check sample should be spiked with the analytes
of interest at the predicted LLOQ concentration levels and carried
through the same preparation and analysis procedures as
environmental samples and other QC samples. For more information,
please see individual methods (e.g., Method 8000) and Chapter One of
SW-846.
Use of the LLOQ--The RCRA program deals with complex wastes and
materials that are managed or used in many different ways (e.g.,
landfilling, land application, incineration, recycling). The thresholds
(e.g., action or clean up levels) for data users (e.g., engineers or
risk assessors) to make their decisions, therefore, vary. Method users
will need to properly plan their analytical strategy to ensure the
LLOQs for targeted analytes are lower than the thresholds needed to
generate data used to determine how waste or materials can be properly
managed or used.
Initial Demonstration of Performance (IDP)--The IDP serves as a
procedure that the laboratory conducts to demonstrate the ability to
generate results with acceptable accuracy and precision for each
preparation and determinative method they perform. Detailed discussion
can be found in the October 23, 2013 Federal Register notice.
The Agency did not receive any comments on the IDP, and has
finalized the language as presented in the original notice. Language
regarding the IDP has been specified in the individual Update V methods
where appropriate (e.g. Methods 6010D, 6020B, 8000D and many others).
The IDP changes allow laboratories to use their time and resources
effectively, especially for the organic analyses. The IDP section for
the Determination of Organic Analytes was expanded to describe two
situations: When a significant change to instrumentation or procedure
occurs: Reliable performance of the methods depends on careful
adherence to the instructions in the written method because many
aspects of the method are mandatory to ensure the method performs as
intended.
Therefore, if a major change to the sample preparation procedure is
made (e.g., a change of solvent), the IDP must be repeated for that
preparation procedure to demonstrate the laboratory technician's
continued ability to reliably perform the method. The Agency considers
conducting IDPs as part of good laboratory practice procedures and has
already included these procedures in the Agency's laboratories'
practices. Alterations in instrumental procedures only (e.g., changing
Gas Chromatograph (GC) temperature programs or High Performance Liquid
Chromatography (HPLC) mobile phases or the detector interface), require
a new calibration, but not a new IDP because the preparation procedure
is unchanged.
When new staff members are trained: A new analyst needs to be
capable of performing the method, or portion of the method, for which
he/she is responsible. For example, when analysts are trained for a
subset of analytes for an 8000 series method, the new sample
preparation analyst should prepare reference samples for a
representative set of analytes (e.g., the primary analyte mix for
Method 8270, or a mixture of Aroclor 1016 and 1260 for Method 8082) for
each preparation method the analyst will perform. The instrument
analyst being trained will need to analyze the prepared samples (e.g.,
semi-volatile extracts). After several training opportunities, the
analyst will be expected to perform the preparation and determinative
step on his/her own and meet the acceptable QA/QC criteria.
Blank Contamination--Another area that affects sample results and
is expanded upon in this notice and addressed in Chapter One and the
individual methods is blank contamination. The results from analyzing
blanks are generally considered to be acceptable if target analyte
concentrations are less than \1/2\ the LLOQ or are less than project-
specific requirements. Blanks may contain analyte concentrations
greater than acceptance limits if the associated samples in the batch
are unaffected (i.e., targets are not present in samples or sample
concentrations are >=10X the blank). Other criteria may be used
depending on the needs of the project. For method specific details see
Methods 6010 and 6020 for inorganics and Method 8000 for organics.
Relative Standard Error (RSE)--The Agency included RSE as an option
(in addition to calculation of the % error) in Update V of SW-846 for
the determination of the acceptability for a linear or non-linear
calibration curve. The Agency received several comments from two
commenters on RSE. The Agency agrees that Method 8000D, Section
11.5.6.1 on RSE should not be grouped with RSD and r\2\ (Regression
Coefficient) but with % Error. Standard deviation (SD) and r\2\ are
indicators for checking the validity of different calibration methods
of response factor and least square linear regression techniques,
respectively. RSE is not equivalent or similar to RSD or r\2\, but
similar to % Error and may be used to evaluate the ``goodness of fit''
of a calibration curve.
To avoid confusion with RSD, RSE has been moved to Section 11.5.4.2
of Method 8000D. In addition, the first sentence in Section 11.5.6.1 of
Method 8000D has been changed to read as follows: ``Corrective action
may be needed if the calibration criteria (RSD/r\2\ and % Error/RSE)
are not met.'' Some corrective actions may include running a new
calibration, preparing fresh standards or performing instrument
maintenance. The laboratory's SOPs should address how to handle and
document these types of problems when encountered.
RSE refits the calibration data back to the calibration model and
evaluates the difference between the measured and the true amounts or
concentrations used to create the model.
[GRAPHIC] [TIFF OMITTED] TN13AU15.000
Where:
xi = True amount of analyte in calibration level i, in
mass or concentration units.
x[acute]i = Measured amount of analyte in calibration
level i, in mass or concentration units.
p = Number of terms in the fitting equation (average = 1, linear =
2, quadratic = 3, cubic = 4)
n = Number of calibration points.
The RSE acceptance limit criterion for the calibration model is the
same as the RSD limit in the determinative method.
If the RSD limit is not defined in the determinative method, the
RSE limit should be set at <=20% for good performing compounds and
<=30% for poor performing compounds.
Chapter Two (Choosing the Correct Procedure)
The Agency received 12 comments on Chapter Two. Most comments were
favorable, and others were editorial in nature. Therefore, the Agency
has revised and finalized the Table of Contents to add the new and
revised methods from Update V to the SW-846 compendium. Method titles
from the 8000 series were added to Section 2.2.3 for completeness.
Other tables were revised to include additional analytes as
appropriate. In addition, a typographical error for bis(2-
chloroisopropyl) ether was corrected to bis(2-chloro-1-methylethyl)
ether in Tables 2-1, 2-4, 2-15, 2-22, and 2-34. This correction is
consistent with the most common way to identify this compound. New
compounds were also added to Tables 2-1, 2-6, 2-20, 2-23A, 2-29A, 2-30,
2-31, 2-35A, 2-36A, 2-41, 2-45 and 2-46.
[[Page 48527]]
Furthermore, Table 2-40(A) includes the current sample preservation
guidance for styrene and vinyl chloride in aqueous samples (i.e.,
deletion of previously recommended practice of collecting a second set
of samples without acid preservatives and analyzing immediately, if
styrene and vinyl chloride are analytes of interest), and Table 2-40(B)
includes Mercury Speciation hold times in addition to totals. Figure 2-
2 was updated to include the most up-to-date guidance and to streamline
the flowchart.
Chapter Three (Inorganic Analytes)
The Agency received six comments on Chapter Three. Most comments
were favorable, and the Agency made the appropriate editorial and
clarification changes (e.g., removed reference to trip blank in Section
3.3.2, title change to Table 3-2 Digestion Volume/Mass, etc.). The
change included finalizing the revised definition for Instrument
Detection Limit (IDL) to be consistent with the revised Methods 6010D
and 6020B. In addition, the term ``bias'' has replaced ``accuracy''
where appropriate; the definition for linear range is now consistent
with Methods 6010D and 6020B. The definition for the spectral
interference check (SIC) solution has replaced the definition for the
interference check sample (ICS) and is consistent with Methods 6010D
and 6020B. The definition of LCS (laboratory control sample) recommends
the use of a spiking solution from the same source as the calibration
standards. Sections 3.6 and 3.7 were finalized to include the
collision/reaction cell technology as an effective method for removing
isobaric interferences when analyzing by ICP-MS. Table 3-2 now includes
a minimum mass of 100 g for solid samples collected for sulfide
analysis.
Chapter Four (Organic Analytes)
The Agency received nine comments on Chapter Four. Most comments
focused on Table 4-1, which has now been finalized to exclude the
recommendation to collect a second set of samples without adding an
acid preservative and analyze in a shorter time frame if vinyl chloride
and styrene are analytes of concern for aqueous samples. A study showed
that there were no significant differences in sample recovery of those
samples preserved with acid versus those not preserved. Other comments
were minor, and appropriate revisions have been made adding additional
methods to section 4.3.3.
Chapter Five (Miscellaneous Test Methods)
The Agency did not receive any comments on Chapter Five. Chapter
5's changes were general (i.e., updated format changes and method
reference to chapters), and it was finalized as appropriate.
Chapter Nine (Sampling Plan)
The Agency also received comments on Chapter Nine, which was not
open for comment. However, the Agency will consider those comments in a
future update.
B. Methods Revisions
Significant revisions were finalized regarding Methods 6010D,
6020B, and 8000D, and are discussed in this notice. Many methods were
revised based on technical and editorial comments received during the
comment period. More detailed discussions and responses to all comments
received on Update V can be found in the Response to Comments
Background Document in the RCRA Docket at: (EPA-HQ-RCRA-2012-0072). A
summary of significant comments has been provided.
Method 6010D (Inductively Coupled Plasma--Atomic Emission
Spectrometry)--The Agency received 12 comments on Method 6010D. Most
comments were favorable and applauded consistency revisions between
methods and chapters. Several commenters requested that the guidance
should clarify how to establish the LLOQ for inorganic methods in
instances when regulatory limits are much lower than the lowest
calibration standard. In response, the Agency added language to address
the reporting of flagged data and other options in interpreting data
when the desired LLOQ has not been met. In addition, revisions were
made where technical and editorial comments were appropriate (e.g.,
title changes and relevant information specific to inorganics or
organics). See section 9.8 of the method for more information on
interpreting the LLOQ.
In addition, the Agency received other comments regarding
clarification of the method blank acceptance criteria and definitions
(such as Instrument Detection Limit procedure (IDL)) which can be found
in detail in Method 6010D.
Method 6020B (Inductively Coupled Plasma-Mass Spectrometry)--The
Agency received nine comments on Method 6020B. Many comments pertained
to the Initial Calibration Blank (ICB), when multi-calibration
standards are used, and the LLOQ. The Agency agreed with the commenter
and revised the appropriate section in Method 6020 to read as follows:
``If the ICB consistently has target analyte concentrations greater
than half the LLOQ, the LLOQ should be re-evaluated.'' In addition, the
Agency has clarified the statement that if there is no regulatory limit
and the method blank is >10% of the lowest sample concentration, then
the method blank may be considered to be acceptable if 10X the concentration in the blank. The data
may also be reported with flags, which is a new option in this version
of Method 8000.
Seven comments were related to QC sample frequency and control
limits. One commenter requested that a numerical limit for LLOQ
standard recovery be used. The users are encouraged to develop
statistical acceptance limits rather than to default to a set of
numerical limits in the method. The suggested criteria remain 20% of the laboratory's control sample (LCS) limits. Another
commenter objected to removal of the word ``must'' from some
calibration criteria (such as calibration coefficients). The Agency
confirmed the intention to allow the project requirements to be
flexible. The laboratories are also instructed to perform corrective
actions whenever calibration criteria for their project requirements
are not met. Some other suggestions were not adopted (such as a
requirement to run an end continuing calibration verification (CCV) for
every 8000 series method or to require all extraction QC from a batch
to be run on the same instrument as every sample and/or dilutions
thereof). The Agency's view is that the methods should remain flexible
and more restrictive QC requirements (where needed) should be listed in
the determinative methods.
[[Page 48528]]
One commenter requested the inclusion of an additional reference
(the Department of Defense Quality Systems Manual, Version 5.0 (DOD QSM
5.0)) as The Agency used it in developing Update V. The Agency agrees,
and added the reference.
Methods 8021B (Aromatic and Halogenated Volatiles by Gas
Chromatography Using Photoionization and/or Electrolytic Conductivity
Detectors), 8111 (Haloethers by Gas Chromatography), and 8430 (Analysis
of Bis(2-chloroethyl) Ether and Hydrolysis Products by Direct Aqueous
Injection GC/FT-IR)--The Agency received the same two comments for
these three methods. Both comments concurred with the nomenclature
change for bis(2-chloro-1-methylethyl)ether, which alleviated
confusion.
Method 8270D (Semivolatile Organic Compounds by Gas Chromatography/
Mass Spectrometry (GC/MS))--The Agency received two comments which
concurred with the nomenclature change for bis(2-chloro-1-
methylethyl)ether. Method 8270D also received one comment asking about
the possibility of reporting flagged data from calibrations where some
compounds were outside the specified criteria. The Agency's RCRA
Organic Workgroup is discussing this issue and intends to address it in
Update VI.
Method 8410D Gas Chromatography/Fourier Transform Infrared (GC/FT-
IR) Spectrometry for Semivolatile Organics: Capillary Column--The
Agency received two comments on Method 8410D which concurred with the
nomenclature change for bis(2-chloro-1-methylethyl)ether. Method 8410D
also received one comment discussing the acceptable temperature range
of samples for preservation. The Agency accepted the updated change.
Method 9014 (Titrimetric and Manual Spectrophotometric
Determinative Methods for Cyanide)--Detailed information on calibration
models and their acceptance criteria are not included in each SW-846
method. This is because these methods are intended as general guidance,
as are all of the methods discussed in this notice. For any test method
which is not a method-defined parameter (MDP), the intention is to
allow the laboratory flexibility under the Methods Innovation Rule
(MIR).\3\ The details of how a laboratory will conduct and approve
calibrations should be included in the individual laboratory's Quality
Management Plan (QMP) or in its Standard Operating Procedure (SOP) for
each method.
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\3\ See 70 FR 34537, June 14, 2005 Federal Register.
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Method 9040 (pH Electrometric Measurement)--This method is a Method
Defined Parameter (MDP) and the Agency cannot revise an MDP through a
Notice of Availability, but instead must use notice-and-comment
rulemaking procedures. During a future rulemaking effort, the Agency
will consider those comments on MDPs that may require rulemaking.
V. Summary
These changes in Update V will assist method users in demonstrating
method competency and in generating better quality data. For the
convenience of the analytical community, the Agency will revise the
OSWER Methods' Team homepage on The Agency's Web site to include the
final Update V. Also, please see the Web site: http://www.epa.gov/epawaste/hazard/testmethods/index.htm for more information. Table 1
provides a listing of the five chapters and 23 methods (8 new methods
and 15 revised methods) in Update V.
Dated: July 22, 2015.
Barnes Johnson,
Director, Office of Resource Conservation and Recovery.
[FR Doc. 2015-20030 Filed 8-12-15; 8:45 am]
BILLING CODE 6560-50-P