
[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: 
kirkland.kim@epa.gov.

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]
------------------------------------------------------------------------
         Analytical method No.               Method or chapter title
------------------------------------------------------------------------
                                         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.
------------------------------------------------------------------------
* 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
------------------------------------------------------------------------
 
------------------------------------------------------------------------
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.
------------------------------------------------------------------------

    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


