80_FR_48678 80 FR 48522 - Waste Management System; Testing and Monitoring Activities; Notice of Availability of Final Update V of SW-846

80 FR 48522 - Waste Management System; Testing and Monitoring Activities; Notice of Availability of Final Update V of SW-846

ENVIRONMENTAL PROTECTION AGENCY

Federal Register Volume 80, Issue 156 (August 13, 2015)

Page Range48522-48528
FR Document2015-20030

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.

Federal Register, Volume 80 Issue 156 (Thursday, August 13, 2015)
[Federal Register Volume 80, Number 156 (Thursday, August 13, 2015)]
[Notices]
[Pages 48522-48528]
From the Federal Register Online  [www.thefederalregister.org]
[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]
------------------------------------------------------------------------
         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.
---------------------------------------------------------------------------

    \3\ See 70 FR 34537, June 14, 2005 Federal Register.
---------------------------------------------------------------------------

    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



                                              48522                       Federal Register / Vol. 80, No. 156 / Thursday, August 13, 2015 / Notices

                                                 Persons unable to file electronically                guidance since the changes in this                    IV. What does final Update V contain?
                                              should submit an original and 5 copies                  document to the SW–846 analytical                     V. What revisions are discussed in this
                                              of the intervention or protest to the                   methods are not required by RCRA’s                         Notice?
                                              Federal Energy Regulatory Commission,                   hazardous waste regulations. Any                      VI. Summary
                                              888 First Street NE., Washington, DC                    required analytical methods have not                  II. What is the subject and purpose of
                                              20426.                                                  been changed.                                         this Notice?
                                                 The filings in the above-referenced                  FOR FURTHER INFORMATION CONTACT: Kim                     The Agency is announcing
                                              proceeding are accessible in the                        Kirkland, Office of Resource                          publication of Final Update V to ‘‘Test
                                              Commission’s eLibrary system by                         Conservation and Recovery (5304P),                    Methods for Evaluating Solid Waste,
                                              clicking on the appropriate link in the                 Environmental Protection Agency, 1200                 Physical/Chemical Methods,’’ EPA
                                              above list. They are also available for                 Pennsylvania Avenue NW., Washington,                  publication SW–846, which is now part
                                              electronic review in the Commission’s                   DC 20460–0002; telephone number:                      of the SW–846 methods compendium.
                                              Public Reference Room in Washington,                    (703) 308–8855, fax number: (703) 308–                Specifically, Update V of SW–846
                                              DC. There is an eSubscription link on                   0509, email address: kirkland.kim@                    contains revisions to the first five
                                              the Web site that enables subscribers to                epa.gov.                                              chapters of SW–846 and 23 new and
                                              receive email notification when a
                                                                                                      SUPPLEMENTARY INFORMATION:                            modified analytical methods that the
                                              document is added to a subscribed
                                                                                                                                                            Agency has evaluated, and/or revised
                                              docket(s). For assistance with any FERC                 I. General Information                                and determined to be appropriate and
                                              Online service, please email
                                                                                                      A. Does this action apply to me?                      may be used for monitoring or
                                              FERCOnlineSupport@ferc.gov. or call
                                                                                                                                                            complying with the RCRA hazardous
                                              (866) 208–3676 (toll free). For TTY, call                 This notice is directed to the public
                                                                                                                                                            waste regulations. Eight of the 23
                                              (202) 502–8659.                                         in general. It may, however, be of
                                                                                                                                                            methods are new methods that have
                                                Dated: August 6, 2015.                                particular interest to those conducting
                                                                                                                                                            been fully validated, i.e., they have
                                              Nathaniel J. Davis, Sr.,                                waste sampling and analysis for RCRA-
                                                                                                                                                            completed technical and Agency
                                                                                                      related activities. This universe might
                                              Deputy Secretary.                                                                                             workgroup review and approval. In
                                                                                                      include any entity that generates, treats,
                                              [FR Doc. 2015–19887 Filed 8–12–15; 8:45 am]                                                                   addition these eight new methods are
                                                                                                      stores, or disposes of hazardous or
                                              BILLING CODE 6717–01–P                                                                                        being announced in the Federal
                                                                                                      nonhazardous solid waste and might
                                                                                                                                                            Register through this notice. Since the
                                                                                                      also include any laboratory that
                                                                                                                                                            methods have completed the approval
                                                                                                      conducts waste sampling and analyses
                                              ENVIRONMENTAL PROTECTION                                                                                      process, they will be removed from the
                                                                                                      for such entities.
                                              AGENCY                                                                                                        ‘‘Validated Methods’’ link at: http://
                                                                                                      B. How can I get copies of Final Update               www.epa.gov/epawaste/hazard/
                                              [EPA–HQ–RCRA–2012–0072; FRL–9929–37–                    V and other related information?                      testmethods/sw846/new_meth.htm and
                                              OSWER]                                                                                                        incorporated in the SW–846 methods
                                                                                                         1. The Agency has established a
                                              Waste Management System; Testing                        docket for this action under Docket ID                compendium at: http://www.epa.gov/
                                              and Monitoring Activities; Notice of                    No. EPA–RCRA–2012–0072; FRL–9901–                     epawaste/hazard/testmethods/sw846/
                                              Availability of Final Update V of                       86–OSWER and FRL–9929–37–OSWER.                       online/index.htm.
                                                                                                                                                               The 15 revised methods have replaced
                                              SW–846                                                  Publicly available docket materials are
                                                                                                                                                            the previous versions in the final update
                                                                                                      available either electronically through
                                              AGENCY: Environmental Protection                                                                              package and will also be placed into the
                                                                                                      www.regulations.gov or in hard copy at
                                              Agency (EPA).                                                                                                 SW–846 methods compendium.
                                                                                                      the OSWER RCRA Docket in the EPA
                                              ACTION: Notice.                                                                                               Because the RCRA hazardous waste
                                                                                                      Docket Center (EPA/DC), EPA West,
                                                                                                                                                            regulations do not require the analytical
                                              SUMMARY: The Environmental Protection
                                                                                                      Room 3334, and 1301 Constitution Ave.
                                                                                                                                                            methods contained in Update V, the
                                              Agency (EPA or Agency) is providing                     NW., Washington, DC. The EPA Docket
                                                                                                                                                            Agency is issuing this update as
                                              notice of the availability of ‘‘Final                   Center Public Reading Room is open
                                                                                                                                                            guidance. This guidance does not add or
                                              Update V’’ to the Third Edition of the                  from 8:30 a.m. to 4:30 p.m., Monday
                                                                                                                                                            change the RCRA regulations, and does
                                              manual, ‘‘Test Methods for Evaluating                   through Friday, excluding legal
                                                                                                                                                            not have any impact on existing
                                              Solid Waste, Physical/Chemical                          holidays. The telephone number for the
                                                                                                                                                            rulemakings associated with the RCRA
                                              Methods,’’ EPA publication SW–846.                      Public Reading Room is (202) 566–1744,
                                                                                                                                                            program. To date, the Agency has
                                              Final Update V contains analytical                      and the telephone number for the
                                                                                                                                                            finalized Updates I, II, IIA, IIB, III, IIIA,
                                              methods, of which 8 are new and 15 are                  OSWER RCRA Docket is (202) 566–
                                                                                                                                                            IIIB, IVA, and IVB to the SW–846
                                              revised. The methods in Update V may                    0270.
                                                                                                                                                            manual, which can be found on the
                                              be used in monitoring or complying                      C. How can I get copies of the Third                  Agency’s ORCR Web page at: http://
                                              with the Resource Conservation and                      Edition of SW–846 its updates?                        www.epa.gov/SW-846.
                                              Recovery Act (RCRA) hazardous waste
                                                                                                         The Third Edition of SW–846, as                    III. Why is the Agency releasing final
                                              regulations. This action includes
                                                                                                      amended by Final Updates I, II, IIA, IIB,             Update V to SW–846?
                                              revisions to the methods in response to
                                                                                                      III, IIIA, IIIB, IVA, IVB, and V, is
                                              comments received on a Notice                                                                                    SW–846 is revised over time as new
                                                                                                      available in pdf format on the Internet
                                              published in the Federal Register on                                                                          information and data become available.
                                                                                                      at http://www.epa.gov/SW-846.
                                              October 23, 2013 and finalizes the                                                                            The Agency continually reviews
tkelley on DSK3SPTVN1PROD with NOTICES




                                              methods and guidance. In addition, the                  D. How is the rest of this Notice                     advances in analytical instrumentation
                                              Agency is also finalizing revisions to                  organized?                                            and techniques and periodically
                                              Chapters One through Five of SW–846                     Sections:
                                                                                                                                                            incorporates such advances into SW–
                                              and an Office of Resource Conservation                  II. What is the subject and purpose of this           846 as method updates by adding new
                                              and Recovery (ORCR) policy statement                         Notice?                                          methods to the manual, and replacing
                                              in the SW–846 methods compendium.                       III. Why is the Agency releasing Update V to          existing methods with revised versions
                                              The Agency is issuing this Update as                         SW–846?                                          of the same method. On October 23,


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                                                                                      Federal Register / Vol. 80, No. 156 / Thursday, August 13, 2015 / Notices                                                                 48523

                                              2013, the Agency published a FR Notice                                        SW–846, specifically seeking                               procedure, and may be modified where
                                              (78 FR 63185), announcing the                                                 clarification about which versions of a                    appropriate.
                                              availability of Update V to SW–846.                                           revised method are recommended, and                           In addition, included in the original
                                              When the comment period closed on                                             seeking clarification in defining                          Update V Notice, was ‘‘The ORCR
                                              January 23, 2014, the Agency received a                                       terminology used to identify the                           Policy Statement,’’ which was
                                              total of 111 technical and general                                            category of methods.                                       developed as a result of stakeholders’
                                              comments on the Update. The Agency                                               The Agency did not receive any                          discussions regarding a need for
                                              revised the methods and chapters based                                        comments regarding the content of the                      clarification of the status and definitions
                                              on comments received, when it was                                             ORCR Policy Statement and has                              (e.g., validated, final, superseded) of
                                              appropriate to do so.                                                         finalized it without change. As a                          methods in SW–846. For example, the
                                                Revisions made were either editorial                                        reminder, the Agency strongly                              policy statement is clear that ‘‘the most
                                              for clarity or technical for accuracy. A                                      recommends the use of the latest                           recent version’’ of an approved method
                                              summary of significant changes are                                            version of an SW–846 method. The                           in SW–846, should be used, unless an
                                              noted in Appendix A of each revised                                           Agency, however, is not imposing                           existing permit, consent decree, etc.)
                                              method.1 In addition, significant                                             restrictions on the use of earlier versions                This policy statement appeared in the
                                              revisions to the chapters are discussed                                       of non-required SW–846 methods or                          original Update V Federal Register
                                              in Section V of this Notice. These                                            precluding the use of previous                             Notice. See: October 23, 2013 (78 FR
                                              methods can be used for any RCRA                                              guidance, if such use is appropriate. For                  63188–63190), and has been inserted in
                                              applications, other than those                                                example, earlier versions of an SW–846                     SW–846 in the table of contents after the
                                              specifically required by regulation. In                                       method may be more appropriate for                         Preface. For more information on the
                                              cases that the regulation does not                                            regulatory purposes (e.g., for                             policy statement see: http://
                                              specify the method, the analyst should                                        compliance with an existing permit or                      www.epa.gov/wastes/hazard/
                                              select an appropriate method in which                                         consent decree), or when new method                        testmethods/sw846/online/index.htm.
                                              the performance can be demonstrated                                           versions may be more costly to run or                      The Agency further notes that its
                                              and meet project-specific Data Quality                                        perform, than necessary for meeting                        Quality Assurance/Quality Control (QA/
                                              Objectives (DQOs). On a related matter,                                       project-specific objectives.                               QC) guidance (e.g., lower limit of
                                              the Agency is also finalizing an ORCR                                                                                                    quantitation (LLOQ), relative standard
                                                                                                                            IV. What does final Update V contain?
                                              Policy Statement that responds to                                                                                                        error (RSE), initial demonstration of
                                              concerns the Environmental Laboratory                                           Final Update V contains revisions to                     proficiency (IDP), etc.), while it appears
                                              Advisory Board (ELAB) has expressed                                           Chapters One through Five of EPA’s                         in Chapter One, is also discussed in
                                              regarding the official version and status                                     publication SW–846. As noted above,                        appropriate sections of the individual
                                              of various methods. ELAB is a                                                 no changes are made to Method Defined                      methods. Updated V documents are
                                              committee established under the                                               Parameters (MDPs), which are required                      dated July 2014, even though this
                                              Federal Advisory Committee Act                                                by the RCRA regulation and must be                         Update is announced publicly in this
                                              (FACA) that advises the Agency on                                             followed prescriptively. Also, no                          2015 Federal Register Notice. The July
                                              measurement, monitoring, and                                                  changes were made to general sections                      2014 documents are identified as
                                              laboratory science issues. The ELAB                                           of SW–846 to the extent they apply to                      ‘‘Update V’’ in the document footer.
                                              contacted the Agency’s Forum on                                               MDPs. The analytical methods in                               Table 1 provides a listing of the five
                                              Environmental Measurements (FEM) 2                                            Update V are considered guidance,                          revised chapters and 23 methods in this
                                              with several issues regarding the use of                                      provide a basic standard operating                         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, Se-
                                                                                                                                           lective 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 Hydro-
                                                                                                                                           carbon Receptor PCR Assay.
tkelley on DSK3SPTVN1PROD with NOTICES




                                              4435 * ...........................................................................         Method for Toxic Equivalent (TEQS) Determination for Dioxin-Like Chemical Activity With
                                                                                                                                           the CALUX® Bioassay.

                                                1 Specifically, this summary of significant                                 of the method. EPA also intends to include such            measurement issues, and provide an internal and
                                              changes (Appendix A) is included in each newly-                               summaries in future method revisions.                      external contact point for addressing measurement
                                                                                                                              2 The FEM is a standing committee of senior EPA
                                              revised method referenced in this notice, to assist                                                                                      methodology, monitoring, and laboratory science
                                              users in identifying changes from the prior version                           managers established in 2003 to promote                    issues with multi-program impacts.
                                                                                                                            consistency and consensus within the EPA on



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                                              48524                                    Federal Register / Vol. 80, No. 156 / Thursday, August 13, 2015 / Notices

                                                                                                                        TABLE 1—FINAL UPDATE V—Continued
                                                                                                                                    [Methods, Chapters and Guidance]

                                                                       Analytical method No.                                                                              Method or chapter title

                                              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                                    guidance when conducting sample                           chapter titles for SW–846 are listed in
                                              notice?                                                                    collection, preparation, treatment and                    Table 2.
                                              A. SW–846 Chapters One Through Five                                        disposal. The first five chapters were
                                              and QA/QC Guidance                                                         revised and/or updated in accordance
                                                                                                                         with Update V method revisions. All the
                                                SW–846 contains the following 13
                                              chapters, which provide additional
                                                                                                                                   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                                    guidance on QA/QC implementation                          October 2013 Federal Register notice,
                                              officially updated the methods is also                                     and procedures (e.g., Quality Assurance                   the Agency recommends establishing
                                              displayed in the footer of Update V                                        Project Plans (QAPPs), DQOs, and the                      the LLOQ as the lowest point of
                                              methods and chapters. Specifically,                                        Flexible Approach to Environmental                        quantitation, which in most cases is the
                                              discussion of the comments and the                                         Measurement), located at: http://                         concentration of the lowest calibration
                                              Agency’s responses follow:                                                 www.epa.gov/quality/qa_                                   standard in the calibration curve that
                                              Chapter One (Quality Control)                                              docs.html#noneparqt. Revisions were                       has been adjusted for the preparation
                                                                                                                         also made to improve and clarify the                      mass and/or volume. The LLOQ value is
                                                The Agency received 20 comments on                                       language on LLOQ and blank                                a function of both the analytical method
                                              Chapter One. Most comments were                                            contamination. In addition, EPA added                     and the sample being evaluated.
                                              favorable. For those that were not, the
                                                                                                                         and revised several QA/QC concepts in                        The Method Detection Limit (MDL)
                                              comments mainly focused on the
                                                                                                                         Chapter One. The concepts are now                         procedure in 40 CFR part 136,
                                              interpretation of terminology used (e.g.,
                                                                                                                         included in Chapter One (Quality                          Appendix B, for the determination of
                                              Field Blank, Sensitivity, Limit of
                                                                                                                         Control) and individual methods where
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                                              Quantitation (LOQ), Reproducibility,                                                                                                 MDLs developed for the Clean Water
                                              etc.). Changes to this terminology have                                    appropriate. These changes are                            Act (CWA) program uses a clean matrix
                                              been added to the glossary section. The                                    described below:                                          (i.e., reagent water for preparing
                                              Agency has revised Chapter One for                                           Lower Limit of Quantitation (LLOQ)—                     ‘‘spiked’’ samples, or samples with
                                              clarity of terminology. The final                                          The Agency received 35 comments on                        known constituent concentrations).
                                              guidance is more user friendly and more                                    the LLOQ concept. Most comments                           Analytical laboratories often have
                                              consistent with the Agency’s official                                      were favorable. As discussed in the                       difficulty demonstrating they can meet


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                                                                          Federal Register / Vol. 80, No. 156 / Thursday, August 13, 2015 / Notices                                           48525

                                              the MDL established using Part 136                      notice and comment rulemaking effort.                 representative sample matrix free of
                                              when evaluating complex matrices,                       The Agency recommends the use of                      target compounds. Optimally, the LLOQ
                                              such as wastes (e.g., soils, sludges,                   LLOQ, as appropriate, for the non-MDP                 should be less than the desired
                                              wipes, and spent materials). This MDL                   methods that have not yet been updated.               regulatory action levels based on the
                                              approach generally yields unrealistic                   See Section 9.8 in Method 6020B for                   stated project-specific requirements. For
                                              and/or unachievable method detection                    Inorganic analytes and Section 9.7 in                 more information, please see the
                                              limits for these complex matrices. Since                Method 8000 for Organic analytes on                   individual methods (e.g., Methods 6010
                                              the current Part 136 procedure is                       LLOQ for further information on                       and 6020) and Chapter One of SW–846.
                                              generally not suitable for RCRA wastes                  implementation. Also, if method users                    Establishing LLOQ for Organic
                                              or materials encountered under the                      choose to run the LLOQ sample, it must                Analytes—When performing methods
                                              RCRA program, the Agency has chosen                     be run with each batch to see if it meets             for organic analyses, the LLOQ should
                                              to finalize the LLOQ for SW–846. The                    the established acceptance criteria.                  be verified using either a clean control
                                              procedure outlined in Part 136 is                       Lastly, results above the LLOQ are                    material (e.g., reagent water, method
                                              currently under review and is being                     quantifiable within an acceptable                     blanks, Ottawa sand, diatomaceous
                                              revised for consideration in a future                   precision and bias. Thus, the LLOQ                    earth, etc.) or a representative sample
                                              rulemaking effort. The LLOQ considers                   approach better suits the needs of the                matrix free of target compounds.
                                              the effect of sample matrix (e.g.,                      RCRA program, because it provides                     Optimally, the LLOQ should be less
                                              components of a sample other than the                   reliable and defensible results,                      than the desired regulatory action levels
                                              analyte) by taking the LLOQ sample                      especially at the lower level of                      based on the stated project-specific
                                              through the entire analytical process,                  quantitation, and can be reported with                requirements.
                                              including sample preparation, clean up                  a known level of confidence for the                      For organic analyses, the acceptable
                                              (to remove sample interferences), and                   complex matrices being evaluated.                     recovery ranges of target analytes will
                                              determinative procedures. Lastly,                       Various programs use SW–846 methods                   vary more than for other types of
                                              results above the LLOQ are quantifiable                 in implementing different statutes,                   analyses, such as inorganics. The
                                              within acceptable precision and bias.                   including RCRA, the Comprehensive                     recovery of target analytes in the LLOQ
                                              Thus, the LLOQ approach better suits                    Environmental Response,                               check sample should be within
                                              the needs of the RCRA program, because                  Compensation, and Liability Act                       established limits, or other such project-
                                              it provides reliable and defensible                     (CERCLA), the Toxic Substances Control                required acceptance limits, for precision
                                              results, especially at the lower level of               Act (TSCA), the Oil Pollution Act,                    and bias to verify the data reporting
                                              quantitation, and can be reported with                  Homeland Security Presidential                        limits. Until the laboratory has
                                              a known level of confidence for the                     Directives and Presidential Policy                    sufficient data to determine acceptance
                                              complex matrices being evaluated. The                   Directives, for waste and materials                   limits statistically, the laboratory
                                              Agency uses MDLs in some of the MDPs                    characterization, compliance testing,                 control sample (LCS) criterion, +20%
                                              and understands that other Agency                       site/incident characterization and extent             (i.e., lower limit minus 20% and upper
                                              programs may continue to use MDLs to                    of contamination, risk assessment, and                limit plus 20%) may be used for an
                                              meet their program use and needs (e.g.,                 remediation for protection of human                   acceptable range for the LLOQ. This
                                              the National Pollutant Discharge                        health and the environment, and better                approach acknowledges the poorer
                                              Elimination System (NPDES) permit                       management and use of wastes and                      overall response at the low end of the
                                              program).                                               materials, for a wide range of difficult
                                                 Since the current MDL procedure is                                                                         calibration curve. Historically based
                                                                                                      matrices. The Agency believes that the                LLOQ acceptance criteria should be
                                              not suitable for complex matrices found
                                                                                                      LLOQ approach is an important                         determined as soon as practical once
                                              in RCRA waste, references to the MDL
                                                                                                      improvement and supports the essential                sufficient data points have been
                                              have been replaced with the LLOQ for
                                                                                                      need to provide data that are verified to             acquired.
                                              non-regulatory methods (guidance). As
                                                                                                      meet the precision and accuracy                          In-house limits (which a laboratory
                                              the regulations are revised, the RCRA
                                                                                                      requirements of the RCRA program.                     establishes) for bias (e.g., % Recovery)
                                              program will remove the MDL reference
                                              from the MDPs and replace it with the                      Establishing the LLOQ for Inorganic                and precision (e.g., Relative Percent
                                              LLOQ concept where appropriate.                         Analytes—When performing methods                      Difference (%RPD)) of the LLOQ for a
                                                 The Agency refined the procedure for                 for inorganic analyses, the LLOQ should               particular sample matrix may be
                                              establishing the LLOQ. This refinement                  be verified by the analysis of at least               calculated when sufficient data points
                                              considers sample matrix effects;                        seven replicate samples (prepared in a                exist. The laboratory should have a
                                              includes a provision to verify the                      clean matrix or control material) and                 documented procedure for establishing
                                              reasonableness of the reported                          spiked at the LLOQ and processed                      its in-house acceptance ranges.
                                              quantitation limit (QL); and                            through all preparation and analysis                  Sometimes the laboratory instrument
                                              recommends a frequency of LLOQ                          steps of the method. The mean recovery                and/or analyst performance vary or test
                                              verification (found in Chapter One and                  and relative standard deviation (RSD) of              samples cause problems with the
                                              each method) to be balanced between                     these samples provide an initial                      detector (e.g., samples may have
                                              rigor and practicality.                                 statement of precision and bias at the                interferences; may clog the instruments
                                                 The Agency understands that                          LLOQ. In most cases, the mean recovery                cells, wall or tube; may cause
                                              previous versions of methods published                  should be no more than ±35% of the                    contamination; etc.). Therefore, a
                                              in SW–846 may contain the MDL                           true value and the RSD should be ≤20%.                laboratory establishes the limits of
                                              reference and as methods are updated,                   Ongoing LLOQ verification, at a                       acceptance (for precision and bias) with
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                                              the Agency will remove references to                    minimum, is on a quarterly basis to                   sufficient data to demonstrate that they
                                              the MDLs. The Agency will also remove                   validate quantitation capability at low               can report down to the LLOQ with a
                                              MDL references in older methods that                    analyte concentration levels. This                    certain level of confidence. As an
                                              have not yet been updated, as time and                  verification may be accomplished either               alternative, a QAPP may include the
                                              resources allow. References in MDPs                     with clean control material (e.g., reagent            acceptance limits (for precision and
                                              will be revised in a future effort since                water, method blanks, Ottawa sand,                    bias) for LLOQ at the project level
                                              they can only be revised through a                      diatomaceous earth, etc.) or a                        through the DQOs it includes. The


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                                              48526                       Federal Register / Vol. 80, No. 156 / Thursday, August 13, 2015 / Notices

                                              frequency of the LLOQ check is not                      only (e.g., changing Gas Chromatograph                evaluate the ‘‘goodness of fit’’ of a
                                              specified for organic analytes.                         (GC) temperature programs or High                     calibration curve.
                                                 Note: The LLOQ check sample should be                Performance Liquid Chromatography                        To avoid confusion with RSD, RSE
                                              spiked with the analytes of interest at the             (HPLC) mobile phases or the detector                  has been moved to Section 11.5.4.2 of
                                              predicted LLOQ concentration levels and                 interface), require a new calibration, but            Method 8000D. In addition, the first
                                              carried through the same preparation and                not a new IDP because the preparation                 sentence in Section 11.5.6.1 of Method
                                              analysis procedures as environmental                    procedure is unchanged.                               8000D has been changed to read as
                                              samples and other QC samples. For more                     When new staff members are trained:                follows: ‘‘Corrective action may be
                                              information, please see individual methods                                                                    needed if the calibration criteria (RSD/
                                              (e.g., Method 8000) and Chapter One of SW–              A new analyst needs to be capable of
                                                                                                      performing the method, or portion of the              r2 and % Error/RSE) are not met.’’ Some
                                              846.
                                                                                                      method, for which he/she is                           corrective actions may include running
                                                 Use of the LLOQ—The RCRA program                     responsible. For example, when analysts               a new calibration, preparing fresh
                                              deals with complex wastes and                           are trained for a subset of analytes for              standards or performing instrument
                                              materials that are managed or used in                                                                         maintenance. The laboratory’s SOPs
                                                                                                      an 8000 series method, the new sample
                                              many different ways (e.g., landfilling,                                                                       should address how to handle and
                                                                                                      preparation analyst should prepare
                                              land application, incineration,                                                                               document these types of problems when
                                                                                                      reference samples for a representative
                                              recycling). The thresholds (e.g., action                                                                      encountered.
                                                                                                      set of analytes (e.g., the primary analyte
                                              or clean up levels) for data users (e.g.,                                                                        RSE refits the calibration data back to
                                                                                                      mix for Method 8270, or a mixture of
                                              engineers or risk assessors) to make                                                                          the calibration model and evaluates the
                                                                                                      Aroclor 1016 and 1260 for Method
                                              their decisions, therefore, vary. Method                                                                      difference between the measured and
                                                                                                      8082) for each preparation method the
                                              users will need to properly plan their                                                                        the true amounts or concentrations used
                                                                                                      analyst will perform. The instrument
                                              analytical strategy to ensure the LLOQs                                                                       to create the model.
                                                                                                      analyst being trained will need to
                                              for targeted analytes are lower than the
                                              thresholds needed to generate data used                 analyze the prepared samples (e.g.,
                                              to determine how waste or materials can                 semi-volatile extracts). After several
                                              be properly managed or used.                            training opportunities, the analyst will
                                                 Initial Demonstration of Performance                 be expected to perform the preparation
                                              (IDP)—The IDP serves as a procedure                     and determinative step on his/her own
                                              that the laboratory conducts to                         and meet the acceptable QA/QC criteria.               Where:
                                              demonstrate the ability to generate                        Blank Contamination—Another area                   xi = True amount of analyte in calibration
                                              results with acceptable accuracy and                    that affects sample results and is                         level i, in mass or concentration units.
                                                                                                      expanded upon in this notice and                      x´i = Measured amount of analyte in
                                              precision for each preparation and                                                                                 calibration level i, in mass or
                                              determinative method they perform.                      addressed in Chapter One and the
                                                                                                                                                                 concentration units.
                                              Detailed discussion can be found in the                 individual methods is blank                           p = Number of terms in the fitting equation
                                              October 23, 2013 Federal Register                       contamination. The results from                            (average = 1, linear = 2, quadratic = 3,
                                              notice.                                                 analyzing blanks are generally                             cubic = 4)
                                                 The Agency did not receive any                       considered to be acceptable if target                 n = Number of calibration points.
                                              comments on the IDP, and has finalized                  analyte concentrations are less than 1⁄2                The RSE acceptance limit criterion for
                                              the language as presented in the original               the LLOQ or are less than project-                    the calibration model is the same as the
                                              notice. Language regarding the IDP has                  specific requirements. Blanks may                     RSD limit in the determinative method.
                                              been specified in the individual Update                 contain analyte concentrations greater                  If the RSD limit is not defined in the
                                              V methods where appropriate (e.g.                       than acceptance limits if the associated              determinative method, the RSE limit
                                              Methods 6010D, 6020B, 8000D and                         samples in the batch are unaffected (i.e.,            should be set at ≤20% for good
                                              many others). The IDP changes allow                     targets are not present in samples or                 performing compounds and ≤30% for
                                              laboratories to use their time and                      sample concentrations are ≥10X the                    poor performing compounds.
                                              resources effectively, especially for the               blank). Other criteria may be used
                                              organic analyses. The IDP section for the               depending on the needs of the project.                Chapter Two (Choosing the Correct
                                              Determination of Organic Analytes was                   For method specific details see Methods               Procedure)
                                              expanded to describe two situations:                    6010 and 6020 for inorganics and                        The Agency received 12 comments on
                                              When a significant change to                            Method 8000 for organics.                             Chapter Two. Most comments were
                                              instrumentation or procedure occurs:                       Relative Standard Error (RSE)—The                  favorable, and others were editorial in
                                              Reliable performance of the methods                     Agency included RSE as an option (in                  nature. Therefore, the Agency has
                                              depends on careful adherence to the                     addition to calculation of the % error)               revised and finalized the Table of
                                              instructions in the written method                      in Update V of SW–846 for the                         Contents to add the new and revised
                                              because many aspects of the method are                  determination of the acceptability for a              methods from Update V to the SW–846
                                              mandatory to ensure the method                          linear or non-linear calibration curve.               compendium. Method titles from the
                                              performs as intended.                                   The Agency received several comments                  8000 series were added to Section 2.2.3
                                                 Therefore, if a major change to the                  from two commenters on RSE. The                       for completeness. Other tables were
                                              sample preparation procedure is made                    Agency agrees that Method 8000D,                      revised to include additional analytes as
                                              (e.g., a change of solvent), the IDP must               Section 11.5.6.1 on RSE should not be                 appropriate. In addition, a typographical
                                              be repeated for that preparation                        grouped with RSD and r2 (Regression                   error for bis(2-chloroisopropyl) ether
                                              procedure to demonstrate the laboratory                 Coefficient) but with % Error. Standard               was corrected to bis(2-chloro-1-
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                                              technician’s continued ability to reliably              deviation (SD) and r2 are indicators for              methylethyl) ether in Tables 2–1, 2–4,
                                              perform the method. The Agency                          checking the validity of different                    2–15, 2–22, and 2–34. This correction is
                                              considers conducting IDPs as part of                    calibration methods of response factor                consistent with the most common way
                                              good laboratory practice procedures and                 and least square linear regression                    to identify this compound. New
                                              has already included these procedures                   techniques, respectively. RSE is not                  compounds were also added to Tables
                                              in the Agency’s laboratories’ practices.                equivalent or similar to RSD or r2, but               2–1, 2–6, 2–20, 2–23A, 2–29A, 2–30, 2–
                                                                                                                                                                                                            EN13AU15.000</GPH>




                                              Alterations in instrumental procedures                  similar to % Error and may be used to                 31, 2–35A, 2–36A, 2–41, 2–45 and 2–46.


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                                                                          Federal Register / Vol. 80, No. 156 / Thursday, August 13, 2015 / Notices                                            48527

                                              Furthermore, Table 2–40(A) includes                     Chapter Five (Miscellaneous Test                      the appropriate section in Method 6020
                                              the current sample preservation                         Methods)                                              to read as follows: ‘‘If the ICB
                                              guidance for styrene and vinyl chloride                   The Agency did not receive any                      consistently has target analyte
                                              in aqueous samples (i.e., deletion of                   comments on Chapter Five. Chapter 5’s                 concentrations greater than half the
                                              previously recommended practice of                      changes were general (i.e., updated                   LLOQ, the LLOQ should be re-
                                              collecting a second set of samples                                                                            evaluated.’’ In addition, the Agency has
                                                                                                      format changes and method reference to
                                              without acid preservatives and                                                                                clarified the statement that if there is no
                                                                                                      chapters), and it was finalized as
                                              analyzing immediately, if styrene and                                                                         regulatory limit and the method blank is
                                                                                                      appropriate.
                                              vinyl chloride are analytes of interest),                                                                     >10% of the lowest sample
                                              and Table 2–40(B) includes Mercury                      Chapter Nine (Sampling Plan)                          concentration, then the method blank
                                              Speciation hold times in addition to                      The Agency also received comments                   may be considered to be acceptable if
                                              totals. Figure 2–2 was updated to                       on Chapter Nine, which was not open                   <LLOQ. In addition, typographical
                                                                                                      for comment. However, the Agency will                 errors were corrected.
                                              include the most up-to-date guidance                                                                             Method 8000D (Determinative
                                              and to streamline the flowchart.                        consider those comments in a future
                                                                                                                                                            Chromatographic Separations)—The
                                                                                                      update.
                                              Chapter Three (Inorganic Analytes)                                                                            Agency received comments on Method
                                                                                                      B. Methods Revisions                                  8000 during the public comment period
                                                 The Agency received six comments                                                                           and an additional four afterward. The
                                                                                                         Significant revisions were finalized
                                              on Chapter Three. Most comments were                                                                          comments received are summarized
                                                                                                      regarding Methods 6010D, 6020B, and
                                              favorable, and the Agency made the                                                                            below in several categories.
                                                                                                      8000D, and are discussed in this notice.
                                              appropriate editorial and clarification                                                                          Eight comments were related to the
                                                                                                      Many methods were revised based on                    use and implementation of the LLOQ
                                              changes (e.g., removed reference to trip                technical and editorial comments
                                              blank in Section 3.3.2, title change to                                                                       and its application to method blanks.
                                                                                                      received during the comment period.                   Several additions and changes were
                                              Table 3–2 Digestion Volume/Mass, etc.).                 More detailed discussions and
                                              The change included finalizing the                                                                            made in the method as a result of these
                                                                                                      responses to all comments received on                 comments. The method blank language
                                              revised definition for Instrument                       Update V can be found in the Response
                                              Detection Limit (IDL) to be consistent                                                                        in Sections 9.2.6.9 through 9.2.6.11 was
                                                                                                      to Comments Background Document in                    updated to reflect that blanks should be
                                              with the revised Methods 6010D and                      the RCRA Docket at: (EPA–HQ–RCRA–
                                              6020B. In addition, the term ‘‘bias’’ has                                                                     considered acceptable if the
                                                                                                      2012–0072). A summary of significant                  concentrations found were below one
                                              replaced ‘‘accuracy’’ where appropriate;                comments has been provided.                           half of the LLOQ (or project DQOs).
                                              the definition for linear range is now                     Method 6010D (Inductively Coupled                  Blanks may contain hits for reported
                                              consistent with Methods 6010D and                       Plasma—Atomic Emission                                compounds if the results in the
                                              6020B. The definition for the spectral                  Spectrometry)—The Agency received 12                  associated samples are >10X the
                                              interference check (SIC) solution has                   comments on Method 6010D. Most                        concentration in the blank. The data
                                              replaced the definition for the                         comments were favorable and                           may also be reported with flags, which
                                              interference check sample (ICS) and is                  applauded consistency revisions                       is a new option in this version of
                                              consistent with Methods 6010D and                       between methods and chapters. Several                 Method 8000.
                                              6020B. The definition of LCS (laboratory                commenters requested that the guidance                   Seven comments were related to QC
                                              control sample) recommends the use of                   should clarify how to establish the                   sample frequency and control limits.
                                              a spiking solution from the same source                 LLOQ for inorganic methods in                         One commenter requested that a
                                              as the calibration standards. Sections                  instances when regulatory limits are                  numerical limit for LLOQ standard
                                              3.6 and 3.7 were finalized to include the               much lower than the lowest calibration                recovery be used. The users are
                                              collision/reaction cell technology as an                standard. In response, the Agency added               encouraged to develop statistical
                                              effective method for removing isobaric                  language to address the reporting of                  acceptance limits rather than to default
                                              interferences when analyzing by ICP–                    flagged data and other options in                     to a set of numerical limits in the
                                              MS. Table 3–2 now includes a                            interpreting data when the desired                    method. The suggested criteria remain
                                              minimum mass of 100 g for solid                         LLOQ has not been met. In addition,                   ±20% of the laboratory’s control sample
                                              samples collected for sulfide analysis.                 revisions were made where technical                   (LCS) limits. Another commenter
                                                                                                      and editorial comments were                           objected to removal of the word ‘‘must’’
                                              Chapter Four (Organic Analytes)                         appropriate (e.g., title changes and                  from some calibration criteria (such as
                                                                                                      relevant information specific to                      calibration coefficients). The Agency
                                                The Agency received nine comments                     inorganics or organics). See section 9.8              confirmed the intention to allow the
                                              on Chapter Four. Most comments                          of the method for more information on                 project requirements to be flexible. The
                                              focused on Table 4–1, which has now                     interpreting the LLOQ.                                laboratories are also instructed to
                                              been finalized to exclude the                              In addition, the Agency received other             perform corrective actions whenever
                                              recommendation to collect a second set                  comments regarding clarification of the               calibration criteria for their project
                                              of samples without adding an acid                       method blank acceptance criteria and                  requirements are not met. Some other
                                              preservative and analyze in a shorter                   definitions (such as Instrument                       suggestions were not adopted (such as a
                                              time frame if vinyl chloride and styrene                Detection Limit procedure (IDL)) which                requirement to run an end continuing
                                              are analytes of concern for aqueous                     can be found in detail in Method 6010D.               calibration verification (CCV) for every
                                              samples. A study showed that there                         Method 6020B (Inductively Coupled                  8000 series method or to require all
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                                              were no significant differences in                      Plasma-Mass Spectrometry)—The                         extraction QC from a batch to be run on
                                              sample recovery of those samples                        Agency received nine comments on                      the same instrument as every sample
                                              preserved with acid versus those not                    Method 6020B. Many comments                           and/or dilutions thereof). The Agency’s
                                              preserved. Other comments were minor,                   pertained to the Initial Calibration Blank            view is that the methods should remain
                                              and appropriate revisions have been                     (ICB), when multi-calibration standards               flexible and more restrictive QC
                                              made adding additional methods to                       are used, and the LLOQ. The Agency                    requirements (where needed) should be
                                              section 4.3.3.                                          agreed with the commenter and revised                 listed in the determinative methods.


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                                              48528                       Federal Register / Vol. 80, No. 156 / Thursday, August 13, 2015 / Notices

                                                 One commenter requested the                          (QMP) or in its Standard Operating                    title 40 of the CFR. CROMERR
                                              inclusion of an additional reference (the               Procedure (SOP) for each method.                      establishes electronic reporting as an
                                              Department of Defense Quality Systems                     Method 9040 (pH Electrometric                       acceptable regulatory alternative to
                                              Manual, Version 5.0 (DOD QSM 5.0)) as                   Measurement)—This method is a                         paper reporting and establishes
                                              The Agency used it in developing                        Method Defined Parameter (MDP) and                    requirements to assure that electronic
                                              Update V. The Agency agrees, and                        the Agency cannot revise an MDP                       documents are as legally dependable as
                                              added the reference.                                    through a Notice of Availability, but                 their paper counterparts. Subpart D of
                                                 Methods 8021B (Aromatic and                          instead must use notice-and-comment                   CROMERR requires that state, tribal or
                                              Halogenated Volatiles by Gas                            rulemaking procedures. During a future                local government agencies that receive,
                                              Chromatography Using Photoionization                    rulemaking effort, the Agency will                    or wish to begin receiving, electronic
                                              and/or Electrolytic Conductivity                        consider those comments on MDPs that                  reports under their EPA-authorized
                                              Detectors), 8111 (Haloethers by Gas                     may require rulemaking.                               programs must apply to EPA for a
                                              Chromatography), and 8430 (Analysis of                  V. Summary                                            revision or modification of those
                                              Bis(2-chloroethyl) Ether and Hydrolysis                                                                       programs and obtain EPA approval.
                                                                                                        These changes in Update V will assist               Subpart D provides standards for such
                                              Products by Direct Aqueous Injection                    method users in demonstrating method
                                              GC/FT–IR)—The Agency received the                                                                             approvals based on consideration of the
                                                                                                      competency and in generating better                   electronic document receiving systems
                                              same two comments for these three                       quality data. For the convenience of the
                                              methods. Both comments concurred                                                                              that the state, tribe, or local government
                                                                                                      analytical community, the Agency will                 will use to implement the electronic
                                              with the nomenclature change for bis(2-                 revise the OSWER Methods’ Team
                                              chloro-1-methylethyl)ether, which                                                                             reporting. Additionally, § 3.1000(b)
                                                                                                      homepage on The Agency’s Web site to                  through (e) of 40 CFR part 3, subpart D
                                              alleviated confusion.                                   include the final Update V. Also, please              provides special procedures for program
                                                 Method 8270D (Semivolatile Organic                   see the Web site: http://www.epa.gov/                 revisions and modifications to allow
                                              Compounds by Gas Chromatography/                        epawaste/hazard/testmethods/                          electronic reporting, to be used at the
                                              Mass Spectrometry (GC/MS))—The                          index.htm for more information. Table 1               option of the state, tribe or local
                                              Agency received two comments which                      provides a listing of the five chapters               government in place of procedures
                                              concurred with the nomenclature                         and 23 methods (8 new methods and 15                  available under existing program-
                                              change for bis(2-chloro-1-                              revised methods) in Update V.                         specific authorization regulations. An
                                              methylethyl)ether. Method 8270D also                      Dated: July 22, 2015.                               application submitted under the subpart
                                              received one comment asking about the                                                                         D procedures must show that the state,
                                                                                                      Barnes Johnson,
                                              possibility of reporting flagged data                                                                         tribe or local government has sufficient
                                              from calibrations where some                            Director, Office of Resource Conservation and
                                                                                                      Recovery.                                             legal authority to implement the
                                              compounds were outside the specified                                                                          electronic reporting components of the
                                                                                                      [FR Doc. 2015–20030 Filed 8–12–15; 8:45 am]
                                              criteria. The Agency’s RCRA Organic                                                                           programs covered by the application
                                              Workgroup is discussing this issue and                  BILLING CODE 6560–50–P
                                                                                                                                                            and will use electronic document
                                              intends to address it in Update VI.                                                                           receiving systems that meet the
                                                 Method 8410D Gas Chromatography/                     ENVIRONMENTAL PROTECTION                              applicable subpart D requirements.
                                              Fourier Transform Infrared (GC/FT–IR)                   AGENCY                                                Once an authorized program has EPA’s
                                              Spectrometry for Semivolatile Organics:                                                                       approval to accept electronic documents
                                              Capillary Column—The Agency                             [FRL–9927–87–OEI]                                     under certain programs, CROMERR
                                              received two comments on Method                                                                               § 3.1000(a)(4) requires that the program
                                                                                                      Cross-Media Electronic Reporting:
                                              8410D which concurred with the                                                                                keep EPA apprised of any changes to
                                                                                                      Authorized Program Revision
                                              nomenclature change for bis(2-chloro-1-                                                                       laws, policies, or the electronic
                                                                                                      Approval, State of Washington
                                              methylethyl)ether. Method 8410D also                                                                          document receiving systems that have
                                              received one comment discussing the                     AGENCY: Environmental Protection                      the potential to affect the program’s
                                              acceptable temperature range of samples                 Agency (EPA).                                         compliance with CROMERR § 3.2000.
                                              for preservation. The Agency accepted                   ACTION: Notice.                                          On May 21, 2009, the Washington
                                              the updated change.                                                                                           State Department of Ecology (ECY WA)
                                                                                                      SUMMARY: This notice announces EPA’s
                                                 Method 9014 (Titrimetric and Manual                                                                        submitted an amended application
                                                                                                      approval of the State of Washington’s                 titled ‘‘Turbowaste.net’’ or revisions/
                                              Spectrophotometric Determinative
                                                                                                      request to revise/modify its Approved                 modifications to its EPA-approved
                                              Methods for Cyanide)—Detailed
                                                                                                      State Hazardous Waste Management                      program under title 40 CFR to allow
                                              information on calibration models and
                                                                                                      EPA-authorized program to allow                       new electronic reporting Part 262, 264–
                                              their acceptance criteria are not
                                                                                                      electronic reporting.                                 265, and 270 program under title 40
                                              included in each SW–846 method. This
                                                                                                      DATES: EPA’s approval is effective                    CFR to allow new electronic reporting.
                                              is because these methods are intended
                                              as general guidance, as are all of the                  August 13, 2015.                                      EPA reviewed ECY WA’s request to
                                              methods discussed in this notice. For                   FOR FURTHER INFORMATION CONTACT:                      revise/modify its EPA-authorized Part
                                              any test method which is not a method-                  Karen Seeh, U.S. Environmental                        272—Approved State Hazardous Waste
                                              defined parameter (MDP), the intention                  Protection Agency, Office of                          Management Programs and, based on
                                              is to allow the laboratory flexibility                  Environmental Information, Mail Stop                  this review, EPA determined that the
                                              under the Methods Innovation Rule                       2823T, 1200 Pennsylvania Avenue NW.,                  application met the standards for
tkelley on DSK3SPTVN1PROD with NOTICES




                                              (MIR).3 The details of how a laboratory                 Washington, DC 20460, (202) 566–1175,                 approval of authorized program
                                              will conduct and approve calibrations                   seeh.karen@epa.gov.                                   revision/modification set out in 40 CFR
                                              should be included in the individual                    SUPPLEMENTARY INFORMATION: On                         part 3, subpart D. In accordance with 40
                                              laboratory’s Quality Management Plan                    October 13, 2005, the final Cross-Media               CFR 3.1000(d), this notice of EPA’s
                                                                                                      Electronic Reporting Rule (CROMERR)                   decision to approve Washington’s
                                                3 See 70 FR 34537, June 14, 2005 Federal              was published in the Federal Register                 request to revise/modify its Part 272—
                                              Register.                                               (70 FR 59848) and codified as part 3 of               Approved State Hazardous Waste


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Document Created: 2018-02-23 10:57:04
Document Modified: 2018-02-23 10:57:04
CategoryRegulatory Information
CollectionFederal Register
sudoc ClassAE 2.7:
GS 4.107:
AE 2.106:
PublisherOffice of the Federal Register, National Archives and Records Administration
SectionNotices
ActionNotice.
ContactKim Kirkland, Office of Resource Conservation and Recovery (5304P), Environmental Protection Agency, 1200 Pennsylvania Avenue NW., Washington, DC 20460-0002; telephone
FR Citation80 FR 48522 

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