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

Persons unable to file electronically 

should submit an original and 5 copies 

of the intervention or protest to the 

Federal Energy Regulatory Commission, 

888 First Street NE., Washington, DC 

20426. 

The filings in the above-referenced 

proceeding are accessible in the 

Commission’s eLibrary system by 

clicking on the appropriate link in the 

above list. They are also available for 

electronic review in the Commission’s 

Public Reference Room in Washington, 

DC. There is an eSubscription link on 

the Web site that enables subscribers to 

receive email notification when a 

document is added to a subscribed 

docket(s). For assistance with any FERC 

Online service, please email 

FERCOnlineSupport@ferc.gov. or call 

(866) 208–3676 (toll free). For TTY, call 

(202) 502–8659. 

Dated: August 6, 2015. 

Nathaniel J. Davis, Sr., 

Deputy Secretary. 

[FR Doc. 2015–19887 Filed 8–12–15; 8:45 am] 

BILLING CODE 6717–01–P 

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. 

SUMMARY: The Environmental Protection 

Agency (EPA or Agency) is providing 

notice of the availability of ‘‘Final 

Update V’’ to the Third Edition of the 

manual, ‘‘Test Methods for Evaluating 

Solid Waste, Physical/Chemical 

Methods,’’ EPA publication SW–846. 

Final Update V contains analytical 

methods, of which 8 are new and 15 are 

revised. The methods in Update V may 

be used in monitoring or complying 

with the Resource Conservation and 

Recovery Act (RCRA) hazardous waste 

regulations. This action includes 

revisions to the methods in response to 

comments received on a Notice 

published in the Federal Register on 

October 23, 2013 and finalizes the 

methods and guidance. In addition, the 

Agency is also finalizing revisions to 

Chapters One through Five of SW–846 

and an Office of Resource Conservation 

and Recovery (ORCR) policy statement 

in the SW–846 methods compendium. 

The Agency is issuing this Update as 

guidance since the changes in this 

document to the SW–846 analytical 

methods are not required by RCRA’s 

hazardous waste regulations. Any 

required analytical methods have not 

been changed. 

FOR FURTHER INFORMATION CONTACT: Kim 

Kirkland, Office of Resource 

Conservation and Recovery (5304P), 

Environmental Protection Agency, 1200 

Pennsylvania Avenue NW., Washington, 

DC 20460–0002; telephone number: 

(703) 308–8855, fax number: (703) 308– 

0509, email address: kirkland.kim@

epa.gov. 

SUPPLEMENTARY INFORMATION: 

I. General Information 

A. Does this action apply to me? 

This notice is directed to the public 

in general. It may, however, be of 

particular interest to those conducting 

waste sampling and analysis for RCRArelated 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, 


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1Specifically, this summary of significant 

changes (Appendix A) is included in each newlyrevised 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. 2The 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. 

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. 

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® Bioassay. 


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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 

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 


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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 projectrequired 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 


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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 projectspecific 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 r2 (Regression 

Coefficient) but with % Error. Standard 

deviation (SD) and r2 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 r2, 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/ 

r2 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. 

Where: 

xi = True amount of analyte in calibration 

level i, in mass or concentration units. 

x ́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. 


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

<LLOQ. In addition, typographical 

errors were corrected. 

Method 8000D (Determinative 

Chromatographic Separations)—The 

Agency received comments on Method 

8000 during the public comment period 

and an additional four afterward. The 

comments received are summarized 

below in several categories. 

Eight comments were related to the 

use and implementation of the LLOQ 

and its application to method blanks. 

Several additions and changes were 

made in the method as a result of these 

comments. The method blank language 

in Sections 9.2.6.9 through 9.2.6.11 was 

updated to reflect that blanks should be 

considered acceptable if the 

concentrations found were below one 

half of the LLOQ (or project DQOs). 

Blanks may contain hits for reported 

compounds if the results in the 

associated samples are >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. 


tkelley on DSK3SPTVN1PROD with NOTICES
48528 Federal Register / Vol. 80, No. 156 / Thursday, August 13, 2015 / Notices 

3See 70 FR 34537, June 14, 2005 Federal 

Register. 

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 methoddefined 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. 

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 

ENVIRONMENTAL PROTECTION 

AGENCY 

[FRL–9927–87–OEI] 

Cross-Media Electronic Reporting: 

Authorized Program Revision 

Approval, State of Washington 

AGENCY: Environmental Protection 

Agency (EPA). 

ACTION: Notice. 

SUMMARY: This notice announces EPA’s 

approval of the State of Washington’s 

request to revise/modify its Approved 

State Hazardous Waste Management 

EPA-authorized program to allow 

electronic reporting. 

DATES: EPA’s approval is effective 

August 13, 2015. 

FOR FURTHER INFORMATION CONTACT: 

Karen Seeh, U.S. Environmental 

Protection Agency, Office of 

Environmental Information, Mail Stop 

2823T, 1200 Pennsylvania Avenue NW., 

Washington, DC 20460, (202) 566–1175, 

seeh.karen@epa.gov. 

SUPPLEMENTARY INFORMATION: On 

October 13, 2005, the final Cross-Media 

Electronic Reporting Rule (CROMERR) 

was published in the Federal Register 

(70 FR 59848) and codified as part 3 of 

title 40 of the CFR. CROMERR 

establishes electronic reporting as an 

acceptable regulatory alternative to 

paper reporting and establishes 

requirements to assure that electronic 

documents are as legally dependable as 

their paper counterparts. Subpart D of 

CROMERR requires that state, tribal or 

local government agencies that receive, 

or wish to begin receiving, electronic 

reports under their EPA-authorized 

programs must apply to EPA for a 

revision or modification of those 

programs and obtain EPA approval. 

Subpart D provides standards for such 

approvals based on consideration of the 

electronic document receiving systems 

that the state, tribe, or local government 

will use to implement the electronic 

reporting. Additionally, § 3.1000(b) 

through (e) of 40 CFR part 3, subpart D 

provides special procedures for program 

revisions and modifications to allow 

electronic reporting, to be used at the 

option of the state, tribe or local 

government in place of procedures 

available under existing programspecific authorization regulations. An 

application submitted under the subpart 

D procedures must show that the state, 

tribe or local government has sufficient 

legal authority to implement the 

electronic reporting components of the 

programs covered by the application 

and will use electronic document 

receiving systems that meet the 

applicable subpart D requirements. 

Once an authorized program has EPA’s 

approval to accept electronic documents 

under certain programs, CROMERR 

§ 3.1000(a)(4) requires that the program 

keep EPA apprised of any changes to 

laws, policies, or the electronic 

document receiving systems that have 

the potential to affect the program’s 

compliance with CROMERR § 3.2000. 

On May 21, 2009, the Washington 

State Department of Ecology (ECY WA) 

submitted an amended application 

titled ‘‘Turbowaste.net’’ or revisions/

modifications to its EPA-approved 

program under title 40 CFR to allow 

new electronic reporting Part 262, 264– 

265, and 270 program under title 40 

CFR to allow new electronic reporting. 

EPA reviewed ECY WA’s request to 

revise/modify its EPA-authorized Part 

272—Approved State Hazardous Waste 

Management Programs and, based on 

this review, EPA determined that the 

application met the standards for 

approval of authorized program 

revision/modification set out in 40 CFR 

part 3, subpart D. In accordance with 40 

CFR 3.1000(d), this notice of EPA’s 

decision to approve Washington’s 

request to revise/modify its Part 272— 

Approved State Hazardous Waste 


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