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PUBLIC COMMENT SUMMARIES AND RESPONSES 

UPDATE V TO SW-846 

"TEST METHODS FOR EVALUATING SOLID WASTE, 

PHYSICAL/CHEMICAL METHODS" 

July 2014 

Prepared by: 

TechLaw, Inc. 

14500 Avion Parkway 

Suite 300 

Chantilly, VA 20151 

Prepared For: 

U.S. Environmental Protection Agency 

Methods Team, Office of Resource Conservation and Recovery (ORCR) 

EPA Contract No.: GS-10F-0168J 

EPA Work Assignment Mangers: 

K. Kirkland and S. Yang 

EPA Project Officer: 

S. Fowler 

 
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TABLE OF CONTENTS 

INTRODUCTION ....................................................................................................................... 3 

CHAPTER ONE ......................................................................................................................... 4 

CHAPTER TWO .......................................................................................................................12 

CHAPTER THREE ....................................................................................................................16 

CHAPTER FOUR ......................................................................................................................18 

CHAPTER NINE .......................................................................................................................21 

METHOD 3200 .........................................................................................................................22 

METHOD 6010D .......................................................................................................................23 

METHOD 6020B .......................................................................................................................27 

METHOD 8000D .......................................................................................................................31 

METHOD 8021B .......................................................................................................................38 

METHOD 8111 .........................................................................................................................39 

METHOD 8270D .......................................................................................................................40 

METHOD 8290 .........................................................................................................................41 

METHOD 8410 .........................................................................................................................42 

METHOD 8430 .........................................................................................................................43 

METHOD 9014 .........................................................................................................................44 

METHOD 9040 .........................................................................................................................45 

REFERENCE TABLE ................................................................................................................46 

GENERAL COMMENTS ...........................................................................................................47 

 
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INTRODUCTION 

On October 23, 2013, the U.S. EPA published a notice to announce the availability of, 

and to request comment on, "Update V" (Docket EPA–HQ–RCRA–2012–0072; FRL–9901–86–

OSWER) to the Third Edition of EPA publication SW-846, "Test Methods for Evaluating Solid 

Waste, Physical/Chemical Methods". EPA welcomed the public to submit comments on 23 new 

and revised analytical methods. In addition, the Agency also invited comments on revisions to 

Chapters One through Five of EPA publication SW-846, an ORCR Policy Statement, and other 

guidance. The Agency has received public comment on Update V, and after consideration, is 

placing these new and revised methods, guidance, and chapters in the SW-846 methods 

compendium. EPA is issuing this update as guidance. 

This document provides draft summaries and responses to the public comments 

submitted to date regarding those parts of the Update V chapters and methods which were 

open to comment. Complete copies of the comments can be found in the docket to the notices 

for Update V. 

 
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CHAPTER ONE 

1. Comment: 

a) Commenter #4 commented, regarding Chapter One, that the guide does not define the 

difference between a limit of quantitation (LOQ) and lower level of quantitation (LLOQ). 

b) Commenter #4 made a second comment on LOQ, regarding Chapter One, Glossary Page 

ONE-21, that the LOQ should be defined as a level with defined precision and bias. However, 

the glossary text for precision states that precision is only to be calculated at concentrations 

above the LLOQ. Therefore, this further implies that the LLOQ exists at a level without known 

precision. If the LLOQ is assumed to be at the lowest calibration standard, then the guidance is 

also implying that precision cannot be calculated at the lowest calibration standard. 

Recommended edit: Change definition of precision to "concentration equal to or above the 

LLOQ". 

Response: 

The Agency agrees with the commenter (comment 1a) and has updated Chapter One to 

remove the reference to limit of quantitation (LOQ). Section 1.1.4.9 of Chapter One now reads: 

"Sensitivity is an instrument's or method's minimum concentration that can be reliably measured 

or reported (i.e., lower limit of quantitation [LLOQ])." The glossary text for precision is changed 

to reflect that precision can be calculated at or above the LLOQ. Section 1.1.4.9 was 

renumbered due to the addition of repeatability as Section 1.1.4.8. 

2. Comment: 

Commenter #4 commented, regarding Sec. 1.1.4 of Chapter One, that "Sensitivity" in terms of 

Detection Limits and Quantitation Limits is not included as data quality indicator (DQI), although 

it is discussed later. Although "sensitivity" is closely tied to precision and bias (i.e., without high 

precision and low bias, there is no good "sensitivity"), data quality requirements on "sensitivity" 

should still be included for reliably reporting analyte presence/absence at the detection limits 

and analyte quantitation at the quantitation limits. For environmental analyses, one needs to 

know the detection limit to reliably report "detections", the limit of detection to reliably report 

"non-detects", and the limit of quantitation for reliably reporting "quantitative results" 

(http://www.denix.osd.mil/edqw/upload/Final-DQ-Fact-Sheet-091409.pdf). Recommended edit: 

Suggest that sensitivity in term of IUPAC/ACS Critical Level, Detection Limit, and Quantitation 

Limit (or the DoD's equivalent Detection Limit, Limit of Detection, and Limit of Quantitation 

(http://www.denix.osd.mil/edqw/upload/Final-DQ-Fact-Sheet-091409.pdf) be used. 

Response: 

The Agency thanks the commenter for their input, but disagrees with the commenter that the 

current definition of sensitivity is not adequate. A more detailed definition of sensitivity is not 

needed in Chapter One since it is intended as general guidance. For a more detailed 

discussion of the terminology (i.e., sensitivity), readers are encouraged to reference the 

guidance documents listed in Section 1.4 of Chapter One. 

3. Comment: 

Commenter #4 commented, regarding the first sentence of Section 1.1.4 of Chapter One, that 

procedures on establishing project-specific DQIs be provided or referenced. Recommended 

edit: Add a concise paragraph or a reference for a procedure about establishing project-specific 

DQIs (e.g., how to establish the acceptance criteria for project-specific relative percent 

differences (RPDs) of laboratory duplicate analyses).
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Response: 

The Agency thanks the commenter for their input. Chapter One is intended as general 

guidance and does not contain detailed instructions about how each project-specific DQI is 

established. The project team should reference the documents listed in Sec. 1.1.2.7 and follow 

the data quality objective (DQO) process to develop their project-specific data collection plan; 

establish DQIs using proven, defensible statistical methods; and document how these DQI limits 

are established in the appropriate location (e.g., laboratory Quality Management Plans (QMP), 

method standard operating procedures (SOPs), etc.).

4. Comment: 

Commenter #4 commented, regarding Section 1.1.4.4 of Chapter One, that only data of known 

quality (i.e., precision and bias) can be reliably compared. Recommended edit: Add a sentence 

to the end of the Section - "Measurement data shall be of known and documented data quality 

(e.g., precision and bias) to ensure comparability."

Response: 

The Agency agrees with the commenter and has added the following sentence to the end of 

Section 1.1.4.4: "Further, when assessing comparability, data sets should be of known and 

documented quality." 

5. Comment: 

Commenter #4 commented, regarding Sec. 1.1.4.7 of Chapter One, that if "reproducibility" is 

addressed, that "repeatability" be also addressed. "Reproducibility" addresses inter-laboratory 

variances and "repeatability" addresses intra-laboratory variances. The two are paired and 

should be addressed together. Recommended edit: Please reference national and international 

standard organizations such as NIST, ISO, etc. to define and address both "repeatability" and 

"reproducibility" for completeness.

Response: 

The Agency agrees with the commenter and has added a discussion of repeatability to the DQIs 

in Section 1.1.4 of Chapter One. 

6. Comment: 

Commenter #4 commented, regarding Section 1.1.4.8 of Chapter One, that "sensitivity" is the 

slope of a calibration curve (i.e., instrument responses to concentration changes) and "detection 

limit" is the intercept of a calibration curve, but they often are mistakenly used interchangeably. 

For all environmental analyses, one needs "critical levels" to report detections with 99% 

confidence, "detection limits" to report non-detects with 99% confidence, and "quantitation 

limits" to report quantitative results with known precision and bias. Without critical levels, one 

cannot reliably report "presence" at or above the "critical levels". Without "detection limits", one 

cannot reliably report "absence" at or below the "detection limit". Therefore, one must consider 

the sensitivity or detection limits of any chemical analyses before the sample analysis. 

Recommended edit: Better definition of detection and quantitation limits needed.

Response: 

The Agency thanks the commenter for their input. A more detailed definition of sensitivity is not 

needed in Chapter One since it is intended as general guidance. For a more detailed 

discussion of these terms, readers are encouraged to reference the guidance documents listed 

in Sec. 1.4 of Chapter One. 
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7. Comment: 

Commenter #4 commented, regarding Sections 1.1.1, 1.1.2, 1.1.3, 1.1.4, and 1.3.1 of Chapter 

One, that the systematic planning process (1.1.1), DQOs (1.1.2), QAPP (1.1.3), DQIs (1.1.4), 

and data verification and validation (1.3.1) do not provide any information on how LLOQ 

information should be considered. The documents referenced for these areas speak to method 

detection limits (MDLs) and reporting limits (RLs). Recommended edit: Discuss how LLOQ 

information should be considered. 

Response: 

The Agency thanks the commenter for their input, but disagrees with the commenter. Chapter 

One is intended as general guidance. It is recommended to establish 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. This makes the consideration of the LLOQ level functionally equivalent to the RL for 

the individual method. Results at or above the LLOQ are quantifiable within an acceptable 

precision and bias. Thus, the LLOQ approach suits the needs of the Resources Conservation 

and Recovery Act (RCRA) program, because it provides reliable and defensible results, 

especially at the LLOQ, and can be reported with a known level of confidence for the complex 

matrices being evaluated. The LLOQ should be established at a level equal to or below the 

regulatory limit or threshold, depending on the project needs/data use. 

8. Comment: 

Commenter #4 commented, regarding Sections 1.1.4, 1.1.4.2, and 1.1.4.6 of Chapter One, that 

"accuracy" is a combination of "precision" and "bias". Where "accuracy" is used in SW-846, it 

should often be changed to "bias". Or, the term of "trueness", which is adopted as a parallel 

term to "precision" by ISO, may be used. Also, please notice that the DQIs defined in Section 

1.1.4 are not consistent with the DQIs defined in the Glossary on Page ONE-17. Updated 

guidance from EPA Quality has already changed "accuracy" to "bias". Recommended edit: 

Suggest that "accuracy" in Section 1.1.4 be changed to "accuracy (bias)" and explain that the 

"accuracy" originally used as PARCC was a mistake of "bias". Also, replace Section 1.1.4.2 

with Section 1.1.4.6 and change the title to "Accuracy (Bias)". In addition, most "accuracy" used 

in SW-846 Update V chapters and methods should be replaced with "bias". 

Response: 

For consistency with the text of 1.1.4, reproducibility has been added to the DQI glossary 

definition. The definition was listed as: "Reproducibility is defined as the closeness of the 

agreement between the results of measurements of the same analyte carried out under variable 

conditions of measurement." 

On the other items raised in the comment, the Agency thanks the commenter for their input, but 

disagrees with the commenter that the current definitions are not adequate. More detailed 

definitions and discussion of these terms are not in Chapter One since it is intended as general 

guidance. For more detailed discussion of terms, readers are encouraged to reference the 

guidance documents listed in Section 1.4 of Chapter One. 

9. Comment: 

Commenter #4 commented, regarding Chapter One, Glossary, Page ONE-20, that the glossary 

stipulates that: "Individual methods may recommend procedures for verifying the LLOQ and 

acceptance limits for use until the laboratory has sufficient data to determine acceptance limits 

statistically". However, there is no guidance on how to perform the statistical determination of 
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the LLOQ. Recommended edit: Add guidance on how to perform the statistical determination of 

the LLOQ.

Response: 

The Agency thanks the commenter for their input, but disagrees with the commenter that the 

current definition of LLOQ is not adequate. The Glossary (in Chapter One) is not intended to 

provide a procedure for statistically determining the LLOQ. The statement quoted in Comment 

9 is changed to read: "Individual methods may recommend procedures for verifying the LLOQ 

and acceptance limits for use until the laboratory has sufficient data to determine acceptance 

limits". 

10. Comment: 

Commenter #4 commented, regarding Chapter One, Glossary Page ONE-17, that under 

BLANK, "Reagent blank" is improperly defined as the same as "method blank". "Reagent 

blank", which is mentioned in the instrument detection limit (IDL) addressed on Page ONE-19, is 

assumed to be equivalent to a "method blank" that goes through the sample preparation 

process. This imposes a problem to the determination of IDL, which is based on the results of 

multiple "reagent blanks". "Reagent blank" should be individual or a combination of individual 

reagents that do not go through sample preparation procedures like the "method blank", and 

hence used for IDL determination. (A method blank that goes through all sample preparation 

procedures is used for MDL determination.) A reagent blank is used to ensure contaminant-free 

individual reagents are used. Only clean reagents shall be used to prepare "instrument blank" 

to test instrument cleanliness and "method blank" to test the analytical systems. Recommended 

edit: Add "reagent blank" to the "BLANK" and revise "reagent blank" definition to distinguish it 

from "method blank" in the Glossary.

Response: 

The Agency agrees with the commenter and has added a separate definition for reagent blank 

in addition to method blank. The following definition was added to Chapter One Glossary: 

REAGENT BLANK: Reagent blanks are analyzed to assess background interference or 

contamination that exists in the analytical system that might lead to 

the reporting of elevated concentration levels or false positive data. 

The reagent blank is defined as an interference-free blank matrix, to 

which all reagents are added in the same volumes or proportions as 

used in sample preparation but are NOT carried through the complete 

sample preparation, cleanup, and determinative procedures. The 

purpose of a reagent blank is to gauge contamination from chemical 

inputs and instrumental factors only. A reagent blank is NOT run as 

part of a digestion or preparation method. 

11. Comment: 

Commenter #4 commented, regarding Chapter One, Glossary Page ONE-18, that under FIELD 

BLANK, there are two editorial errors in the second paragraph of FIELD BLANK. The second 

paragraph needs revisions for clarification too. Recommended edit: Change the second 

paragraph to, "A field blank may also be defined as a container of reagent water or a solid blank 

material that is opened in the field for a predefined period of time and then sent to the laboratory 

for analysis. This type of field blank is typically used to measure ambient contamination of 

volatile organic samples in the field."

 
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Response: 

The Agency agrees with the commenter. The text was revised as follows: "Field blanks may 

also be obtained by the sampling organization to measure ambient contamination in the field. If 

this type of field blank is requested, a container of reagent water or a solid blank material is 

opened in the field for a predefined period of time. The sample is then sent to the laboratory for 

analysis." 

12. Comment: 

Commenter #4 commented, regarding Chapter One, Glossary Page ONE-19 and Chapter 3, 

DEFINITIONS, Page THREE-2, that under IDL, the "reagent blank" used for IDL determination 

shall not be equivalent to the "method blank" that goes through all sample preparation 

procedures. Recommended edit: Change the definition of "reagent blank" to a mixture of all 

analytical regents of the same proportions used for sample preparation but the “reagent blank” 

does not go through the sample preparation process. It may be used for determining IDLs 

and/or to test the cleanliness of reagents.

Response: 

The Agency agrees with the commenter. Please see response to Comment #10 above for 

further details. 

13. Comment: 

Commenter #4 commented, regarding Chapter One, Glossary Page ONE-20, that under 

LABORATORY DUPLICATE that the SW-846 distinguish and clarify "analytical" and 

"measurement" in the second sentence. "Measurement" should be defined as a combination of 

"field sampling" and "laboratory analysis" and "analytical (analysis)" be defined a combination of 

"sample preparation" and "instrument determination". (See Section 2.2.4 of SW-846 Chapter 

Two) Recommended edit: Delete the "or measurement" from the second sentence.

Response: 

The Agency thanks the commenter for their input, but disagrees that a change is needed in this 

section. 

14. Comment: 

Commenter #4 commented, regarding Chapter One, Glossary Page ONE-20, that under LLOQ, 

the introduction of LLOQ is not clear. A LOQ is well and commonly defined as "the minimum 

levels, concentrations, or quantities of a target variable (e.g., target analyte) that can be 

reported with a specified degree of confidence". An LLOQ could be established at the lowest 

calibration standard if the precision and bias at the lowest calibration standard are established 

and documented. Recommended edit: Suggest that LLOQ be changed to LOQ to comply with 

well accepted national and international definition for LOQ, and provide procedures or guidance 

for establishing laboratory-specific LOQ.

Response: 

The Agency thanks for commenter for their input. The reference to LOQ has been removed 

from Chapter One. 

 
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15. Comment: 

Commenter #4 commented, regarding Chapter One, Glossary Page ONE-21, that under 

METHOD BLANK, the acceptance criteria for method blank should be "less than or equal to 

50% of the LLOQ (except for common laboratory blank contaminants which shall be less than or 

equal to the LLOQ), 10% of the amount measured in any associated batch samples, or 10% of 

the regulatory limit, whichever is greater. If data uncertainty of method blank results, decision 

errors, and practical issues are considered, method blanks should be less than or equal to 50% 

of the LLOQ (or LOQ for common laboratory contaminants) and 10% of sample concentrations 

or regulatory limits, whichever is greater." Recommended edit: Change the second to the last 

sentence to "The method blank results should not be greater than 50% of the LLOQ (or the 

LLOQ for common laboratory contaminants), 10% of the amount measured in any associated 

batch samples, or 10% of the regulatory limit, whichever is greater." 

Response: 

The Agency thanks the commenter for their input. Chapter One is intended as general 

guidance; as such it does not discuss method blank acceptance criteria for individual 

procedures. The reader should look to the individual determinative methods for that 

information. 

16. Comment: 

Commenter #4 commented, regarding Chapter One, Glossary Page ONE-21, that under 

PRECISION, the numerator for the RPD should include an absolute sign (i.e., RPD = (100) |(X1 

- X2)| / [(X1 + X2) / 2]). Duplicate/replicate should be independently prepared and analyzed, 

and the text needs to clarify the "independently" prepared and analyzed. Duplicate or replicate 

samples should be "independently" prepared and analyzed, but in practice it is typically not 

"independently" prepared and analyzed. Recommended edit: Change the RPD equation to 

RPD = (100) |(X1 - X2)| / [(X1 + X2) / 2]. Change the last sentence to "independently prepared 

and analyzed" and clarify "independently". 

Response: 

The Agency agrees with the commenter and has modified the language and the equation for 

RPD in Chapter One to: "The agreement among a set of replicate measurements without 

assumption of knowledge of the true value. Precision is estimated by means of 

duplicate/replicate analyses of separate aliquots of the same sample (not multiple runs of a 

single digestion/extraction). These samples should contain concentrations of analyte at or 

above the LLOQ, and may involve the use of matrix spikes. The most commonly used 

estimates of precision are:" 

 =

| − 	

|




 + 	

2




∗ 	100

17. Comment: 

Commenter #4 commented, regarding Chapter One, Glossary Page ONE-22, that under 

QUALITY CONTROL SAMPLE, "Analytical batch" is not clearly defined. An analytical batch is 

composed of a "sample preparation batch" and an "instrument determination batch". Based on 

the example QC samples addressed in the paragraph, the batch should be a "sample 

preparation batch". The QC samples for an "instrument determination batch" include calibration 

blanks, calibration verifications, post digestion spike, etc. Recommended edit: Change the "an 

analytical batch" to "a sample preparation batch". 
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Response: 

The Agency agrees with the commenter and has modified the glossary for "QUALITY 

CONTROL SAMPLE" in Chapter One to read: "A sample made from standards or matrix and 

used to verify acceptability of the results from preparation and/or analysis of a batch of samples. 

Examples of laboratory quality control samples are method blanks, laboratory duplicates, and 

laboratory control samples; field quality control samples are field blanks, trip blanks, field 

duplicates, and matrix spikes." 

18. Comment: 

Commenter #4 recommended, regarding Chapter One, Glossary Page ONE-23, that under 

REPRESENTATIVENESS, delete "and precisely" from the first sentence. Accuracy is a 

combination of high precision and low bias. Hence, "accurately" covers "precisely". 

Recommended edit: Delete "and precisely" from the first sentence. 

Response: 

The Agency agrees with the commenter and has made the requested edit in the text. 

19. Comment: 

Commenter #4 recommended, regarding Chapter One, Glossary Page ONE-23, that the third 

and fourth sentences be revised for consistency. Recommended edit: Change the third and 

fourth sentences to "Surrogate spikes are added to field samples and QC samples for organic 

analyses at known amounts and their recoveries are used to assess matrix effects and, to some 

extent, verify proper processing and instrument performance for each sample. The analytes 

used as surrogates mimic the behavior of the target analyte(s) throughout sample preparation 

and instrument determination." 

Response: 

The Agency agrees with the commenter and has made the suggested edits to Chapter One. 

20. Comment: 

Commenter #9 commented, regarding Chapter One and Chapter Nine, that additional guidance 

has been provided in the proposed revision of Chapter One (including references) regarding the 

calculation of the upper confidence limit (UCL) for making the determination as to whether a 

waste may be hazardous. Specifically, in Section 1.1.3.2 of Chapter One, several documents 

are listed for the development of Sampling and Analysis Plans. At least two of these documents 

contradict one another in their use of the UCL for making the determination that the analytical 

results for a given waste could exceed the RCRA limit. 

• In SW-846, Chapter 9, page 16, starting in Section 7 and Equation 6 (which is repeated 

multiple times in Chapter 9), the two-tailed critical value for the Student's t distribution is used. 

• In Chapter One, Reference 8, "RCRA Waste Sampling Draft Technical Guidance" (EPA 503-

D-02-002), in Section 3.4.3.1, Appendices F (Equation F.6) and G (Table G-1) the single-tailed 

critical value for the Student's t distribution is used. 

The commenter believes that use of the single-tailed critical value is statistically correct and 

asks that either Chapter Nine be revised to utilize the single-tailed critical value for the UCL or 

the conflicting references in Chapter One be removed. 

 
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Response: 

Chapter One does not directly discuss the Student t test referred to by the commenter. The 

Commenter is comparing a discussion of the two-tailed Student’s t found in Chapter 9 with a 

different version of Student’s t test found in one of the references provided in Chapter One. 

Chapter One expresses no preference between the two differing methods of statistical analysis, 

but merely lists additional references that can be used to find more detailed discussions on 

various topics. Chapter One is intended to be general guidance and cannot discuss in detail 

every specific scenario and/or conflict (if they exist) between reference documents. 

In addition, Chapter Nine is not included in Update V and as such, is not subject to revision at 

this time. The Agency thanks the commenter for their input and the comment will be discussed 

the next time Chapter Nine is updated. 

 
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CHAPTER TWO 

1. Comment: 

Commenter #1 commented, regarding Chapter Two, that another document in the Docket, 

specifically EPA-HQ-RCRA-2012-0072-0019, needs revisions to its Figure 2-2 (entitled 

"Schematic of Sequence to Determine if a Waste is Hazardous by Characteristic") as follows: 

A. The figure's references to "49 CFR 173.300" and "49 CFR 173.151" make it clear that the 

schematic does not reflect the extensive changes made by EPA to 261.21 in the July 14, 2006 

Federal Register. 

B. The diamond reading "Is waste a gas" should be changed to "Is waste a containerized gas" 

to reflect EPA's position as stated in RO# 14823 that non-containerized gases are not solid 

waste. 

C. The box "Perform Paint Filter Test (method 9095)" should have the left arrow leaving that box 

changed from "Liquid" to "Liquid Result" and the right arrow changed from "Solid" to "Solid 

Result." This will prevent a reader from erroneously concluding that no solids can be present for 

the "liquids" direction or that no liquids can be present for the "solids" direction. 

D. The diamond "Is total concentration of TC constituents ÷ 20 < TC regulatory limit?" should be 

changed to reflect the formula given in RO# 14695 and the Dec 21, 1995 FR (on page 66389), 

since the 20:1 ratio will decrease to 1:1 as the percentage of solids present decreases from 

100% to 0%. Also note that the procedure used for determining that percentage is not the 

above-mentioned 9095 paint filter test but instead the 50 psi filtering procedure found within the 

1311 TCLP test. This latter procedure will remove much more liquid from a sample than the 

9095 procedure will. 

E. The schematic does not give a proper determination for a gel that has a pH of 2 or below (or 

12.5 or above). Specifically, if a gel does not produce a liquid result with the 9095 Paint Filter 

Test, it is nonetheless a D002 if a pH reading can be obtained that is at or below 2 (or at or 

above 12.5). This is made clear in RO# 11719 (which is identified in RCRA online as "Official 

OSW Policy"). Yet the schematic never shows such a gel as needing to be checked for 

corrosivity. (Note that 261.22(a) (1) requires a waste to be aqueous, not that it be a liquid; gels 

can be aqueous while at the same time not necessarily liquids [particularly when 9095 is the 

measure of whether a waste is a liquid].)

Response: 

The Agency thanks the commenter for their input. The responses to this comment are labeled 

A through E, as the individual comments had varying resolutions: 

Comment 1A: Regarding the CFR listing in comment 1A, the Agency agrees with the 

commenter and has removed the outdated references. 

Comment 1B: The Agency agrees with the commenter and has changed the description to “is 

the waste a containerized gas?” as requested. 

Comment 1C: The Agency disagrees with the commenter and no change was made to the paint 

filter section. 

Comment 1D: The Agency agrees with the commenter and acknowledges that biphasic or 

multiphasic wastes pose an additional challenge for the user. The diagram has been updated 

and a reference to the Federal Register (Dec 21, 1995 page 66389) has been added. 

http://nepis.epa.gov/Exe/ZyNET.exe/10001E3Y.txt?ZyActionD=ZyDocument&Client=EPA&Inde

x=1995%20Thru%201999&Docs=&Query=&Time=&EndTime=&SearchMethod=1&TocRestrict=
 Page 13 

n&Toc=&TocEntry=&QField=&QFieldYear=&QFieldMonth=&QFieldDay=&UseQField=&IntQFiel

dOp=0&ExtQFieldOp=0&XmlQuery=&File=D%3A\ZYFILES\INDEX%20DATA\95THRU99\TXT\

00000000\10001E3Y.txt&User=ANONYMOUS&Password=anonymous&SortMethod=h|-

&MaximumDocuments=1&FuzzyDegree=0&ImageQuality=r75g8/r75g8/x150y150g16/i425&Dis

play=p|f&DefSeekPage=x&SearchBack=ZyActionL&Back=ZyActionS&BackDesc=Results%20p

age&MaximumPages=1&ZyEntry=48

Comment 1E: A footnote has been added showing where the reader can find RO#11719, which 

discusses gels. Gels present unique problems to characterization, as they can be aqueous, but 

still pass a paint filter test. Care should be taken when performing corrosivity measurement in a 

gel matrix as the gels can block the ceramic junctions in some types of pH probes. 

http://yosemite.epa.gov/osw/rcra.nsf/0/7D573EA3E0F1576D8525670F006BEA5F/$file/11719.p

df 

2. Comment: 

Commenter #4 commented, regarding Chapter Two, Page 84, number 8, that there is an extra 

"." Recommended edit: Correct Typo. 

Response: 

The Agency agrees with the commenter. The published PDF shows an extra period (in number 

8 of Appendix A on Page 84) that was not present in the source document. The typo was 

corrected in the final version. 

3. Comment 

Commenter #4 commented, regarding Chapter Two, Section 2.3.3, Page 10, that this Section is 

incomplete. Missing are methods 8520, 8540, and 8325. Recommended edit: Add methods 

8520, 8540, and 8325 to this Section. 

Response: 

The Agency agrees with the commenter. The methods were added to Section 2.3.3 and the 

following tables were added and/or modified as required: Method 8520 (Table 2-36A), Method 

8325 (Table 2-30) and Method 8540 (Table 2-30). 

4. Comment: 

Commenter #4 asked, regarding Chapter Two, Section 2.3.3, Page 10, 4th and 5th paragraphs, 

"Why does the discussion of Methods 8260 and 8270 clarify they employ capillary columns 

when the discussion of Methods 8081, 8082, 8141, and 8151 does not? This omission implies 

they do not use capillary columns. This same comment is true of Method 8410 (stated as 

capillary gas chromatography (GC) using Fourier Transform infrared (FT-IR)) and Method 8430 

(which is stated as GC using FT-IR but does not mention that it is also a capillary column 

method)." Recommended edit: Clarify the use of capillary columns in methods 8081, 8082, 

8141, 8151, 8410, and 8430. 

Response: 

The Agency acknowledges the commenter's observation that an unintended distinction was 

made here. The word capillary was removed as all GC and GC/mass spectrometer (MS) 

methods now employ capillary columns. The use of older technologies (such as the packed 

columns that used to be an alternative to the modern capillary) is not encouraged. The 

reference to "capillary" GC methods was removed in Section 2.3.3 of Chapter 2. 

 
 Page 14 

5. Comment: 

Commenter #4 recommended, regarding Chapter Two, Section 2.3.3, Page 10, second to last 

paragraph, that Method 8321 should not be included. All other methods in this Section are high 

performance liquid chromatography (HPLC) as stated in the first sentence, but this method is 

HPLC/MS. Recommended edit: Delete Method 8321 from this Section. 

Response: 

The Agency thanks the commenter for their input, but disagrees. Method 8321 is included in 

this section (with HPLC methods) as no separate HPLC-MS section is listed. 

6. Comment: 

Commenter #4 recommended, regarding Chapter Two, Section 2.3.3, Page 10, third paragraph, 

that the last sentence should include consulting Method 8000 prior to any HPLC-specific 

method as well. Recommended edit: Last sentence should include consulting Method 8000 

prior to any HPLC specific method as well. 

Response: 

The Agency agrees and has amended paragraph three of Section 2.3.3 of Chapter Two to state: 

"Method 8000 gives a general description of the techniques of GC and HPLC. Method 8000 

should be consulted prior to application of any of the GC or HPLC methods." 

7. Comment: 

Commenter #4 commented, regarding Chapter Two, Section 2.3.3, that the four categories 

discussed in the first paragraph do not make it clear where liquid chromatography (LC)/MS, 

LC/MS/MS, and GC/time-of-flight (TOF) analyses fall. Recommended edit: Make it clear where 

LC/MS, LC/MS/MS, and GC/TOF analyses fall. 

Response: 

The Agency thanks the commenter for their input. LC/MS and LC/MS/MS (triple quadrupole) 

are considered HPLC methods. GCs equipped with TOF mass spectrometers and triple 

quadrupole mass spectrometers are considered part of the GC/MS section. A short clarification 

was added to Section 2.3.3 in the first paragraph. 

8. Comment: 

Commenter #4 commented, regarding Chapter Two, Section 2.4.2, Page 74, Table 2-45 that 

Synthetic Precipitation Leaching Procedure (SPLP) is missing. Recommended edit: Add SPLP 

to this Section. 

Response: 

The Agency agrees with the commenter and has added SPLP to Section 2.4.2. 

9. Comment: 

Commenter #4 commented, regarding Chapter Two, Table 2-43, that the Table is missing 

Methods 8276 and 8430. Recommended edit: Add methods 8276 and 8430. 

Response: 

The Agency agrees with the commenter and has added Methods 8276 and 8430 to Table 2-43. 

 
 Page 15 

10. Comment: 

Commenter #4 commented, regarding Chapter Two, Table 2-44, that the Table is missing 

Methods 3511 and 3572. Recommended edit: Add Methods 3511 and 3572. 

Response: 

The Agency thanks the commenter for their input, but disagrees with the commenter. Table 2-

44 (PREPARATION METHODS FOR INORGANIC ANALYSES) is correct. Methods 3511 and 

3572 are both organics in nature and are included in Table 2-41. 

11. Comment: 

Commenter #4 commented, regarding Chapter Two, Tables, that Table 2-1 is missing analytes 

from Method 8276. The tables contains analytes not listed in the applicable method: Tables 2-

4, 2-6, 2-7, 2-20, 2-29; The Tables are missing analytes listed in the applicable methods: Table 

2-6, 2-20, 2-30, 2-31; The Tables list internal standards or surrogates as target analytes: Tables 

2-7; Tables do not contain analytes routinely analyzed for by users: Tables 2-10 (Aroclors 1262 

and 1268). Analytes are not in alphabetical order. Recommended edit: Reconcile methods and 

tables. 

Response: 

The Agency agrees with the commenter that Chapter 2 tables did not list all applicable 

compounds presented in the associated methods, and that the compounds were not in 

alphabetical order. Table 2-1 was revised to include Method 8276 analytes. In addition, 

Chapter 2 Tables were revised to include all compounds listed in the most recent versions of the 

referenced methods in alphabetical order. Extraneous compounds (i.e., compounds not 

included in the most recent versions of the applicable methods) were removed from Chapter 2 

tables. The Agency does not agree with the commenter on surrogates and internal standards 

being listed in the Chapter 2 tables. As noted in the referenced methods, certain compounds 

listed in the tables can be used as surrogates, but may also be analytes of interest. 

In addition, the Agency does not agree with the commenter on the issue of Chapter 2 tables not 

containing analytes routinely analyzed. The Chapter 2 tables contain all analytes discussed in 

the applicable methods. While it is understood that additional compounds may be analyzed by 

these methods, it is not EPA's intent to include all possible compounds in the tables and thus 

differ from the analytical methods. Users may analyze other compounds by these methods, if 

desired, as long as they can demonstrate adequate performance for that compound. 

12. Comment: 

Commenter #4 commented, regarding Chapter Two, Tables, that analyte tables for Methods 

8323, 8440, 8520, 8276 are missing. Recommended edit: Add tables for Methods 8323, 8440, 

8520, and 8276. 

Response: 

The Agency agrees with the commenter and has made the requested edits. The following 

tables were added to address this comment: Table 2-29A for Method 8323, Table 2-35A for 

Method 8440, Table 2-36A for Method 8520 and Table 2-23A for Method 8276. 

 
 Page 16 

CHAPTER THREE 

1. Comment: 

Commenter #4 commented, regarding Chapter Three, that for inorganics it states the mean 

recovery should be +/- 35% with a relative standard deviation (RSD) of ≤20%. Then it states 

that organics will vary more than inorganics but a limit of +/-20% is proposed until you develop 

your own limits. That is more restrictive not less. Recommended edit: Resolve the 

inconsistency between the statement that organics will show more variation than inorganics and 

the 20% limit. 

Response: 

The Agency disagrees with the commenter. The LLOQ limits for inorganics and organics are 

discussed in the Notice (on page 25), but not in Chapters 3 or 4. The inorganic requirement is 

±35% of the true value of the spike. The organic requirement is ±20% of the LCS limits a 

laboratory has in place, which should be a wider recovery limit for most compounds, but will 

vary with each individual laboratory's statistical values. 

2. Comment: 

Commenter #3 noted, regarding Chapter Three, that consistency between Chapter 3 and 

Methods 6010 and 6020 has been improved. They also applaud the approval of 

collision/reaction cell technology for interference reduction in inductively coupled plasma 

(ICP)/MS. 

Response: 

The Agency thanks the commenter for their input. 

3. Comment: 

Commenter #9 noted, regarding Chapter Three, FR Page 63191: thanks and congratulates the 

Agency on improvements in consistency between Chapter 3 and Methods 6010 and 6020 and 

on the inclusion of collision cell approval. 

Response: 

The Agency thanks the commenter for their input. 

4. Comment: 

Commenter #4 commented, regarding Chapter Three, the text for LLOQ states: "[LLOQ], which 

is ideally less than or equal to the desired regulatory action levels based on the stated project 

requirements." Recommended edit: The guidance should provide clarification on how the LLOQ 

is to be established in instances when regulatory limits are much lower than the lowest 

calibration standard. 

Response: 

The Agency appreciates the commenter's input, but does not currently publish directions for 

how the individual laboratory determines their appropriate LLOQ level for each instrument 

and/or method used. The Chapters are intended as general guidance. The details of how a 

laboratory will determine its LLOQ levels should be included in the individual laboratory's quality 

management plan (QMP) and in their SOPs for each method. If the LLOQ for a given method is 

higher than the required regulatory limit, the user should select a different determinative method 

(or a different preparation method) with an appropriate LLOQ level for that user's need. 

 
 Page 17 

5. Comment: 

Commenter #4 commented, regarding Chapter Three, Section 3.3.2, the second to the last 

sentence in this Section includes a reference to "trip blanks", which are only applicable to 

volatiles analyses, not to inorganic analyses. Recommended edit: Remove "trip blanks" from 

the sentence. 

Response: 

The Agency agrees with the commenter that trip blanks are not commonly used in inorganic 

analysis. The reference to trip blanks has been removed from Chapter 3, Section 3.3.2. 

6. Comment: 

Commenter #4 commented, regarding Chapter Three, Table 3-2, that the title of "Digestion 

Volume" does not cover samples with solid matrices. Recommended edit: Change the title of 

"Digestion Volume" to "Digestion Volume/Mass". 

Response: 

The Agency agrees with the commenter and the requested edits were made to Table 3-2 of 

Chapter 3. 

 
 Page 18 

CHAPTER FOUR 

1. Comment: 

Commenter #4 commented, regarding Chapter 4, that for inorganics it states the mean recovery 

should be +/- 35% with an RSD of ≤20%. Then it states that organics will vary more than 

inorganics but a limit of +/-20% is proposed until you develop your own limits. That is more 

restrictive not less. Recommended edit: Resolve the inconsistency between the statement that 

organics will show more variation than inorganics and the 20% limit. 

Response: 

The Agency disagrees with the commenter. The LLOQ limits for inorganics and organics are 

discussed in the Notice (on page 25) and in the methods, but not in Chapters 3 or 4. The 

inorganic requirement is ±35% of the true value of the spike. The organic requirement is ±20% 

of the LCS limits a laboratory has in place, which should be a wider recovery limit for most 

compounds, but will vary with each individual laboratory's statistical values. 

2. Comment: 

Commenter #2 commented, regarding Chapter 4, Table 4-1, that for volatile organics analyses 

(VOAs), "If compounds that readily degrade in acidified water (e.g., 2-chloroethyl vinyl ether) are 

analytes of interest, collect a second set of samples without acid preservatives and analyze as 

soon as possible." The table shows a holding time of 7 days for such analyses. 

Footnote b to the table reads: "See References 1-10 for the preservation and holding times 

studies for volatile organics and the January and February 2012 RCRA Organic Workgroup 

discussion for preservation and holding times for vinyl chloride, styrene and 2-chloroethyl vinyl 

ether in aqueous samples." References 15, 16 and 17 then list the RCRA Organic Methods 

Workgroup Meeting Minutes from January 19, 2012, January 26, 2012 and February 9, 2012. 

From this combination of information, it is not clear whether the intended guidance is for 

collection of a second set of unpreserved samples only in cases where 2-chloroetyhyvinyl ether 

is an analyte of interest, or whether a second set of unpreserved samples should be collected 

when 2-chloroethyl vinyl ether, vinyl chloride or styrene are among the analytes of interest. The 

table should be revised to clarify the intent of the guidance. 

The January and February 2012 RCRA Organics Workgroup Meeting Minutes from January 19, 

January 2 and February 9, 2012 are not publically available. EPA should either make these 

available, include the pertinent information from them in Chapter 4, or refrain from citing them as 

references. If the content of the references is not available, the references are useless. 

Response: 

The Agency agrees with the commenter and has placed the January 19, 26 and February 9, 

2012 minutes in the Docket. 

Footnote b of Table 4-1 has been revised to read: "See References 1-10 for the preservation 

and holding times studies for volatile organics. It is the intention of the Agency that separate, 

unpreserved vials be collected when 2-chloroethylvinyl ether is an analyte of interest." 
 Page 19 

3. Comment: (The Agency received two similar comment on volatile preservation. They 

are answered here together.) 

Commenter #3 commented, regarding Chapter 4, that we approve of the removal of the 

requirement to analyze vinyl chloride and styrene from an unpreserved sample in Chapter 4. 

Both compounds have been demonstrated to be stable at pH 2. However we noted that the 

same change had not been made for soil samples, and request the following change in the 

volatile organics, solid samples Section of Table 4.1 of Chapter 4: If compounds that may be 

reactive in acidified soils (e.g., vinyl chloride, styrene, 2-chloroethyl vinyl ether) are analytes of

interest, do not use acid preservation options. Collect a second set of samples without acid 

preservatives and analyze as soon as possible. 

and 

Commenter #9 commented, regarding Chapter 4, FR page 63191: Previous versions of Chapter 

4 stated that vinyl chloride and styrene had to be analyzed from an unpreserved vial. EPA 

responded by removing the requirement in Chapter 4, for aqueous samples. This is a positive 

change; however, styrene and vinyl chloride should also be removed from the following 

statement for solid samples: "If compounds that may be reactive in acidified soils (e.g., vinyl 

chloride, styrene, 2-chloroethyl vinyl ether) are analytes of interest, collect a second set of 

samples without acid preservatives and analyze as soon as possible." 

Response: 

The Agency removed the requirement for vinyl chloride and styrene in a water matrix after 

reviewing performance data from a study that was received by ORCR. In order to remove the 

requirement for soils, the Agency welcomes data from a similar study demonstrated for solid 

matrices. The Agency still recommends a second unpreserved set of samples be taken any 

time 2-chloroethylvinyl ether is a target compound. 

4. Comment: 

Commenter #9 commented, regarding Chapter 4, FR (on page 63191), that they thank and 

congratulate the Agency on the removal of the requirement for a separate sample for styrene 

and vinyl chloride in Chapter 4. 

Response: 

The Agency appreciates the input. 

5. Comment: 

Commenter #4 commented, regarding Chapter 4, Section 4.1.6, Page FOUR-7, Step 3: Please 

note that both AlconoxTM and SparkleenTM contain a substantial amount of phosphate, and are 

not recommended for the phosphate-free decontamination applications prescribed in Section 

3.3.3 of SW-846 Chapter Three. When a phosphate-free detergent is recommended, AlconoxTM 

and SparkleenTM should not be used. LiquinoxTM, which does not contain phosphate, should be 

used. Recommended edit: Suggest that the last two sentences about AlconoxTM and 

SparkleenTM be deleted. Or, delete the last sentence and change "Alconox" to "LiquinoxTM", 

and explain that LiquinoxTM is a phosphate-free detergent that will not cause false positives for 

phosphate analysis or contribute to excess weed growth in surface water. 

Response: 

Chapter 4 deals with organic analyses and as such, phosphate contamination is not a primary 

concern. Any detergents used by the laboratories should be eliminated during the washing and 
 Page 20 

thorough rinsing process. It is up to the individual laboratories to select whatever detergents 

best suit their cleaning needs. If phosphates are concern to the analysis, a low phosphate or 

phosphate-free detergent would be most appropriate. 

6. Comment: 

Commenter #4 commented, regarding Chapter 4, Section 4.3.2, Method 8276 should be 

included in the list of methods in this Section. Recommended edit: Add method 8276 to the list 

of methods in this Section. 

Response: 

The Agency agrees with the commenter and has added Method 8276 to Table 4.3.2. 

7. Comment: 

Commenter #4 asked, regarding Chapter 4, Section 4.3.3, should method 8330A be changed to 

8330B in the list of methods in this Section? Or should method 8330B be included in the list? 

Recommended edit: Replace or add method 8330B to the list of methods in this Section. 

Response: 

The Agency disagrees with the commenter as 8330A is the current published method. We will 

revisit and publish 8330B when time and resources allow in the future. 

8. Comment: 

Commenter #4 commented, regarding Chapter 4, Table 4-1, Pages FOUR-11 & FOUR-12, 

Aqueous samples: Aqueous samples should not be cooled to ≤ 6 °C (i.e., < 0 °C) and frozen. 

Also, suggest that "3 x 40-mL vials" be collected. To avoid potential breakage of 1-L glass 

containers due to frozen water, aqueous samples should be cooled to 0 - 6 °C. Recommended 

edit: Change "≤ 6 °C" to "0 - 6 °C" and "2 x 40-mL" to "3 x 40-mL". 

Response: 

The Agency agrees with the commenter and has made the proposed edits. 

9. Comment: 

Commenter #4 commented, regarding Chapter 4, Table 4-1, Pages FOUR-9 & FOUR-10, 

Aqueous VOC samples: Aqueous samples should not be cooled to ≤ 6 °C (i.e., < 0 °C) and 

frozen. Also, suggest that "3 x 40-mL vials" be collected. To avoid potential VOC vial breakage 

due to frozen water, aqueous samples should be cooled to 0 - 6 °C. Also, recommend that 3 x 

40-mL vials be collected for the initial sample screening, sample analysis, and sample reanalysis, if needed. Recommended edit: Change "≤ 6 °C" to "0 - 6 °C" and "2 x 40-mL" to "3 x 

40-mL". 

Response: 

The Agency agrees with the commenter and has made the proposed edits. 

 
 Page 21 

CHAPTER NINE 

1. Comment: 

Commenter #9 commented, regarding Chapter One and Chapter Nine, that additional guidance 

has been provided in the proposed revision of Chapter 1 (including references) regarding the 

calculation of the UCL for making the determination as to whether a waste may be hazardous. 

Specifically, in Section 1.1.3.2 of Chapter 1, several documents are listed for the development 

of Sampling and Analysis Plans. At least two of these documents contradict one another in their 

use of the UCL for making the determination that the analytical results for a given waste could 

exceed the RCRA limit. 

• In SW-846, Chapter 9, Page 16, starting in Section 7 and Equation 6 (which is repeated 

multiple times in Chapter 9), the two-tailed critical value for the Student's t distribution is used. 

• In Chapter 1, Reference 8, "RCRA Waste Sampling Draft Technical Guidance" (EPA 503-D02-002), in Section 3.4.3.1, Appendices F (Equation F.6) and G (Table G-1) the single-tailed 

critical value for the Student's t distribution is used. 

The commenter believes that use of the single-tailed critical value is statistically correct and 

asks that either Chapter 9 be revised to utilize the single-tailed critical value for the UCL or the 

conflicting references in Chapter 1 be removed. 

Response: 

Chapter 9 is not included in Update V and as such, is not subject to revision at this time. The 

Agency thanks the commenter for their input and the comment will be discussed the next time 

Chapter 9 is updated. 

 
 Page 22 

METHOD 3200 

1. Comment: 

Commenter #4 commented, regarding Method 3200, Section 11.2.1.4, that the Section states 

cold sample storage requirements "Store extracts in the cold at 4 °C until analysis". The current 

storage requirements as stated in Chapter 3 are to "store extracts in the cold at ≤6 °C until 

analysis." Recommended edit: Update from old requirements (4 °C) to new requirements (≤6 

°C). 

Response: 

The Agency agrees with the commenter and has made the requested change in Method 3200, 

Section 11.2.1.4. 

The rest of the Update V methods were searched and the same temperature range correction 

was made in Method 8410 (Section 7.4.2) and Method 8430 (Sections 7.5.2, 8.2 and 11.3.4). 

 
 Page 23 

METHOD 6010D 

1. Comment: 

Commenter #4 commented, regarding Method 6010D, that the text states: "In the absence of 

project-specific DQOs, the method blank may be considered to be acceptable with respect to 

each target element, if it is less than the LLOQ, 50% of the regulatory limit, or 10% of the lowest 

sample concentration, whichever is greater." Recommended edit: Define if the "lowest sample 

concentration" is relative to the sample delivery group (SDG), batch, or site samples. 

Response: 

The Agency believes that guidance in this section is clear and refers to analytical batch. Refer 

to the subsequent sentences of this paragraph as follows: "If the method blank fails to meet the 

necessary acceptance criteria, it should be re-analyzed once. If still unacceptable, then all 

samples associated with the method blank must be re-prepared and re-analyzed, along with all 

other appropriate analysis batch QC samples". Also refer to the previous language in section 

9.7: "At a minimum, this should include the analysis of QC samples including a method blank, a 

matrix spike (MS), a laboratory control sample (LCS), and a duplicate sample in each analytical 

batch". 

2. Comment: 

Commenter #7 commented, regarding Method 6010D, regarding method blank (Section 9.7.1): 

In the absence of project level DQOs, the method blank may be considered to be acceptable if 

< LLOQ or < 50% of regulatory limit or < 10% of the lowest sample concentration, whichever is 

greater. This guidance should be revised such that if there is no regulatory limit and the method 

blank is >10% of the lowest sample concentration, then the method blank must be less than 

50% of the LLOQ to avoid significant bias for samples near the LLOQ. Allowing a method blank 

to be at the LLOQ would significantly bias the sample results near the LLOQ. 

Response: 

The Agency disagrees and contends 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. 

3. Comment: 

Commenter #7 asked, regarding Method 6010D (Section 9.7.3): Is there an error in line 6 of the 

2nd paragraph? Should "method blank" be changed to "LCS"? In this same section of 6010C, 

the term LCS was used. 

Response: 

The Agency confirms there is no error and "method blank" is correct as it helps define the 

analytical batch associated with the unacceptable LCS. 

4. Comment: 

Commenter #7 commented, regarding Method 6010D (Section 9.11.1): If the analyte 

concentration is within the linear range of the instrument and sufficiently high (minimally, a factor 

of 25 times greater than the LLOQ), an analysis of a 1:5 dilution should agree to within ± 20% of 

the original determination. The acceptance limit of +/- 10% of the original determination should 

be maintained (same limits as Method 6010C). Responses that are outside +/- 10% of the 

original response are likely biased by the sample matrix. 

 
 Page 24 

Response: 

The Agency disagrees and contends that concentrations that are outside +/- 20% of the original 

determination are likely biased by the sample matrix. This method is intended as guidance. 

The analytical laboratory may use tighter QC limits than specified in the method (such as ±10%) 

if their regulatory body recommends them or if they have a good reason to do so. 

5. Comment: 

Commenter #4 commented, regarding Method 6010D, Sections 4.1.1.2 & 9.6 that "analytical 

range" is not well defined in the SW-846 and is not commonly used by the environmental labs. 

Recommended edit: Change the "analytical range" to "quantitation range" or "calibration range". 

Response: 

The Agency appreciates this comment; however, the Agency feels the term "analytical range" is 

adequately defined in describing how to mitigate spectral interferences, which is the major 

emphasis of section 4.1.1.2. "Analytical range" is not mentioned in Section 9.6. 

6. Comment: 

Commenter #4 recommended, regarding Method 6010D, Section 7.9, correct the typo of "105 

EC". Recommended edit: Change "105 EC" to "105 °C". 

Response: 

The Agency agrees with the commenter's suggested correction. "105 EC" in Section 7.9 has 

been changed to "105 °C". 

7. Comment: 

Commenter #4 commented, regarding Method 6010D, Section 7.9.24, that silver standard 

solutions should be protected from light. Silver ions may precipitate out from solution if exposed 

to light. Recommended edit: Request that silver standard solutions be protected from light by 

storing in a dark room or wrapping the standard containers with aluminum foils. 

Response: 

The Agency agrees with the commenter's suggested edit. The following sentence has been 

added to Section 7.9.24: "Protect standard from light during storage." 

8. Comment: 

Commenter #4 recommended, regarding Method 6010D, Section 9.3, provide the detailed 

procedures for calculating the IDL. The procedures for determining IDL are not provided in the 

SW-846. Recommended edit: Please provide the procedures or references for determining and 

calculating an IDL for metals analysis. 

Response: 

The Agency thanks the commenter for their input; however, the Agency feels the procedures for 

calculating the IDL are sufficiently described in Section 9.3 as follows: "IDLs in μg/L can be 

estimated as the mean of the blank results plus three times the standard deviation of 10 

replicate analyses of the reagent blank solution. (Use zero for the mean if the mean is 

negative)". 

9. Comment: 

Commenter #4 commented, regarding Method 6010D, Section 9.8.2, that more details on LLOQ 

verifications are needed. The frequency LLOQ verifications for infrequently run analyses should 

be increased to establish in-house control limits. The logistics on LLOQ verifications with 
 Page 25 

sample matrices should also be addressed. Recommended edit: More guidance should be 

provided. 

Response: 

The Agency believes the method provides adequate guidance on LLOQ verifications. The 

method allows for more frequent LLOQ verifications by only specifying a minimum frequency. 

Logistics are not detailed to allow options for laboratories to use a clean control material or a 

representative sample matrix (free of target compounds) to achieve LLOQ verifications less than 

the desired regulatory action levels or based on the stated project-specific requirements. 

10. Comment: 

Commenter #4 commented, regarding Method 6010D, Sections 10.8.4 and 10.8.5, and Method 

6020B, Sections 10.5.4 and 10.5.5, that Sections 10.8.4 and 10.5.4 address the analysis and 

acceptance criteria for the initial calibration blank (ICB), as in the following paragraph: "Initial 

Calibration Blank (ICB) - If a multi-level calibration is used, an ICB is analyzed immediately after 

the calibration (or after the ICV) and must not contain analytes above half the LLOQ. If a single 

point calibration is used, the calibration is forced through the ICB, but a second ICB is analyzed 

as a check and must not contain target analytes above half the LLOQ." Sections 10.8.5 and 

10.5.5 address the analysis of and acceptance criteria for continuing calibration blanks (CCBs). 

The CCB acceptance criteria is that the CCB must not contain target analytes > the LLOQ, 

which differs from the ICB acceptance criteria. Section 10.8.5 then contains this sentence: "If 

the ICB consistently has target analyte concentrations greater than half the LLOQ, the LLOQ 

should be re-evaluated." The last sentence would make more sense in Section 10.8.4, where 

the ICB analysis and acceptance is addressed. Recommended edit: Move the following 

sentence from Sections 10.8.5 and 10.5.5 to 10.8.4 and 10.5.4: "If the ICB consistently has 

target analyte concentrations greater than half the LLOQ, the LLOQ should be re-evaluated." 

Do NOT include a similar sentence in 10.8.5 or 10.5.5. 

Response: 

The Agency agrees with the recommended edit to move the sentence: "If the ICB consistently 

has target analyte concentrations greater than half the LLOQ, the LLOQ should be reevaluated" from Section 10.8.5 to Section 10.8.4. The Agency acknowledges and confirms that 

the acceptance criteria for the CCB differ from the acceptance criteria for the ICB. 

11. Comment: 

Commenter #4 commented, regarding Method 6010D, Section 7.10, and 6020B, Section 7.27, 

that the following sentence does not make sense: "If the determination of one or more metals 

using a non-aqueous solvent is required, then all standards and quality control samples must be 

prepared on a weight/weight basis in the non-aqueous solvent since the density of non-aqueous 

solvents is not unity." Recommended edit: Change the sentence to: "If the determination of one 

or more metals using a non-aqueous solvent is required, then all standards and quality control 

samples must be prepared on a weight/weight basis in the non-aqueous solvent since the 

density of non-aqueous solvents is not uniform." 

Response: 

The Agency agrees with the commenter's recommended edit. The word "unity" in Method 

6010D, Section 7.10, and Method 6020B, Section 7.27 has been changed to "uniform". 

12. Comment: 

Commenter #4 commented, regarding Method 8000D, Section 9.4.2.1, and Method 6010D, 

Section 9.7.2 ,that the "1 - 5 times the background concentration" is not always appropriate. If 
 Page 26 

the background concentration is very low or non-detect (e.g., organic analytes), any spike 

amount may lead to a ratio between the spike concentration and the background concentration 

> 5; however, the MS/MSD data are generally useable. Recommended edit: Suggest that a 

NOTE such as "NOTE: If the background sample concentration is very low or non-detect, a 

spike of greater than 5 times the background concentration is still acceptable. To assess data 

precision with duplicate analyses, it is preferred to use a low concentration field sample to 

prepare MS/MSD for organic analyses and a high concentration field sample to prepare 

unspiked laboratory duplicates for metals analyses." 

Response: 

The Agency agrees with the commenter and has revised the note in Section 9.7.2 of 6010D and 

6020B: "NOTE: If the background sample concentration is very low or non-detect, a spike of 

greater than 5 times the background concentration is still acceptable. To assess data precision 

with duplicate analyses, it is preferable to use a high concentration field sample to prepare 

unspiked laboratory duplicates for metals analyses." 

Comments on 6010D received after Public Comment period was over: 

Comment #2, regarding Methods 6010D, Section 9.6 and 6020B, Section 9.6: Running a linear 

range on each run puts every sample at risk of a false positive due to carry-over that cannot be 

distinguished from low level analyte in the sample. Running a linear range on each run also 

significantly increases out of specifications for initial and continuing check blanks, as well as 

method blanks, due to carry-over. Any individual sample can randomly contain high levels of 

analyte and cause this issue, but analyzing a linear range on every run elevates the risk. 

Response: 

The Agency thanks the commenter for their input; however, Section 9.6 of Method 6010D and 

Section 9.6 of Method 6020B do not require the analysis of a higher standard to extend the 

linear range, but gives the laboratory the option to do so. A laboratory should not run a highlevel linear range standard if doing so produces memory effects that affect lower level readings. 

The laboratory can go with the option of demonstrating linearity up to their highest calibration 

standard and dilute if any samples are out of the calibration range. 

Comment #3, regarding Methods 6010D, Sections 9.9.1 and 9.9.2 and Method 6020B, Section 

9.9: The analysis of a SIC (Spectral Interference Check) has contradictory wording in Method 

6010D. Section 9.9.1 says single element checks should be < 2x the LOQ, Section 9.9.2 says 

that multi element SIC should be < LOQ. Previous methods require < 2x LOQ. The 

requirement of < LOQ in a solution with interferences in this range will require that laboratories 

raise their routine LOQs in order to pass this more restrictive requirement. Raised LOQs are 

contradictory to the requirements requested by most clients. 

Response: 

The Agency thanks the commenter for their input; however the requirement for the mixed 

element SIC solution in Section 9.9.2 of Method 6010D is +/- the LLOQ and not <LLOQ as 

stated in the comment. The requirement for the mixed element SIC is to ensure interference 

corrections are in control on a regular basis. The laboratory also has the option of raising the 

LLOQ to twice the concentration measured in the mixed element SIC solution. The requirement 

for the mixed element SIC solution in Section 9.9 of Method 6020B is stated as <2x the LLOQ. 

 
 Page 27 

METHOD 6020B 

1. Comment: 

Commenter #4 commented, regarding Method 6020B, Sections 10.5.4 and 10.5.5, and 6010D, 

Sections 10.8.4 and 10.8.5, that Sections 10.8.4 and 10.5.4 address the analysis and 

acceptance criteria for the ICB, as in the following paragraph: "Initial Calibration Blank (ICB) - If 

a multi-level calibration is used, an ICB is analyzed immediately after the calibration (or after the 

ICV) and must not contain analytes above half the LLOQ. If a single point calibration is used, 

the calibration is forced through the ICB, but a second ICB is analyzed as a check and must not 

contain target analytes above half the LLOQ." Sections 10.8.5 and 10.5.5 address the analysis 

of and acceptance criteria for continuing calibration blanks (CCBs). The CCB acceptance 

criteria is that the CCB must not contain target analytes > the LLOQ, which differs from the ICB 

acceptance criteria. Section 10.8.5 then contains this sentence: "If the ICB consistently has 

target analyte concentrations greater than half the LLOQ, the LLOQ should be re-evaluated." 

The last sentence would make more sense in Section 10.8.4, where the ICB analysis and 

acceptance is addressed. Recommended edit: Move the following sentence from Sections 

10.8.5 and 10.5.5 to 10.8.4 and 10.5.4: "If the ICB consistently has target analyte 

concentrations greater than half the LLOQ, the LLOQ should be re-evaluated." Do NOT include 

a similar sentence in 10.8.5 or 10.5.5 

Response: 

The Agency agrees with the recommended edit to move the sentence: "If the ICB consistently 

has target analyte concentrations greater than half the LLOQ, the LLOQ should be reevaluated." from Section 10.5.5 to Section 10.5.4. The Agency acknowledges and confirms that 

the acceptance criteria for the CCB differ from the acceptance criteria for the ICB. 

2. Comment: 

Commenter #4 commented, regarding Method 6020B, Section 7.27, and 6010D, Section 7.10, 

that the following sentence does not make sense: "If the determination of one or more metals 

using a non-aqueous solvent is required, then all standards and quality control samples must be 

prepared on a weight/weight basis in the non-aqueous solvent since the density of non-aqueous 

solvents is not unity." Recommended edit: Change the sentence to: "If the determination of one 

or more metals using a non-aqueous solvent is required, then all standards and quality control 

samples must be prepared on a weight/weight basis in the non-aqueous solvent since the 

density of non-aqueous solvents is not uniform." 

Response: 

The Agency agrees with the commenter's recommended edit. The word "unity" in Method 

6020B, Section 7.27, and Method 6010D, Section 7.10 has been changed to "uniform". 

3. Comment: 

Commenter #7 commented, regarding Method 6020B (Section 9.7.1): In the absence of project 

level DQOs, the method blank may be considered to be acceptable if < LLOQ or < 50% of 

regulatory limit or <10% of the lowest sample concentration, whichever is greater. This 

guidance should be revised such that if there is no regulatory limit and the method blank is 

>10% of the lowest sample concentration, then the method blank must be less than 50% of the 

LLOQ to avoid significant bias for samples near the LLOQ. Allowing a method blank to be at 

the LLOQ would significantly bias the sample results near the LLOQ. 
 Page 28 

Response: 

The Agency disagrees and contends 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. 

4. Comment: 

Commenter #7 commented, regarding Method 6020B (Section 9.10): The intensities of each 

internal standard must be monitored for every analysis to ensure that it does not decrease 

below 30%, with respect to its intensity during the initial calibration. Allowing up to a 70% drop 

in response will significantly compromise the sensitivity of the analysis. A lower limit of 50% in 

internal standard response would be more appropriate. 

Response: 

The Agency believes the commenter is misinterpreting the criterion. The criterion allows up to a 

30% drop in response. As an example, if the initial calibration internal standard response is 

100,000 counts per second (cps), anything below 70,000 cps in the sample would be 

unacceptable. The text from 9/10 of 6020B currently states: "The intensities of each internal 

standard must be monitored for every analysis to ensure that it does not decrease below 30%, 

with respect to its intensity during the initial calibration."

5. Comment: 

Commenter #7 commented, regarding Method 6020B (Section 9.13.1): If the analyte 

concentration is within the linear range of the instrument and sufficiently high (minimally, a factor 

of 25 times greater than the LLOQ), an analysis of a 1:5 dilution should agree to within ± 20% of 

the original determination. The acceptance limit of +/- 10% of the original determination should 

be maintained (same limits as method 6020A). Responses that agree to only +/- 11% thru +/- 

20% are likely biased by the sample matrix. 

Response: 

The Agency disagrees and contends that concentrations that are outside +/- 20% of the original 

determination are likely biased by the sample matrix. This method is intended as guidance. 

The analytical laboratory may use tighter QC limits than specified in the method (such as ±10%) 

if their regulatory body recommends them or if they have a good reason to do so. 

6. Comment: 

Commenter #7 commented, regarding Method 6020B (Section 10.4): If a multipoint calibration 

is used, the low standard must be at or below the LLOQ. There may be situations where the 

low standard could be above the LLOQ. The wording should be changed from "must" to 

"should". If the LLOQ is not on the curve, an LLOQ Check Standard should be analyzed and 

evaluated against the curve. We recommend a limit of +/- 20%. 

Response: 

The Agency disagrees. The Agency believes the low standard should be representative of a 

concentration at or below the laboratory's LLOQ; therefore there will be no situations where the 

low standard of a multipoint calibration could be above the LLOQ. For all multipoint calibration 

scenarios, the lowest non-zero standard concentration should be considered the LLOQ. 

7. Comment: 

Commenter #7 commented, regarding Method 6020B (Section 11.4): Replicate scans of the 

tuning solution should be required to confirm the instrument is stable (≤5% RSD), as per Method 

6020A. 
 Page 29 

Response: 

The Agency appreciates this comment; however, replicate scans of the tuning solution were 

eliminated to allow the laboratory the ability to determine instrument stability. 

8. Comment: 

Commenter #4 commented, regarding Method 6020B, Section 1.2, Page 2 of the method, below 

the table of analytes, that the term "inductively coupled plasma-atomic emission spectrometry" 

is used, when, in Method 6010D all references to that term have been changed to "inductively 

coupled plasma-optical emission spectrometry." Recommended edit: Change all references in 

6020B from "inductively coupled plasma-atomic emissions spectrometry" to inductively coupled 

plasma-optical emission spectrometry." 

Response: 

The Agency agrees with the commenter's recommended edit. The term "inductively coupled 

plasma-atomic emission spectrometry" in Method 6020B, Section 1.2, below the table of 

analytes, has been changed to the term "inductively coupled plasma-optical emission 

spectrometry." 

9. Comment: 

Commenter #4 commented, regarding Method 8000D, Section 9.4.2.1, and Method 6010D, 

Section 9.7.2 , that the "1 - 5 times the background concentration" is not always appropriate. If 

the background concentration is very low or non-detect (e.g., organic analytes), any spike 

amount may lead to a ratio between the spike concentration and the background concentration 

> 5; however, the MS/MSD data are generally useable. Recommended edit: Suggest that a 

NOTE such as "NOTE: If the background sample concentration is very low or non-detect, a 

spike of greater than 5 times the background concentration is still acceptable. To assess data 

precision with duplicate analyses, it is preferred to use a low concentration field sample to 

prepare MS/MSD for organic analyses and a high concentration field sample to prepare 

unspiked laboratory duplicates for metals analyses." 

Response: 

The Agency agrees with the commenter and has revised the note in Section 9.7.2 of 6020B: 

"NOTE: If the background sample concentration is very low or non-detect, a spike of greater 

than 5 times the background concentration is still acceptable. To assess data precision with 

duplicate analyses, it is preferable to use a high concentration field sample to prepare unspiked 

laboratory duplicates for metals analyses." 

Comments on 6020B received after Public Comment period was over: 

Comment #2, regarding Methods 6010D, Section 9.6 and 6020B, Section 9.6: Running a linear 

range on each run puts every sample at risk of a false positive due to carry-over that cannot be 

distinguished from low level analyte in the sample. Running a linear range on each run also 

significantly increases out of specifications for initial and continuing check blanks, as well as 

method blanks, due to carry-over. Any individual sample can randomly contain high level of 

analyte and cause this issue, but analyzing a linear range on every run elevates the risk. 

Response: 

The Agency thanks the commenter for their input; however, Section 9.6 of Method 6010D and 

Section 9.6 of Method 6020B do not require the analysis of a higher standard to extend the 

linear range, but gives the laboratory the option to do so. A laboratory should not run a high-
 Page 30 

level linear range standard if doing so produces memory effects that affect lower level readings. 

The laboratory can go with the option of demonstrating linearity up to their highest calibration 

standard and dilute if any samples are out of the calibration range. 

Comment #3, regarding Methods 6010D, Sections 9.9.1 and 9.9.2 and Method 6020B, Section 

9.9: The analysis of a SIC (Spectral Interference Check) has contradictory wording in Method 

6010D. Section 9.9.1 says single element checks should be < 2x the LOQ, Section 9.9.2 says 

that multi element SIC should be < LOQ. Previous methods require < 2x LOQ. The 

requirement of < LOQ in a solution with interferences in this range will require that laboratories 

to raise their routine LOQs in order to pass this more restrictive requirement. Raised LOQs are 

contradictory to the requirements requested by most clients. 

Response: 

The Agency thanks the commenter for their input; however the requirement for the mixed 

element SIC solution in Section 9.9.2 of Method 6010D is +/- the LLOQ and not <LLOQ as 

stated in the comment. The requirement for the mixed element SIC is to ensure interference 

corrections are in control on a regular basis. The laboratory also has the option of raising the 

LLOQ to twice the concentration measured in the mixed element SIC solution. The requirement 

for the mixed element SIC solution in Section 9.9 of Method 6020B is stated as <2x the LLOQ. 

Comment from the Method Information Communication Exchange (MICE) line: 

The only item that remains a little unclear is what defines "official" with regard to a version of 

6020B. The Federal Register notice of 10/23/13 which made available 6020B, Revision 2, 

October 2012 states, "Update V contains 23 new and revised analytical methods that the 

Agency has evaluated, and which may be used for monitoring or complying with the RCRA 

hazardous and non-hazardous waste regulations". I can appreciate that the methods were 

issued with the need for a public comment period, after which the methods could be changed 

yet again. However, there is some level of "officialness" if the Agency has declared these 

methods suitable for use in complying with RCRA. This of course is in agreement with the core 

philosophy of SW846 methods being guidance documents in the first place. 

The only other item we found yesterday was that Table 2 Recommended Elemental Isotopes for 

Selected Elements is missing one of the most important isotopes for molybdenum (Mo) at mass 

95. This may not be the most abundant Mo isotope but it is the most abundant Mo isotope that 

does not require isobar corrections. Even though it is only in Table 2 as a potential interferent, 

when it is quantified as an analyte it might be beneficial to use Mo-95. 

Response: 

The draft version of 6020B found on the Federal Register notice should not be considered final. 

It was a draft for public comment. The official release of 6020B will be with Update V with all the 

public comments addressed. The updated methods will have a July 2014 date in the footer. 

The Agency agrees with the comment and has added Mo-95 as an analytical mass to Table 2. 

 
 Page 31 

METHOD 8000D 

1. Comment: 

Commenter #3 commented, regarding Method 8000D, that they approve of the use of LCS 

limits with an additional +/- 20% as a reasonable way to set initial limits for LLOQ standards. 

Response: 

The Agency thanks the commenter for their input.

2. Comment: 

Commenter #3 commented, regarding Method 8000D, that clarifications to the initial 

demonstration of proficiency requirements are useful and will serve to improve consistency in 

the ways that laboratories approach their demonstrations of capability. 

Response: 

The Agency thanks the commenter for their input.

3. Comment: 

Commenter #3 commented, regarding Method 8000D, that they strongly approve of the addition 

of relative standard error (RSE) as a method for evaluation of calibration curves, and appreciate 

the consistency with similar approval in CFR 40 Part 136. 

Response: 

The Agency thanks the commenter for their input.

4. Comment: (Note: The Agency received two similar comments on this Section. They have 

been listed together as the response covers both items.) 

Commenter #7 commented, regarding Method 8000D (Section 9.2.6.7): The LLOQ may be 

raised to 5x the method blank response to avoid reporting false positives. This allowance to 

elevate the LLOQ for individual data sets due to lab contamination may be inappropriate for 

some data sets. The elevated LLOQ could mask the method blank response and make it 

appear that sample responses just above the LLOQ were unbiased by lab contamination. The 

preferred approach would be to determine an LLOQ that is consistently 5x greater than lab 

contamination. Data sets where the method blank exceeds that LLOQ should have appropriate 

corrective actions taken and then if the blank is still greater than the LLOQ, the sample results 

should be appropriately qualified. 

and 

Commenter #4 commented, regarding Method 8000D, Section 9.2.6.7, note, that the analyst 

may raise the LLOQ to 5x the blank concentration to avoid reporting false positive results. If the 

LLOQ is raised, the precision and bias should be updated. Recommended edit: Add statement 

that: When raising the LLOQ to 5x the blank concentration, the precision and bias must be 

updated as well. 

Response: 

The note in 8000D Section 9.2.6.7: "NOTE: The analyst may raise the LLOQ to 5x the blank 

concentration to avoid reporting false positive results" was removed and replaced by the 

following language, which was discussed and approved by the work group: 
 Page 32 

9.2.6.9 Blanks are generally considered to be acceptable if target analyte concentrations are 

less than one-half 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. 

9.2.6.10 If an analyte of interest is found in a sample in the batch near a concentration 

confirmed in the blank (refer to Sec. 9.5.2), the presence and or/concentration of that analyte 

should be considered suspect and may require qualification. Contaminants in the blank should 

meet most or all of the qualitative identifiers in Section 11.6 to be considered. Samples may 

require re-extraction and/or re-analysis if the blanks do not meet lab established or projectspecific criteria. Re-extraction and/or re-analysis is not necessary if the analyte concentration 

falls well below the action or regulatory limit or if the analyte is deemed not important for the 

project. 

9.2.6.11 When new reagents or chemicals are received, the lab should monitor the blanks 

associated with samples for any signs of contamination. It is not necessary to test every new 

batch of reagents or chemicals prior to sample preparation if the source shows no prior 

problems. However, if reagents are changed during a preparation batch, separate blanks need 

to be prepared for each set of reagents.

5. Comment: 

Commenter #7 commented, regarding Method 8000D (Section 9.3): Section 9.3.4.4: Multiplelaboratory performance data are included in some determinative methods and may be used as 

guidance in evaluating performance in a single laboratory. Many of the individual organics 

methods in SW-846 do not have acceptance criteria so default limits should be defined. We 

suggest adding the target limits 50% to 150% for recovery. 

Response: 

The following language was added to Section 9.3.4.4: "Once sufficient data points are available, 

each laboratory is strongly encouraged to develop in-house control limits." DoD 2013 LCS 

study results can be referenced in Section 16 of Method 8000D. 

6. Comment: 

Commenter #7 commented, regarding Method 8000D (Section 9.7): The laboratory shall 

establish the LLOQ as the lowest point of quantitation, which in most cases, is the lowest 

concentration in the calibration curve. It would be helpful to include a more complete and 

detailed section in Method 8000D that describes techniques to establish the LLOQ. Simply 

defining it as the lowest concentration in the calibration curve does not seem adequate or 

appropriate in many cases. There are situations where you would want to have calibration 

standards below the equivalent LLOQ for a particular sample matrix to establish more 

appropriate calibration factors near the LLOQ. We would recommend referencing the following 

approach for determining the LLOQ, to be done as part of the method validation process: 

Report of the Federal Advisory Committee on Detection and Quantitation Approaches and Uses 

in Clean Water Act Programs (December 2007). 

Response: The Agency thanks the commenter for their input. The language in Section 9.7 has 

been updated. 
 Page 33 

7. Comment: 

Commenter #7 commented, regarding Method 8000D, that acceptance criteria for linear 

regressions (Section 11.5.2.2): r or r2 should be at or above 0.995 and 0.99, respectively. I 

think this should remain as a "must" criterion. 

Response: 

The Agency will retain the existing language in the method. The use of "should" in the text is to 

allow flexibility for project-level DQOs to determine the data use. 

8. Comment: 

Commenter #9 commented, regarding Method 8000D (found on FR Page 63192), that they 

approve of basing the LLOQ acceptance limits on the laboratory control sample limits with the 

addition of 20 percent. 

Response: 

The Agency appreciates the input. 

9. Comment: 

Commenter #4 commented, regarding Method 8000D, Section 9.4.2.1, and Method 6010D, 

Section 9.7.2, that the "1 - 5 times the background concentration" is not always appropriate. If 

the background concentration is very low or non-detect (e.g., organic analytes), any spike 

amount may lead to a ratio between the spike concentration and the background concentration 

> 5; however, the MS/MSD data are generally useable. Recommended edit: Suggest that a 

NOTE such as "NOTE: If the background sample concentration is very low or non-detect, a 

spike of greater than 5 times the background concentration is still acceptable. To assess data 

precision with duplicate analyses, it is preferable to use a low concentration field sample to 

prepare MS/MSD for organic analyses and a high concentration field sample to prepare 

unspiked laboratory duplicates for metals analyses." 

Response: 

The Agency agrees and has added the following note to Section 9.4.2.1 of Method 8000D: 

"NOTE: If the background sample concentration is very low or non-detect, a spike of greater 

than 5 times the background concentration is still acceptable. To assess data precision with 

duplicate analyses, it is preferable to use a low concentration field sample to prepare a MS/MSD 

for organic analyses." 

The following note was added to Section 9.7.2 of 6010D and 6020B: "NOTE: If the background 

sample concentration is very low or non-detect, a spike of greater than 5 times the background 

concentration is still acceptable. To assess data precision with duplicate analyses, it is 

preferable to use a high concentration field sample to prepare unspiked laboratory duplicates for 

metals analyses." 

10. Comment: 

Commenter #4 commented, regarding Method 8000D, Section 11.5.2.2, that the first sentence 

of the last paragraph, "In order for the linear regression model to be used for quantitative 

purposes, r or r2

 should be ≥ 0.995, and 0.99, respectively" needs a revision. Recommended 

edit: Change the sentence to "In order for the linear regression model to be used for quantitative 

purposes, r or r2 should be ≥ 0.995 or 0.99, respectively." 

Response: 

The Agency agrees and made the requested edit. 
 Page 34 

11. Comment: 

Commenter #4 commented, regarding Method 8000D, Section 11.5.4.2: "If the RSD limit is not 

defined in the determinative method, the limit should be set at ≤20% for good performing 

compounds and ≤30% for poor performing compounds." Poor performing compounds are 

laboratory dependent, and should be held to same criteria as other analytes unless removed 

from consideration through the DQO process. Recommended edit: Remove the 30% criteria for 

poor performers. 

Response: 

The Agency disagrees with the commenter and Section 11.5.4.2 remains unchanged. 

12. Comment: 

Commenter #4 commented, regarding Method 8000D, Section 11.5.6.1, that RSE should not be 

grouped with RSD and r2, 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 back check a calibration curve. To avoid confusions with RSD, 

RSE should not be grouped with RSD; especially since there is no mathematical derivation for 

RSE like RSD. Recommended edit: Change the first sentence to "Corrective action may be 

needed if the calibration criteria (RSD/r2 and % Error/RSE) are not met." 

Response: 

The Agency agrees with the commenter and made the edit in the text. 

13. Comment: 

Commenter #4 suggested, regarding Method 8000D, Section 11.8.2, that a closing CCV be run 

at the end of a run sequence for both external and internal standard calibrations. The validity of 

a calibration curve should be checked, despite the type of calibration techniques. 

Recommended edit: Change the second to the last sentence to "All samples analyzed should 

be bracketed with a continuing calibration verification (CCV) standard at the beginning and the 

end of the analytical sequence." 

Response: 

The Agency disagrees with the commenter. Section 11.8.2 remains unchanged. 

14. Comment: 

Commenter #4 recommended, regarding Method 8000D, Section 16: Add an additional DoD 

reference document, QSM Version 5.0, which contains updated LCS control limits. Do not 

delete DoD QSM Version 4.2, which has a list of poorly-performing compounds. Recommended 

edit: Add "Department of Defense: "Quality Systems Manual for Environmental Laboratories", 

Version 5.0 http://www.denix.osd.mil/edqw/upload/QSM-Version-5-0-FINAL.pdf." 

Response: 

The Agency agrees and the additional reference was added to Method 8000D in Section 16. 

15. Comment: 

Commenter #4 commented, regarding Method 8000D, Section 9.2.1, that it is generally 

advisable, although not required, that all method QC samples be run at the same time as the 

samples on the same instrument. This should be required, not advisable. Recommended edit: 

Delete the sentence. 
 Page 35 

Response: 

The Agency thanks the commenter for their input, but disagrees with the proposed edit. The 

existing text has been retained. 

16. Comment: 

Commenter #4 commented, regarding Method 8000D, Section 9.2.6.2, that when samples that 

are extracted together are analyzed on separate instruments or in separate analytical shifts, the 

method blank associated with those samples (e.g., extracted with the samples) must be 

analyzed on at least one of those instruments. Recommended edit: "When samples that are 

extracted together are analyzed on separate instruments or in separate analytical shifts, the 

method blank associated with those samples (e.g., extracted with the samples) must be 

analyzed on each of those instruments". 

Response: 

The Agency thanks the commenter for their input, but disagrees with the proposed edit. The 

existing text has been retained. 

17. Comment: 

Commenter #4 commented, regarding Method 8000D, Section 9.4.2, that for those methods 

that apply to a large list of analytes or that contain compounds that may interfere with an 

accurate assessment (i.e., coeluting or multi-peak analytes), a smaller subset of analytes may 

be used. All analytes that are reported to a client should be included in the LCS/MS/MSD. 

Recommended edit: All analytes that are reported to a client should be included in the 

LCS/MS/MSD. 

Response: 

The Agency thanks the commenter for their input. That specification can be included in a 

project QAPP if needed, but will not be required in Method 8000D. Laboratories often include 

samples received from multiple clients in an analytical batch. Analytical requirements including 

but not limited to compound lists will vary by client/project and the LCS/MS/MSD for a client/ 

project-specific target analyte list is not necessarily the same as the one for another client or 

project. Therefore, no change has been made based on the comment. 

18. Comment: 

Commenter #4 commented, regarding Method 8000D, Section 9.7, that the first sentence of the 

first paragraph, "The laboratory shall establish the LLOQ as the lowest point of quantitation, 

which in most cases, is the lowest concentration in the calibration curve", may be misleading. 

The lowest calibration standard does not establish an LLOQ either but it shall be equal to or less 

than the LLOQ to support the LLOQ (i.e., an LLOQ must be within a calibration range for 

reliable quantitation). The first sentence is not clear and should be revised. Recommended 

edit: Change the first sentence to, "The laboratory shall establish its LLOQ as the lowest point of 

quantitation, which shall be within the instrument calibration range. An LLOQ could be equal to 

the lowest calibration standard if the associated data precision and bias at the LLOQ are known 

and documented." 

Response: 

The Agency appreciates the feedback. This change was discussed in the work group and the 

first lines of Section 9.7 were updated to the following: "The LLOQ is the lowest concentration at 

which the laboratory has demonstrated target analytes can be reliably measured and reported 

with a certain degree of confidence, which must be ≥ lowest point in the calibration curve. The 
 Page 36 

laboratory shall establish the LLOQ at concentrations where both quantitative and qualitative 

requirements can consistently be met (see Sections 9.9 and 11.6)." 

19. Comment: 

Commenter #4 commented, regarding Method 8000D, Section 9.7, that the last sentence of the 

first paragraph, "Optimally, the LLOQ should be less than the desired regulatory action levels 

based on the stated DQOs", is not sufficient. EPA needs to provide procedures and/or 

guidance on how to determine the "less" quantitatively. This Section describes many excellent 

concepts and recommendations but lacks detailed procedures for performing them. Without 

procedures, this sentence is troublesome and not very useful. Recommended edit: Suggest 

that EPA provide procedures and/or guidance for establishing quantitative data quality 

requirements on precision, bias, and sensitivity based on project DQOs. It is not appropriate to 

state that this is a project DQO or planning process. 

Response: 

The Agency thanks the commenter for their input, but disagrees that a change is needed. The 

Agency does not currently publish a procedure for determining what the level of the LLOQ (or its 

associated check standard) standard should be. The current practice is to use the bottom point 

of the calibration curve for the determinative method. 

20. Comment: 

Commenter #4 commented, regarding Method 8000D, Section 9.7, that "LLOQ verification is 

recommended for each project application to validate quantitation capability at low analyte 

concentration levels." Recommended edit: The minimum frequency required to verify the LLOQ 

(such as per batch) should be defined. 

Response: 

Frequently performed analyses, such as Methods 8260C and 8270D, should have a LLOQ 

check standard verified, at minimum, once a year. This language was added to Method 8000D 

in Section 9.7.2. 

Comments received on Method 8000D after the public comment period had ended: 

Comment #1a, per the MICE Line, 8000D requirements apply to all previous versions of 

methods. It supersedes 8000C, B, etc. Is this correct and does this logic also apply to the 

updated Chapters? 

Response: 

The Agency thanks the commenter for the question; however, the Agency feels the response to 

the original MICE inquiry may be misinterpreted. Here is the MICE response: 

“As stated in Section 1.1, Method 8000 is not a determinative method but instead provides 

guidance on analytical chromatography and describes calibration and QC requirements 

common to all SW-846 chromatographic methods. However, more specific QC requirements 

provided in the applicable determinative method will supersede those noted in Method 8000. 

Method 8000 should be applied in conjunction with all SW-846 determinative chromatographic 

methods. Method 8000D (the current version in Update V) is a general guidance method for 

organics. As such it includes the most up to date guidance (including revised initial 

demonstration of proficiency (IDP), lower level of quantitation (LLOQ) and relative standard 

error (RSE)) on general chromatography in SW-846. The determinative methods are more 

specific in their requirements for particular analyses (such as 8260B for volatiles) and the 
 Page 37 

determinative method's criteria supersede any general guidance found in 8000D or Chapter 1, if 

specific conflicts exist. Method 8260 has an updated version, 8260C, which is available at: 

http://www.epa.gov/epawaste/hazard/testmethods/pdfs/8260c.pdf. 

The older, published methods (such as 8260B and 8000C) are still valid choices and may still 

be followed by those with a need to do so. We recommend using the newest version of any 

SW-846 method, unless your regulator or customer requires you to use an earlier version.” 

Comment #1b, LLOQ – prepped spike at the LOQ; for Organics under 8000D Section 9.2.1, 

this standard must be analyzed every 12 hours. This requirement adds QC to the analytical run 

which takes away a sample analysis. This will increase cost to the lab in both preparation and 

analytical time as well as the cost of the standard itself and the associated solvents. We would 

suggest that the frequency be changed to analysis per ICAL. 

Response: 

The Agency agrees with the commenter and has removed the LLOQ requirement from Method 

8000D, Section 9.2.1. 

Comment #1c, the method states to spike the LLOQ at the LOQ. We suggest an allowance for 

using a spiking range (<LOQ to 4 X LOQ). To spike at the LOQ would either cause the need to 

analyze multiple standards to encompass the levels or to potentially raise LOQs to match a 

standard. 

Response: 

The Agency appreciates the feedback. The work group discussed this topic and the following 

language was added to Section 9.7.2: "The LLOQ verification (to be performed after the initial 

calibration) is prepared by spiking a clean control material with the analyte(s) of interest at 0.5 - 

2 times the LLOQ concentration level(s). Alternatively, a representative sample matrix free of 

targets may be spiked with the analytes of interest at 0.5 - 2 times the LLOQ concentration 

levels." 

Comment #1d, Inorganics already has the LLOQ requirement under Update IV. With the 

acceptance criteria that need to be met for this standard, the LOQs needed to be raised 2-fold 

under Update IV. This is the same for Update V. 

Response: 

The Agency appreciates the feedback. The work group discussed the LLOQ language and has 

updated Section 9.7. 

 
 Page 38 

METHOD 8021B 

1. Comment: (The Agency received two comments on the same topic for this method. The 

response covers both.) 

Commenter #3 commented, regarding Methods 8021B, 8111, 8270D, 8410, that confusion over 

the appropriate naming convention for bis(2-chloro-1-methylethyl)ether has been a thorny issue 

for years and we appreciate the clarification provided in this update. 

and 

Commenter #9 commented, regarding Methods 8021B, 8111, 8270D, 8410, FR page 63191: 

thanks and congratulates the Agency on the resolution of the bis(2-chloro-1-methylethyl)ether 

naming issue (as requested by the commenter). 

Response: 

The Agency thanks the commenters for their input and is gratified that the clarification provided 

was helpful to the method users. 

 
 Page 39 

METHOD 8111 

1. Comment: (The Agency received two comments on the same topic for this method. The 

response covers both.) 

Commenter #3 commented, regarding Methods 8021B, 8111, 8270D, 8410, that confusion over 

the appropriate naming convention for bis(2-chloro-1-methylethyl)ether has been a thorny issue 

for years and we appreciate the clarification provided in this update. 

and 

Commenter #9 commented, regarding Methods 8021B, 8111, 8270D, 8410, FR page 63191: 

thanks and congratulates the Agency on the resolution of the bis(2-chloro-1-methylethyl)ether 

naming issue (as requested by the commenter). 

Response: 

The Agency thanks the commenters for their input and is gratified that the clarification provided 

was helpful to the method users. 

 
 Page 40 

METHOD 8270D 

1. Comment: (The Agency received two comments on the same topic for this method. The 

response covers both.) 

Commenter #3 commented, regarding Methods 8021B, 8111, 8270D, 8410, that confusion over 

the appropriate naming convention for bis(2-chloro-1-methylethyl)ether has been a thorny issue 

for years and we appreciate the clarification provided in this update. 

and 

Commenter #9 commented, regarding Methods 8021B, 8111, 8270D, 8410, FR page 63191: 

thanks and congratulates the Agency on the resolution of the bis(2-chloro-1-methylethyl)ether 

naming issue (as requested by the commenter). 

Response: 

The Agency thanks the commenters for their input and is gratified that the clarification provided 

was helpful to the method users. 

2. Comment: 

Commenter #4 commented, regarding Method 8270D, Section 11.3.6.3, that "If compounds fail 

to meet these criteria, the associated concentrations may still be determined but they must be 

reported as estimated." This statement appears to allow analytes that fail calibration to be 

reported as estimates. Analytes that fail calibration should not be reported. Recommended 

edit: This statement appears to allow analytes that fail calibration to be reported as estimates. 

Analytes that fail calibration should not be reported. 

Response: 

The Agency thanks the commenter for their input. This comment is valid and this subject will be 

addressed in Method 8270E, which will be released in Update VI. 

 
 Page 41 

METHOD 8290 

1. Comment: 

Commenter #8 commented that the response detailed below provides an alternative to the 

LLOQ concept published in the above-referenced notice regarding an update to SW-486, 

particularly for isotope dilution methods, such as Method 8290. Additionally, the response 

explains both why this approach represents a desirable extension to the LLOQ concept and 

addresses some questions regarding the underlying rationale behind the LLOQ. To be clear, 

SGS approves whole-heartedly of ORCR's decision to remove references to the MDL, for all of 

the reasons that ORCR stated for doing so and many others. SGS also approves of ORCR's 

embrace of EPA's Flexible Approach. SGS supports the aim of the Flexible Approach to permit 

quicker and easier adoption of advancing technology without the time lag inherent in 

promulgation of new methods by the Agency. 

The alternative offered here (commenter submitted a paper in support) is in accord with ORCR's 

obvious interest in improving the quality and interpretation of analytical data. SGS believes that 

this alternative extends upon the concepts underlying the LLOQ, in general, rather than 

negating them. SGS applauds ORCR's clear desire to improve analytical data and offers this 

alternative in that same spirit. 

Response: 

The Agency thanks the commenter for their input. Isotope dilution methods, such as 8290, are 

not in the scope of Update V. An alternative to the LLOQ in a paper provided by SGS will be 

considered when we re-evaluate Method 8290 or other isotope dilution methods. 

 
 Page 42 

METHOD 8410 

1. Comment: (The Agency received two comments on the same topic for this method. The 

response covers both.) 

Commenter #3 commented, regarding Methods 8021B, 8111, 8270D, 8410, that confusion over 

the appropriate naming convention for bis(2-chloro-1-methylethyl)ether has been a thorny issue 

for years and we appreciate the clarification provided in this update. 

and 

Commenter #9 commented, regarding Methods 8021B, 8111, 8270D, 8410, FR page 63191: 

thanks and congratulates the Agency on the resolution of the bis(2-chloro-1-methylethyl)ether 

naming issue (as requested by the commenter). 

Response: 

The Agency thanks the commenters for their input and is gratified that the clarification provided 

was helpful to the method users. 

2. Comment: 

Commenter #4 commented, regarding Method 3200, Section 11.2.1.4, that the section states 

cold sample storage requirements "Store extracts in the cold at 4 °C until analysis". The current 

storage requirements as stated in Chapter 3 are to "store extracts in the cold at ≤6 °C until 

analysis." Recommended edit: Update from old requirements (4 °C) to new requirements (≤6 

°C). 

Response: 

The Agency agrees with the commenter and has made the requested change in Method 3200, 

Section 11.2.1.4. 

The rest of the Update V methods were searched and the same temperature range correction 

was made in Method 8410 (Section 7.4.2) and Method 8430 (Sections 7.5.2, 8.2 and 11.3.4). 

 
 Page 43 

METHOD 8430 

1. Comment: 

Commenter #4 commented, regarding Method 3200, Section 11.2.1.4, that the section states 

cold sample storage requirements "Store extracts in the cold at 4 °C until analysis". The current 

storage requirements as stated in Chapter 3 are to "store extracts in the cold at ≤6 °C until 

analysis." Recommended edit: Update from old requirements (4 °C) to new requirements (≤6 

°C). 

Response: 

The Agency agrees with the commenter and has made the requested change in Method 3200, 

Section 11.2.1.4. 

The rest of the Update V methods were searched and the same temperature range correction 

was made in Method 8410 (Section 7.4.2) and Method 8430 (Sections 7.5.2, 8.2 and 11.3.4). 

 
 Page 44 

METHOD 9014 

1. Comment: 

Commenter #4 commented, regarding Method 9014, that Section 10.1 and 10.2 detail the 

concentrations of the calibration standards, and that the calibration curve is generated by 

plotting absorbance versus concentration, but does not include or reference any acceptance 

criteria for the curve, such as correlation coefficient or coefficient of determination. 

Recommended edit: Add sections specifying the acceptance criteria for calibration curves when 

employing the colorimetric options in this method. 

Response: 

The Agency thanks the commenter for their input. Detailed information on calibration models 

and their acceptance criteria is not included in each SW-846 method. The methods are 

intended as general guidance. For any test methods which are not method-defined parameters 

(MDPs), the intention is to allow the laboratory flexibility under the Methods Innovation Rule 

(MIR). The details of how a laboratory will conduct and approve calibrations should be included 

in the individual laboratory's QMP and in their SOPs for each method. SW-846 method limits 

are not intended to be mandatory QC acceptance criteria. 

 
 Page 45 

METHOD 9040 

1. Comment: 

Commenter #1 commented, regarding Method 9040, that Method 9040, which is specified in 40 

CFR 261.22(a)(1) as the analytical method to be used for establishing the pH of an aqueous 

waste, states that this "method is used to measure the pH of aqueous wastes and those 

multiphase wastes where the aqueous phase constitutes at least 20% of the total volume of the 

waste." 

This statement in 9040 is being used by the regulated community to assert, for example, that a 

55-gallon drum full of strong sodium hydroxide liquid and steel pieces is not a D002 hazardous 

waste if the volume of liquid is less than 11 gallons (55 x 0.20 = 11). Such a waste would phase 

separate, with the sodium hydroxide liquid on top at a depth of up to 6 inches (6 inches is 20% 

of 30 inches, the approximate height of a 55-gal drum). Clearly a pH could be easily obtained 

with 6 inches of depth to insert a pH meter's probe into, and hence such a drum-full of waste 

should clearly be classified as a D002. 

This statement in method 9040 should be changed in Update V to make it clear that, depending 

on the sample, 9040 may still be suitable for D002 determinations even if the aqueous phase 

constitutes less than 20% of the entire waste. Incidentally, at least one EPA guidance 

document, RO# 11738, erroneously concludes from the above sentence in 9040 that "any 

waste for which [9040] is applicable must contain at least 20% free water by volume." 

Response: 

The Agency thanks the commenter for their input. Method 9040 is a method-defined parameter 

(MDP) and as such would have to be revised by a formal rulemaking. Method 9040 is not 

included in Update V and as such, is not subject to revision at this time. The Agency will retain 

the comment to be discussed the next time Method 9040 is updated. 

 
 Page 46 

REFERENCE TABLE 

1. Comment: 

Commenter #1 commented, regarding the Reference Table, that one of the documents in the 

Docket (i.e., EPA-HQ-RCRA-2012-0072-0023) has a faulty link for the following entry: "USEPA. 

Waste Analysis at Facilities That Generate, Treat, Store and Dispose of Hazardous Wastes, 

ECDIC 2002-011. Office of Waste Programs Enforcement, United States Environmental 

Protection Agency. April 1994". The faulty link is: 

http://www.epa.gov/compliance/resources/policies/civil/rcra/wasteanalygman-rpt.pdf. 

This link produces an error message. This "waste analysis" document – which is the April 1994 

version and not the draft January 2013 version – is believed to instead be at: 

http://www.epa.gov/osw/hazard/tsd/ldr/wap330.pdf. 

Readers attempting to use the faulty link may, after receiving the error message that this link 

does not exist, do a "Google search" for this document and are likely to select the January 2013 

version of this document. However, the January 2013 version is only a draft (and was reported 

in comments to have a number of errors). 

Response: 

The Agency agrees with the commenter that the displayed link is not functioning at this time. A 

link to the 2013 guidance can be found at: http://www.epa.gov/epawaste/hazard/tsd/permit/tsdregs/tsdf-wap-guide.pdf. 

 
 Page 47 

GENERAL COMMENTS 

1. Comment: 

Commenter #3 commented that they welcomed the opportunity to comment on Update V to 

SW-846. They believe this update considerably strengthens and clarifies the guidance 

provided, and appreciate the work the agency continues to put into improving the manual. 

The clarifications to status of methods and especially the strong guidance to prefer the latest 

version of a method are useful and should improve the consistency with which methods are 

selected by the data users and generators. 

Response: 

The Agency thanks the commenter for their input and is gratified that the clarification provided 

was helpful to the method users.

2. Comment: 

Commenter #9 commented regarding FR Pages 63187 and 63188: The commenter thanks and 

congratulates the Agency on the clarifications to the status of SW-846 methods, naming 

conventions and the strong statement regarding preference for using the latest method version 

(as previously requested by commenter). 

Response: 

The Agency thanks the commenter for their input and is gratified that the clarification provided 

was helpful to the method users.

3. Comment: 

Commenter #9 commented regarding FR Pages 63191 and 63192: The commenter approves of 

the addition of a formal quantitation limit termed the LLOQ. 

Response: 

The Agency thanks the commenter for their input.

4. Comment: 

Commenter #9 commented regarding FR Pages 63191 and 63192: The commenter recognizes 

that the current MDL procedure does not meet ORCR needs, but the commenter believes that 

the Office of Water is considering an update to the MDL, in which case ORCR may want to 

reconsider its position at some time in the future because the LLOQ would be more effective in 

combination with a reliable detection limit. 

Response: 

The Agency thanks the commenter for their input and will review any new policies published for 

relevance and possible use by ORCR in future updates.

5. Comment: 

Commenter #9 commented regarding FR Page 63191: Regarding the elimination of the use of 

the current MDL, the commenter agrees with ORCR that the MDL in its current form has no 

place in the program. However, should The NELAC Institute's proposed revisions to the MDL 

be accepted, the MDL could be valuable for making the determination that a waste is 

nonhazardous for a given constituent if that constituent is not detected and the MDL is less than 

the RCRA limit. The only caveat is that it is necessary to be certain that the MDL is appropriate 

for the specific matrix to which it is being applied. This may mean that the generator would 

have to demonstrate that the MDL can be verified in its specific matrix. 
 Page 48 

Response: 

The Agency thanks the commenter for their input and will review any new published standards 

for relevance and possible use by ORCR in future updates.

6. Comment: 

Commenter #9 commented regarding FR Page 63192: The commenter approves of the 

changes to the Initial Demonstration of Proficiency requirements. 

Response: 

The Agency thanks the commenter for their input.

7. Comment: 

Commenter #9 commented (FR Pages 63192 and 63193): The commenter approves of the 

addition of the relative standard error as a method for evaluation of calibration curves and 

appreciates the consistency with similar approval in 40 CFR Part 136. 

Response: 

The Agency thanks the commenter for their input.

8. Comment: 

Commenter #4 commented that the chapters refer to the methods for details and guidance on 

establishing and verifying the LLOQs, but little guidance can be found in the methods. 

Recommended edit: Clarify details on establishing and verifying the LLOQs, and clarify the 

location of the guidance both within the chapters and the methods. 

Response: 

Guidance on LLOQ verifications can be found in Methods 6010D and 6020B (Section 9.8 for 

both) for inorganics as well as Method 8000D (Section 9.7) for organics. 

9. Comment: 

Commenter #4 commented that the LLOQ requires quarterly verification, but it is unclear exactly 

how the verification is performed. Recommended edit: Clearly define how the LLOQ verification 

should be performed. 

Response: 

The determinative methods may specify how often a particular method's LLOQ verification 

should be performed. For inorganic methods (such as 6010B and 6020B) the requirement is a 

minimum of quarterly. For organic methods, 8000D specifies the following in Section 9.7.2: "It is 

recommended to analyze the LLOQ verification on every instrument where data is reported; 

however, at a minimum, the lab should rotate the verification among similar analytical 

instruments such that all are included within 3 years. Frequently performed analyses, such as 

Methods 8260C and 8270D, should have an LLOQ check standard be verified, at minimum, 

once a year." 

10. Comment: 

Commenter #4 commented that the guidance is unclear on the topic of how many different 

matrices the LLOQ should be determined for and how to mimic the matrix in the LLOQ 

determination. Clarify how the laboratory should mimic the matrix for the LLOQ determination. 
 Page 49 

Response: 

LLOQ can be determined using either clean control material (e.g., reagent water, solvent blank, 

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 DQOs. For a specific project with established DQOs, a representative 

sample, free of target compounds, may be used to provide a more reliable estimate of the lower 

quantitation limit capabilities. For more information, please see Section 9 of Method 8000D. 

11. Comment: 

Commenter #4 commented that no guidance is presented on spiking level. It states the LLOQ 

should be the lowest calibration concentration, but spiking at that level with recoveries less than 

100% would require calculating data below the curve which is not acceptable now unless 

qualified. So should the spike level be 35% higher than the lower calibration standard? This 

way any result below the lowest calibration standard would be not acceptable. Also they refer to 

making sure the LLOQ is below the regulatory limits. These limits for the samples the lab 

receives are not usually known and also vary by state etc. Insert guidance on the spiking 

concentrations for LLOQs. 

Response: 

The Agency thanks the commenter for their input. The LLOQ is prepared by spiking the 

analyte(s) of interest at 0.5 - 2 times the LLOQ concentration level(s) per Method 8000D and <2 

times the LLOQ for inorganic methods. The LLOQ check is carried through the same 

preparation procedures as environmental samples and other QC samples. Recovery of target 

analytes in the LLOQ verification should be within established in-house limits, or other such 

project-specific acceptance limits, to demonstrate acceptable method performance at the LLOQ. 

The laboratory would need to verify with data user(s) and/or regulatory authority to ensure 

project DQOs (including RLs) are appropriate prior to conducting the analysis. 

12. Comment: (The Agency received several comments regarding LLOQ and MDL. They 

are combined for the response.) 

Commenter #4 commented that various environmental applications (risk assessment, statistical 

evaluations, etc.) that utilize SW-846 methods rely heavily on the use of "detected" data. 

Elimination of the MDL without further clarification on issues regarding reporting and use of data 

below the LLOQ will lead to confusion. Further guidance is needed. Recommended edit: 

Clarify how to report and use data below the LLOQ. 

and 

Commenter #5 commented that the proposed change to SW-846 that would eliminate the MDL 

and substitute a new parameter called the LLOQ. This change removes information from the 

test report that is very helpful to state environmental agencies responsible for evaluating and 

remediating public health risks associated with hazardous substance discharges. Currently, 

detections below the RL and above the MDL are stated and qualified with a J flag. This means 

that the chemical is in the sample but can't be quantified well enough to make the quantity 

measurement usable. However there is a 90% certainty that the chemical is in the sample. It is 

very important to know if a specific chemical is in the sample, even though one doesn't know 

how much there is. The reasons are several: 

1. Some health standards are below RLs. If it is reported with a J flag that a chemical of 

concern with a health standard below the RL is in the sample then the professional evaluating 

the contamination site knows that there is a potential health impact that must be searched out 
 Page 50 

by some other means of investigation. If the chemical of concern is present at concentrations 

lower than the LLOQ, then it would go unnoticed under this proposed change to the method, 

leaving the possibility that the health of people living on or near this site may be threatened. 

2. In most cases the health standard is above a RL. In these instances it is also helpful to have 

a chemical of concern J flagged. For example, if the substance is the target of a monitoring 

system and it has been identified by a J flag, remediation professionals would continue 

monitoring for the chemical to see if it will increase to the point where it may exceed the health 

standard. If this change in the method were adopted the professionals would not see the 

chemical of concern reported and would discontinue monitoring for this chemical. This could 

cause them to miss the potential situation where, with time, it increased in value above the 

health standard. This mistake could put someone's health at risk that might be living at or near 

the site. 

and 

Commenter #6 commented that according to update V, both the MDL procedure and the LLOQ 

procedure may be performed using a clean matrix or control material. It is our opinion that the 

LLOQ procedure is not more representative of complex matrices. We understand that the 

LLOQ procedure may be performed using a representative sample matrix free of target 

compounds, but given the option it is likely that the laboratories will opt to use a clean control 

material (e.g., reagent water, method blanks, Ottawa sand, diatomaceous earth, etc.). 

The quotes below taken directly from the Federal Register notice of availability support our 

opinion: 

The procedure outlined in Part 136 is generally not suitable for RCRA wastes or materials 

because the MDL approach generally yields unrealistic and/or unachievable method detection 

limits for the complex matrices (e.g., soils, sludges, wipes, and spent materials) encountered 

under the RCRA program. The MDLs are normally calculated from analysis of a sample that 

does not cause matrix interferences (typically determined using spiked reagent water). 

Establishing 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. 

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. 

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. 

Response: 

ORCR understands that other EPA programs may continue to use MDLs to meet their program 

use and needs (e.g., the National Pollutant Discharge Elimination System (NPDES) permit 

program). However, ORCR has found that the procedure in 40 CFR 136, Appendix B, for the 

determination of MDLs, developed for the Clean Water Act (CWA) program, uses a clean matrix 

(e.g., reagent water for preparing "spiked" samples, or samples with known constituent 

concentrations). Analytical laboratories often have difficulty demonstrating they can meet the 

MDL established using Part 136 when evaluating complex matrices, such as wastes. The 

procedure outlined in Part 136 is generally not suitable for RCRA wastes or materials because 

the MDL approach generally yields unrealistic and/or unachievable MDLs for the complex 
 Page 51 

matrices (e.g., soils, sludges, wipes, and spent materials) encountered under the RCRA 

program. The MDLs are normally calculated from analysis of a sample that does not cause 

matrix interferences (typically determined using spiked reagent water). However, most wastes 

evaluated for compliance with RCRA consist of complex matrices. The LLOQ considers the 

effect of sample matrix (e.g., components of a sample other than the analyte) by taking the 

sample through the entire analytical process, including sample preparation, clean up (to remove 

sample interferences), and determinative procedures. If a laboratory has a need to report a 

value that is at or above the MDL, but lower than the LLOQ, it may do so with qualification, such 

as a flag of "J" to represent that the value is a qualitative positive hit but is not considered to be

quantitatively accurate. Other forms of qualifications may also be used as long as they meet the 

projects DQO and/or any other regulatory requirements.