Response to Comments Document 

for

 

Methods Update Rule Proposal (75 FR 58024; September 23, 2010) 

March 2012 
2010 Methods Update Rule Response to Comments i March 2012 

Foreword

This document contains EPA’s responses to public comments received in response to the Methods Update 

Rule Proposal (75 FR 58024; September 23, 2010). 

A number of changes to the final rule are being made that were not in the proposal. These changes are 

being made for a number of reasons such as typographical errors inadvertent omissions, and new 

requirements for incorporation by reference by the Office of the Federal Register. These changes are 

addressed in a separate memo to the docket. 

EPA is deferring action on the approval of several methods in the original proposal, most notably EPA 

Method 1668C, which was the subject of extensive comments. Therefore, this document does not contain 

responses to comments regarding Method 1668C. At such time as EPA makes a final determination on 

Method 1668C, the Agency will formally document its responses to all the comments received. 

This document also does not contain responses to comments received about ASTM Method D7575-10, a 

solid-phase extraction procedure for “oil and grease” developed by Orion Spectral Solutions. EPA did 

not propose this ASTM method as part of the Methods Update Rule proposal cited above. A number of 

detailed comments were received on this method. These comments were addressed in a Notice of Data 

Availability (NODA) that has been published prior to today's final ruling and are not addressed here. EPA 

refers readers to a December 14, 2011 Federal Register notice (76 FR 77742) for additional information 

on this ASTM method.

The remainder of this document mirrors that of the proposal, in which Section II laid out the proposed 

changes in 13 subsections (A through M), many of which were further divided into as many as two more 

levels (e.g., II.A.3.f). In each section of this document, the commenters responding to a specific topic are 

identified by comment number, name, and affiliation. That list of comments is followed by a broad 

summary of the comments received. EPA provides one response below the summary. Following EPA’s 

response are the original comments, as received by the EPA Docket website. Some comments have been 

aggregated as follows: comments supporting the addition of a method, and comments that are nearly or 

completely identical. In a few instances where a commenter submitted lengthy supporting information or 

other documents, EPA did not include all such supporting information in this document and notes that 

fact at the end of each such comment. 
2010 Methods Update Rule Response to Comments ii March 2012 

Table of Contents 

Section II.A New EPA Methods and New Versions of Previously Approved EPA Methods .................. 1 

II.A.1 Method 1664B and amending the RCRA regulations at 40 CFR 260.11 to include the revised 

Method 1664B ................................................................................................................................... 4 

II.A.2 Method 200.5; clarify axial orientation of the torch is allowed for use with EPA Method 200.7 ..... 6

II.A.3 Method 525.2 ..................................................................................................................................... 11

II.A.3.a Method 608.1 .................................................................................................................................. 13 

II.A.3.b Method 608.2 .................................................................................................................................. 14 

II.A.3.c Method 614 ..................................................................................................................................... 15 

II.A.3.d Method 614.1 .................................................................................................................................. 16 

II.A.3.e Method 615 ..................................................................................................................................... 17 

II.A.3.f Method 617 ..................................................................................................................................... 18 

II.A.3.g Method 619 ..................................................................................................................................... 21 

II.A.3.h Method 622 ..................................................................................................................................... 21 

II.A.3.i Method 622.1 .................................................................................................................................. 21 

II.A.3.j Method 63 ....................................................................................................................................... 22 

II.A.4 Method 1614A .................................................................................................................................... 23 

II.A.5 Method 1668C .................................................................................................................................... 24 

II.A.6 Methods 1622 and 1623 ..................................................................................................................... 24

II.A.7 Bacteriological Methods ..................................................................................................................... 24

II.A.8 Method 1627 ....................................................................................................................................... 25

II.A.9 EPA Method 624 for Quantitation of Acrolein and Acrylonitrile ...................................................... 25

Section II.B New Standard Methods and New Versions of Approved Standard Methods ........................... 29 

II.B.1 General Support ................................................................................................................................. 29 

II.B.2 Cost .................................................................................................................................................... 30 

II.B.3 Version Confusion ............................................................................................................................. 35 

II.B.4 Default Approval Concerns ............................................................................................................... 40 

II.B.5 Quality Assurance/Quality Control (QA/QC) ................................................................................... 43 

II.B.6 Alternate Test Procedures (ATPs) ..................................................................................................... 46 

II.B.7 Biosolids Rule .................................................................................................................................... 49 

II.B.8 Implementation Issues ....................................................................................................................... 50 

II.B.9 Method-specific Issues ...................................................................................................................... 54 

II.B.10 Other Comments ................................................................................................................................ 58 

Section II.C New ASTM Methods and New Versions of Approved ASTM Methods ................................. 59 

II.C.1 ASTM D2036-09 ............................................................................................................................... 62 

II.C.2 ASTM D6888-09 ............................................................................................................................... 62 

II.C.3 ASTM D7284-08 ............................................................................................................................... 62 

II.C.4 ASTM D7511-09e2 ........................................................................................................................... 62 

II.C.5 Add free cyanide in Table IB and allow use of Method OIA 1677-09 and ASTM Methods 

 D4282-02 and D7237-10 ................................................................................................................... 62 

II.C.6 ASTM D888-09 ................................................................................................................................. 64 

II.C.7 ASTM D7573-09 ............................................................................................................................... 65 

II.C.8 ASTM D7065-06 ............................................................................................................................... 65 

II.C.9 ASTM D7574-09 ............................................................................................................................... 69 

II.C.10 ASTM D7485-09 ............................................................................................................................... 70 

II.C.11 Do not add ASTM D7066-04 or ASTM D7575-10 in Table IB........................................................ 71 

Section II.D Alternate Test Procedures (ATPs) ........................................................................................... 72 
2010 Methods Update Rule Response to Comments iii March 2012 

II.D.1 Hach Method 10360 .......................................................................................................................... 75

II.D.2 In-Situ Incorporated’s Method 1002-8-2009 ..................................................................................... 76

II.D.3 In-Situ Incorporated’s Method 1003-8-2009 ..................................................................................... 76

II.D.4 In-Situ Incorporated’s Method 1004-8-2009 ..................................................................................... 76

II.D.5 Mitchell Method M5271.................................................................................................................... 76

II.D.6 Mitchell Method M5331.................................................................................................................... 76

Section II.E Clarifications and Corrections to Previously Approved Methods ............................................ 77 

II.E.1 Immediate Filtration of Samples for Orthophosphate ........................................................................ 77 

II.E.2 Correct missing citations for microbial methods applicable to ambient water monitoring ............... 84 

Section II.F Changes to Required Containers, Preservation Techniques, and Holding Times in 

 Table II ...................................................................................................................................... 85 

II.F.1 Table II takes precedence over other instructions, unless approved by permitting authority ............ 86 

II.F.2 E. coli and Enterococcus Holding Times ........................................................................................... 90 

II.F.3 Revising cyanide sample handling instructions in Footnote 5 to Table II ......................................... 92 

II.F.4 Revising Cyanide Sample Handling Instructions in Footnote 6 to Table II ...................................... 95 

II.F.5 Revise Footnote for Handling WET samples ..................................................................................... 97 

II.F.6 Clarify the Holding Time for WET samples ...................................................................................... 97 

Section II.G Proposed Revisions to 40 CFR 136.4 and 136.5 ..................................................................... 98 

Section II.H Revisions to Method Modification Provisions at 40 CFR 136.6 ............................................. 100 

II.H.1 General Comments ............................................................................................................................ 100 

II.H.2 Use of Relative Standard Error (RSE) to Evaluate Calibrations ....................................................... 103 

II.H.3 Adding Other Analytes to Existing Methods .................................................................................... 106 

II.H.4 Changes to Method-defined Parameters ............................................................................................ 109 

II.H.5 Metals Digestion Changes ................................................................................................................. 110 

II.H.6 Use of Selected Ion Monitoring (SIM) .............................................................................................. 111 

II.H.7 Holding Times and Preservation Change .......................................................................................... 113 

II.H.8 Calibration Models ............................................................................................................................ 113 

II.H.9 Gas Diffusion .................................................................................................................................... 115 

II.H.10 Collision Cell for ICP/MS ................................................................................................................. 116 

II.H.11 Other Comments ................................................................................................................................ 117 

Section II.I Proposed New QA/QC Language at 40 CFR 136.7 ................................................................. 122 

Section II.J Withdrawal of the Appendices ................................................................................................ 152 

Section II.K Proposed Revisions to 40 CFR 423 ......................................................................................... 154 

Section II.L Proposed Revisions to 40 CFR 430 ......................................................................................... 155 

Section II.M Proposed Revisions to 40 CFR 435 ......................................................................................... 155 
2010 Methods Update Rule Response to Comments 1 March 2012 

Section II.A New EPA Methods and New Versions of Previously Approved EPA Methods 

List of Comments: 

Comment 106.1 - Charles Boepple, Upper Occoquan Service Authority 

Comment 109.1 - Andre Brousseau, Maine Wastewater Control Association 

Comment 116.1 - Wendy Harding and Mala Burton, Joint Virginia Water Environment Association and 

Virginia American Water Works Association 

Comment 166.1 - Paul Wiegand, National Council for Air and Stream Improvement, Inc. 

Comment 187 - Peter Halpin, Caltest Analytical Laboratory 

Summary of Comments: EPA proposed to approve a number of new EPA methods and new versions of 

previously approved methods. EPA received comments regarding the method approval or withdrawal 

process as it applies to EPA methods, methods developed by voluntary consensus standard bodies and 

alternate test procedures (ATPs). One commenter questioned why vendor methods based on older 

disapproved methods were still approved. Other comments addressed the need for accessibility of all 

approved methods at federal repositories, and the need to expand the scope of the 600-Series of methods 

to include additional compounds and detectors to correlate with the 8000-Series methods. One 

commenter stated that EPA is required to publish all validation data as part of an ATP petition to but did 

not provide all validation data for certain EPA methods (e.g., Methods 632, 1614A). 

Response: In cases where EPA has approved newer versions of previously approved methods, the newer 

versions are equivalent to the older versions. As stated in the preamble to the proposed rule, the newer 

versions of these methods have been approved in an attempt to reduce inconsistencies in quality 

assurance/quality control (QA/QC) practices across laboratories. Alternate Test Procedures (ATPs) that 

were based on the older procedures are not being withdrawn because the approved ATPs refer to current 

versions of Part 136 methods which have adequate QA/QC procedures. Older methods were withdrawn 

either because a procedural change was made that affected method performance, or because QA/QC 

procedures were missing, not because of any technical deficiencies. 

EPA is not required to make all currently approved methods available for view and use at “federal 

repositories.” Methods developed by EPA are available through several sources, including on the EPA 

web-site at: http://water.epa.gov/scitech/methods/cwa/index.cfm. Methods developed by outside 

organizations such as voluntary consensus standard bodies (VCSBs) are, in most cases, copyrighted 

materials and EPA does not have the authority to make them publicly available. They are generally 

available at the organization’s web-site for a fee. 

Expanding the scope of the 600-Series methods developed for use in water monitoring programs to 

include compounds in the 8000-Series, which were developed for use in the solid waste monitoring 

program, or revising 600-Series methods (e.g., Methods 608 or 614) to include use of a quadrapole mass 

spectrometer as a primary detector, is outside of the scope of the proposed rule. 

There is no requirement at §136.5 for EPA to publish all validation data submitted as part of an ATP 

application. EPA makes data regarding method performance available when proposing new methods for 

the analysis of pollutants to allow the public to comment on the proposed approval of these methods. In 

cases where updated versions of previously approved methods are added, no new validation data are 

required, because the changes are editorial and do not affect method performance. This is true for many 

of the voluntary consensus standards bodies (VCSBs) methods being approved in today’s rule as well as 

for EPA Method 1664B. In the cases of EPA Methods 614, 619, 622.1, and 632, EPA added these 

methods (previously included for Pesticide Active Ingredients in Table IG) to Table ID for general use. 

As stated in the preamble to the proposed rule, these methods have been in use for more than a decade 

and are being added to Table ID to allow for an increased number of options when permittees are required 

to monitor for these compounds. 
2010 Methods Update Rule Response to Comments 2 March 2012 

In the case of EPA Method 1614A, EPA is not adding this method to Part 136 until more extensive 

validation of the method has been completed. After review of the comments and further evaluation of the 

record, EPA concluded that additional validation data are needed to fully characterize the performance of 

this method for various wastewater matrices. 

EPA appreciates the commenters’ concern that consensus methods should be subjected to the same 

validation required for nationwide approval of alternate test procedures and will work with the VCSBs to 

ensure that method validation data for new consensus methods is made available for public comment. 

Original Comment Text: 

Comment 106.1 

Charles Boepple 

Upper Occoquan Service Authority 

Comment 3: If commercially available methods approved under EPA's ATP program and based on older 

methods are still approved, then why are those same older methods no longer allowed for use by 

laboratories? 

Recommendation 3: Please provide justification for what appears to be a contradictory method 

requirement imposed on the laboratory community. 

Comment 5: Why were some methods or versions withdrawn and not others? Was it a change in the 

method per se or a change in method QC? 

Recommendation 5: Please provide the criteria EPA follows for evaluating and eliminating methods. 

Comment 109.1 

Andre Brousseau 

Maine Wastewater Control Association 

MWWCA believes that the listing of EPA's currently approved and required methods must be available 

for view and use at federal repositories, and that only tangible documents should be allowed for this 

purpose. How will the EPA assure that the most current version of an EPA required testing method or 

prescribed quality control and assurance step be available for view and use at federal repositories? 

Comment 116.1 

Wendy Harding and Mala Burton 

Joint Virginia Water Environment Association and Virginia American Water Works Association 

Comment: Expand the 600 series list of organic method compounds to correlate with 8000 series. Current 

examples include xylene, MIBK, MEK, and 1, 2 diphenylhydrazine which are required for NPDES 

program monitoring and are listed under 8000 series but not the 600 series. Since these compounds are 

not listed in the 600 series, there is not an approved method for NPDES monitoring. Laboratories must 

use separate, non-approved methods. 

Recommendation: Several EPA 600 and 8000 series methods have long been known to be similar in 

application such as EPA methods 624 and 8260B, 625 and 8270D, 608 and 8081B. Considering 

equivalency of these methods, the scope of the 600 series list of organic analytes should be expanded to 

include the compounds in the 8000 series methods, provided that the QA/QC requirements of the more 

stringent methods are met. Monitoring requirements that allow only the use of 40CFR sanctioned 

methods now includes some analytes that are not covered by the 600 series methods but are included in 
2010 Methods Update Rule Response to Comments 3 March 2012 

the similar 8000 series methods. Allowing expanding the scope of the 600 series methods will provide 

more flexibility for permittee to meet monitoring requirement using EPA sanctioned and approved 

methods. 

Comment 166.1 

Paul Wiegand 

National Council for Air and Stream Improvement, Inc. 

EPA is required under §136.5 to publish all validation data submitted as part of an ATP petition, and to 

then solicit public comment on approval of the proposed method; this is something that EPA has not done 

as part of this proposal. 

1. Proposed Addition of Analytical Methods for Which Validation Data are not Provided [Sections A, B 

and C, pp. FR 58026 – 58031] 

EPA is proposing adoption of a number of methods without providing any data showing that these 

methods will perform as required on the types of wastewaters regulated in the NPDES program. Methods 

adopted by EPA should be subject to the same level of validation required in the Alternate Test Procedure 

Program. 

It is understood that EPA proposes addition of numerous methods that were developed by voluntary 

consensus organizations (e.g., ASTM and Standard Methods) under the authority and requirements of the 

National Technology Transfer Act. The Act requires EPA to adopt all suitable methods developed by 

consensus organizations but does not release EPA from the responsibility of determining that the 

consensus methods meet the testing requirements under 304(h) of the Clean Water Act. If EPA evaluates 

a candidate consensus method and finds that it does not meet the performance requirements required for 

NPDES permit application and compliance testing, it is not obligated to adopt the method and need only 

communicate the basis for that decision to the Office of Budget and Management annually. 

In the current proposal, EPA has not provided any data that verify that the proposed consensus methods 

perform as required on the types of wastewaters regulated in the NPDES program. If a regulated entity or 

other interested organization (e.g., an instrument manufacturer) requests approval for the use of an 

alternate test procedure, EPA has established strict validation requirements that must be met before an 

approval can be granted. EPA currently proposes to fully incorporate methods that have previously been 

approved for nationwide use, and in so doing has effectively set a minimum method validation 

requirement. Thus EPA has failed to apply the same level of validation required in its own Alternate Test 

Procedure Program to the consensus methods. EPA should provide its rationale and make available the 

related data used for determining that these methods meet the required performance criteria and/or subject 

them to the same level of validation required in the ATP program. Those data should be noticed for 

public review and comment before incorporating a consensus method into 40 CFR Part 136. 

Similarly, EPA proposes addition of several EPA methods (e.g., 1614A, 614.1, 632, 1664 Rev. B, 622.1, 

and 619) but has not provided any validation data demonstrating the capabilities of the methods to meet 

the testing requirements for the NPDES program, nor has it conducted a peer review and made the result 

available for public comment. As noted separately for evaluation of consensus methods, at a minimum 

EPA should subject these methods to the same validation that it requires for nationwide approval of an 

alternate test procedure. Until that minimal validation is completed and made available for public 

comment, EPA should not add these methods to 40 CFR Part 136. 

Comment 187 

Peter Halpin 

Caltest Analytical Laboratory 
2010 Methods Update Rule Response to Comments 4 March 2012 

With regard to use of mass spectrometers, the methods in the CWA, and those proposed to go into general 

use are inconsistent in the language used regarding mass spectrometry. It would be helpful to allow the 

use of mass spectrometers as primary detectors when the performance of the instrument is sufficient for 

the analyte in question. Currently most method references to mass spectrometers assume the use of mass 

spectrometry for confirmation when sensitivity allows. Current mass spectrometers are capable of 

quantitation at the ML of most semivolatile methods, making them useful as the primary detector for both 

identification of analyte and quantitation as well. A similar recognition seems to be involved in moving 

Acrolein and Acrylonitrile to mass spectrometry in EPA Method 624 as a definitive analysis, and not just 

a screening analysis. Our comments on mass spectrometry are not meant to suggest combining all 

possible analytes into the already large list of analytes by EPA Methods 624 and 625, but to use pesticide 

methods like EPA Methods 608 or 614 with the primary detector being a quadrapole mass spectrometer 

as opposed to an ECD, or NPD system. The current proposed update includes language related to Selected 

Ion Monitoring, which is useful. To bring the CWA methods up to current technology it would be 

valuable to address the use of chemical ionization and multiple reaction modes (‘triple quad’ for example) 

as well. 

II.A.1 Method 1664B and amending the RCRA regulations at 40 CFR 260.11 to include the 

revised Method 1664B 

List of Comments: 

Comment 109.1 - Andre Brousseau, Maine Wastewater Control Association 

Comment 112.1 - Colin Elliott, King County Environmental Lab

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Summary of Comments: EPA proposed a new version of EPA Method 1664 Revision B (1664B) for 

use in CWA programs. Two commenters supported the approval of Method 1664B, however, one 

commenter suggested that wording in the method allowing the ability to delay preservation of the sample 

for up to four hours be removed because Table II does not include this holding time allowance. The other 

commenter suggested that the agency should consider allowing the use of both Method 1664A and 

Method 1664B during a specified transition time. One commenter thought the inclusion of allowed and 

prohibited modifications was helpful and agreed with most of the specifics with the exception of two of 

them. The exceptions cited were that the practice of blank subtraction is inappropriate when testing any 

volume of sample (section 1.7.1.5), and that the allowance to do alternate balance calibration checks is 

too vague. Two commenters expressed a desire for EPA to approve new methods for measurement of oil 

and grease that do not rely on the use of n-hexane as the extraction solvent and one of them recommended 

that EPA re-write its current definition of oil and grease so new technologies can be approved. 

Response: EPA is aware of the potential issues associated with n-hexane and addressed them in the 

method. Regarding comments that EPA revise the definition of “oil and grease” to divorce the term from 

the use of a specific solvent, EPA understands the concern, but at present, “oil and grease” remains a 

method-defined parameter, and changing the definition is beyond the scope of today’s rule. Moreover, 

based on EPA’s substantial studies of this parameter that lead to the promulgation of Method 1664A, the 

current definition and solvent, as specified in Method 1664 measure the petroleum, animal or vegetable 

oils and greases of concern to the commenter. In response to commenters expressing the desire to use 

non-hexane methods, EPA recently published a notice of data availability (NODA) requesting comment 

on a new method for the measurement of oil and grease that does not rely on the use of n-hexane as the 

extraction solvent (see 76 FR 77742, December 14, 2011). The Agency will make a decision on this new 

method at a later date. 
2010 Methods Update Rule Response to Comments 5 March 2012 

Regarding the practice of blank subtraction in Sec. 1.7.1.5 of the method, blank subtraction has 

traditionally been an integral part of all EPA gravimetric methods for oil and grease and EPA has not 

identified any issues that would require a change. Thus, EPA is not revising the proposed method in 

response to the blank subtraction comments. 

Regarding the allowance for changes to the balance calibration checks, EPA disagrees that the proposed 

text in the method is vague. EPA’s intent, as indicated by the text in Sec. 1.7.1.6 of the proposed method, 

is to allow the laboratory to calibrate their balance with additional weights, such that their calibration 

range is wider than that described in the method. This allowance would reduce the instances where 

samples that were heavily laden with oil and grease would need to be diluted and reanalyzed, or could 

allow the laboratory to report results to lower levels, based on demonstrating a wider calibration range for 

the balance. 

However, EPA recognizes that Sec. 1.7.1.6 also refers to changes to the balance calibration frequency in 

Sec. 10 of the method, and notes that Sec. 10 does not provide a frequency for the balance calibration. 

Therefore, EPA has revised the text of Sec 1.7.1.6 of the proposed method to read as follows: 

1.7.1.6 Balances may be calibrated with an additional upper class “S” weight and/or a lower 

weight in order to bracket the expected final weighing value. In addition, in situations where more 

than 20 samples are analyzed per day, the frequency of balance calibration in Section 9.5 may be 

reduced to once at the beginning and once at end of each day. 

Regarding the sample preservation, EPA has clarified in Section 8.1.1 of the method that if the analysis is 

to be delayed by more than four hours, the pH must be adjusted to less than 2 with HCl or H2SO4 solution 

and the sample must be refrigerated at 0-6 oC. 

Original Comment Text: 

Comment 109.1 

Andre Brousseau 

Maine Wastewater Control Association 

EPA seeks to approve new technologies for other test parameters as part of its changes to 40 CFR 136, yet 

falls short of being able to accept new methods that include new technologies for Oil & Grease. 

MWWCA finds that the EPA's reasoning for not approving alternative test methods for Oil & Grease is 

contradictory to the Agency's "Summary" statement that these regulations will "provide increased 

flexibility to the regulated community and laboratories in their selection of analytical methods (test 

procedures) for use in Clean Water Act programs." Further, approving the new methods would be more 

consistent with the EPA's mission and purpose to "ensure that all Americans are protected from 

significant risks to human health and the environment where they live learn and work." 

EPA has previously approved hexane extractable methods for Oil & Grease, then reversed that decision 

because hexane was a hazardous solvent and required use of Freon-extractable methods for Oil & Grease. 

Then EPA reversed that decision and went back to hexane, because Freon was considered more harmful 

to human health and the environment than hexane. However, hexane remains a dangerous solvent. nHexane has a flashpoint of 22 degrees Celsius, so most n-hexane waste is considered a RCRA hazardous 

waste by characteristic. According to the U.S. Department of Labor, Occupational Safety and Health 

Administration (OSHA) Guideline for n-Hexane (2008) discussion on toxicology to animals, "n-Hexane 

is a neurotoxin, a narcotic, and an irritant of the eyes, skin, and mucous membranes [Hathaway et al. 

199I]. n-Hexane also causes (re)productive and embryo toxic effects and is cytotoxic in mammalian and 

human test systems [NIOSH 1991]." OSHA also found that n-Hexane is toxic to humans, and 

recommends extensive medical surveillance for persons working with n-Hexane. 
2010 Methods Update Rule Response to Comments 6 March 2012 

EPA must consider the goals of the Clean Water Act when approving test procedures for Clean Water Act 

permittees in 40 CFR 136. MWWCA believes that the fats, oils and greases that may be toxic to aquatic 

organisms, or interfere with sewer collection systems and wastewater treatment, are primarily petroleum, 

animal or vegetable in origin. These fats, oils and greases are not exclusively "hexane extractable" 

compounds. In fact, other technologies and methods may be better at measuring these compounds, and 

may be used to better quantify how much fat, oil or grease is toxic to aquatic life or interferes with 

wastewater treatment. 

EPA should not specifically and uniquely endorse a solvent specific method for "Oil & Grease." The 

MWWCA requests that EPA reverse its decision that only n-hexane extractable Oil & Grease methods are 

acceptable. We understand that, to further that reversal, EPA must re-write its current definition of oil and 

grease so that new technologies and test methods can be approved. 

Comment 112.1 

Colin Elliott 

King County Environmental Lab 

EPA 1664B: 

Comment: The inclusion of allowed and prohibited modifications is a helpful guide and we agree with 

most of the specific examples, with the exception of the following: 1) The practice of blank subtraction is 

inappropriate when testing any volume of sample (section 1.7.1.5). A full liter analysis should be done if 

the background response is a significant portion of the sample result. 2) The allowance to do alternate 

balance calibration checks is too vague. The current requirement for balance checks doesn’t take 

excessive time and provides more assurance of the accuracy of the analysis.

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

The proposed Oil & Grease Method 1664B, section 8.1.1, states that if the oil & grease analyses are to be 

delayed by more than 4 hours, then adjust the pH and preserve the samples. It cites 40 CFR 136.3, Table 

II. However, Table II requires preservation within 15 minutes. It is misleading for the method to cite 

Table II in this manner. Readers of this section of the method may assume the method holding time and 

preservation requirements are those found in Table II. However, the ability to delay the preservation for 

up to 4 hours is not found in Table II and should be removed from EPA Method 1664B prior to 

promulgation. 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

While we support the replacement of method 1664A with method 1664B, we feel that there may be some 

benefit to establishing a sunset period for method 1664A. There is little difference between these 

versions. Many permits have been written to specifically reflect the use of 1664A. In addition, many 

certification programs certify by specific method. While we support the agency’s efforts to approve only 

a single version of a particular method, we’d like the agency to consider allowing both methods during a 

specified transition period. 

II.A.2 Method 200.5; clarify axial orientation of the torch is allowed for use with EPA Method 

200.7. 
2010 Methods Update Rule Response to Comments 7 March 2012 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 84.1 - Scott Kuhn, Clean Harbors Environmental Services 

Comment 86 - Dave Johnson, Muskegon County Wastewater Management System 

Comment 88.1 - Susan D. Hill, Wisconsin State Laboratory of Hygiene 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 108.1 - George Noguchi, U.S. Department of the Interior, U.S. Fish and Wildlife Service 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Comment 171.1 - Lola Guerra, Henrico County DPU 

Summary of Comments: EPA proposed to approve EPA Method 200.5 and to clarify that axial 

orientation of the torch is allowed for use with EPA Method 200.7. Several comments were received in 

support of this clarification. Two commenters recommended that EPA Method 200.7 be added to the list 

of approved methods for measurement of titanium and one of them stated that the method should be 

added to the list of approved methods for total phosphorus as well. Two commenters recommended that a 

footnote be added to 40 CFR Part 136.3, Table IB to further clarify this. One commenter expressed 

concerns over the use of EPA Method 200.5 in wastewater since this method was originally developed for 

drinking water and stated that EPA Method 200.7, Revision 5.0 should be finalized and approved instead, 

as it would be a more appropriate method for use in wastewater compliance monitoring. This commenter 

further stated that EPA should complete the validation study of Method 200.7, Revision 5.0. 

Response: EPA appreciates the comments supporting the use of the axial orientation of the torch when 

using ICP/AES for measurement of certain elements. EPA also appreciates the comments pointing out 

that EPA Method 200.7 was omitted from the list of methods being approved for measurement of 

titanium and has added the method as an approved option for measurement of titanium in Table IB. EPA 

notes that the proposed rule included EPA Method 200.7 as an approved method for measurement of total 

phosphorus and that Method 200.7 is being approved for measurement of total phosphorus in today’s 

final rule. One commenter questioned why EPA is including only Method 200.8 for titanium using 

ICP/MS. EPA has corrected the approved methods for titanium in the final rule. Specifically, EPA added 

Method 200.7 (Rev. 4.4) as an approved method for the measurement of titanium in addition to Method 

200.8 (Rev. 5.4). 

EPA agrees that further clarification is warranted regarding the acceptability of the use of the axially 

oriented torch with EPA Method 200.7 and has added the use of the axial orientation of the torch to the 

list of previously accepted modifications at part 136.6(b)(4)(W) in the final rule, rather than as a footnote 

to Table IB. 

EPA notes that a typographical error occurred in Section II.J of the proposed rule which stated that the 

version of EPA Method 200.7 that was being removed with Appendix C had been superseded by Revision 

5.4 of Method 200.7. In fact, it was Revision 4.4 of EPA Method 200.7 that superseded the version of the 

method that had been published as Appendix C. The final rule corrects this error. 

EPA agrees that EPA Method 200.5 and EPA Method 200.7 were developed for different matrix types. 

The addition of EPA Method 200.5 as an approved method is intended to allow the use of this method 

where applicable, and not to impose a requirement for use of the method in cases where the quality 

control acceptance criteria in the method cannot be met. In cases where EPA Method 200.7 would be the 

more appropriate method, that method is available (Revision 4.4) and may now be used with the axially 

oriented torch. 
2010 Methods Update Rule Response to Comments 8 March 2012 

With respect to the comment regarding the approval of Method 200.7, Revision 5.0, this draft method 

covers a wider variety of matrices (e.g., biosolids) and we do not have a multi-laboratory validation study 

report assessing the performance of this draft method in different wastewater matrices. EPA will consider 

completing a validation study of EPA Method 200.7, Revision 5.0, as resources allow, and may propose 

approval of Revision 5.0 in a future rulemaking, if appropriate. 

Original Comment Text: 

Comment 79.1 

Richard Burrows 

TestAmerica Inc. 

Clarification of axial torch use for method 200.7 

Comment: We welcome this clarification. Use of the axial torch option is important in order to obtain the 

low detection and quantitation limits frequently required for wastewater analysis. 

Comment 84.1 

Scott Kuhn 

Clean Harbors Environmental Services 

Clean Harbors Environmental Services is the largest hazardous waste management company in North 

America. The company operates several Centralized Wastewater Treatment Plants in the US, as has 

captive wastewater treatment plants that support operations at its incinerators, landfills, and other waste 

treatment and processing facilities. This rule will affect the methods used to demonstrate compliance with 

numerical discharge standards at each one of these facilities. 

The Agency is recommending the use of Method 200.8 for Titanium using ICP/MS. Clean Harbors is 

concerned that the use of this method may be too limiting and doesn't give the user any flexibility to use 

alternative ICP methods that are available. At one Clean Harbors' location, there is only one laboratory in 

the area that is doing Method 200.8. Without additional alternative methods, the facility would be forced 

to use laboratories that are located significant distances from the facility, which will affect the ability of 

the facility to receive data in a timely manner and discharge compliance wastewater. 

On November 7, 2007, EPA issued a memorandum (attached) which allowed the use of Method 200.7 for 

certain inorganic constituents, including titanium. At the time, the Agency determined that the use of 

Method 200.7 was an appropriate methods for titanium and we question why EPA did not include it in 

this proposal. We recommend that the proposed rule be modified to allow the use of this method for 

Titanium in addition to Method 200.8. 

Comment 86 

Dave Johnson 

Muskegon County Wastewater Management System 

EPA Method 200.7, (Metals by Inductively Couple Plasma Atomic Emission Spectroscopy) has been 

around for a number of years and is well-established as one of the backbones of metals analysis. 

However, it is not approved for NPDES compliance monitoring for some of the metals in its analyte list. 

I can well understand this when it comes to mercury, but I can’t understand why this method cannot be 

approved for Titanium and Phosphorus. 

The wavelength recommended for titanium in Method 200.7 (334.9 nm) is very sensitive. There are other 

good wavelengths that work very well, such as 336.1 nm and 337.3 nm, both of which are reasonably 

sensitive and neither line is crippled by common spectral inferences. Please consider approving Method 
2010 Methods Update Rule Response to Comments 9 March 2012 

200.7 for titanium for NPDES compliance monitoring. If Method 200.7 is not approved for titanium, on 

what basis is it being rejected? 

With the advent of axial ICP, phosphorus can easily be quantitated using Method 200.7 at levels 

appropriately low enough for NPDES compliance monitoring. Unfortunately, the wavelength 

recommended in the method (214.9 nm) is not the best wavelength available since copper is a significant 

spectral interferent. I believe at the time that the method was published, the lower UV wavelengths were 

not available using the technology of the day. Therefore 214.9 nm was probably the best wavelength 

option available at the time. (It is certainly better than the wavelength recommended in SW-846 Method 

6010 – 213.6 nm, which is crippled by spectral interferences from copper and molybdenum.) Improved 

technology has made more phosphorus wavelengths available in the lower UV ranges, namely 177.4 nm 

and 178.2 nm, both of which lines are relatively sensitive and less bothered by spectral interferences from 

commonly occurring elements. Even though these two wavelengths aren’t mentioned in the method, the 

footnote to Table 1 of Method 200.7 states, “The wavelengths listed are recommended because of their 

sensitivity and overall acceptability. Other wavelengths may be substituted if they can provide the needed 

sensitivity and are treated with the same corrective techniques for spectral interference.” A noteworthy 

advantage of Method 200.7 over the colorimetric methods for phosphorus is the much greater linear 

dynamic range of the calibration curve for Method 200.7. In light of all this, why is Method 200.7 not 

approved for NPDES compliance monitoring of total phosphorus? 

Please consider adding Method 200.7 to the list of approved methods for phosphorus and titanium. Our 

laboratory has ATPs for both these analytes using Method 200.7, and I can assure you that the method 

works very well for both. 

Comment 88.1 

Susan D. Hill 

Wisconsin State Laboratory of Hygiene 

Federal Register, 9/23/10, p. 58026: section A.2—here in the summary section it notes that the axial 

orientation of the torch is allowed for use with EPA Method 200.7; however, in the body of 40 CFR part 

136, table IB there is no note regarding allowing axial torch orientation under EPA 200.7. We are 

concerned that this will not be clear in the final publication. 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 

Comment: Agree with the clarification for ICP operators being able to use axial or radial views of the ICP 

torch in USEPA Method 200.7. Use of the axial torch option is important in order to obtain the low 

detection and quantitation limits frequently required for wastewater analysis. However, why is method 

200.7 rev 4.4 (1994) still specified in Table IB when there is the more recent USEPA revision 5.4, that is 

mentioned on page 49 as superseding rev. 4.4? 

Comment 108.1 

George Noguchi 

U.S. Department of the Interior, U.S. Fish and Wildlife Service 

The Department agrees that EPA Method 200.5 (Determination of Trace Elements in Drinking Water by 

Axially Viewed Inductively Coupled Plasma) should be included in Table IB and that it should be 

clarified that the axial orientation of the torch is allowed for use with EPA Method 200.7. 

We agree that analytical labs should be allowed the flexibility to use axial instruments or radial 

instruments in measuring metals in water for EPA Method 200.7. When Method 200.7 was developed the 
2010 Methods Update Rule Response to Comments 10 March 2012 

axial technology torch performance data was not available. The axial orientation for some elements 

results in lower detection limits, greater sensitivity, and lesser spectral interference than the radial 

orientation. 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

Section II.A.2 In this summary section, it notes that the axial orientation of the torch is allowed for use 

with EPA Method 200.7. However, in the body of 40 CFR Part 136.3, table IB there is no note regarding 

allowance of the axial torch orientation under EPA 200.7. We believe a note clarifying that the axially 

oriented torch is an allowable method modification should be included. Alternatively, mention could be 

made in 40 CFR Part 136.6(b)(4). 

Comment 132.1 

Paula Hogg 

Hampton Roads Sanitation District 

HRSD supports use of axial torch orientation. However, Method 200.5 and Method 200.7 are for different 

matrices and contain two very distinctive sets of criteria for evaluating QC and determining validity of 

analysis. The following are major areas of concern regarding these differences: 

• Sample Matrices and Interferences (1.1 & 4.1). Method 200.5, developed specifically for drinking 

water and drinking water supply analysis, does not adequately address the challenges of complex 

wastewater matrices. The discussion in section 4.1 on inter-element correction factors (lECs) does not 

sufficiently speak to the interferences routinely encountered in wastewater matrices. When analyzing 

wastewaters, lECs should always be used because the concentrations and components of the wastewater 

matrix are variable and often largely unknown. 

• Use of MCLs as action triggers and acceptance criteria (9.2.5, 11.2.8). Acceptance criteria and action 

triggers for some MDLs, matrix spikes, and use of Method of Standard Additions (MSA) are based on 

criteria such as one-fifth the MCL or greater than 80% of the MCL. MCLs are not used for the NPDES 

program. Requiring that method acceptance criteria derived from the Safe Drinking Water Act (SDWA) 

regulatory standards be applied to the NPDES program is inappropriate, at times meaningless and may 

jeopardize NPDES permit compliance. 

• Laboratory Fortified Blank (LFB) and Laboratory Fortified Matrix (LFM) Concentrations (7.9.3 & 

9.4.2). The required concentrations for the LFB and LFM may not be appropriate for wastewater samples 

or the capability of the instrument. Typically the calibration range and matrix spike concentrations are 

based on expected analyte levels. For analysis of low-level metals, the highest calibration standard may 

only be 500f.lg/L to 1000f.lg/L Cu. The required LFB/LFM spike is 1000 ug/L Cu. Conversely, industrial 

pretreatment samples may have such high concentrations that a 1000 ug/L spike would be insufficient. 

• Laboratory Fortified Matrix (LFM) (11.2.8). 

• Method 200.5 requires "a primary contaminant must be reanalyzed by either method of standard 

additions"., or by another approved method, when the concentration of the primary contaminant 

determined by the normal analytical routine." is 2:.80% of the established Mel, or action level, ". 

"(11.2.8). The NPDES program does not have designated primary contaminants or MCLs. It is also 

unclear how or if the analyst is to apply this requirement to the NPDES program. 
2010 Methods Update Rule Response to Comments 11 March 2012 

• The acceptance range of 85%-115% for percent recovery of the LFM is much tighter than the 70%-

130% recovery found in Method 200.7. The complexity of wastewater matrices causes greater variability 

in precision and bias. QC acceptance limits should be developed using matrices applicable to the method. 

Method 200.5 is not applicable to wastewater matrices. 

• Calculations for LFB and LFM (9.3.2 and 9.4.3). Methods 200.7, 200.8 and 200.9 require the 

Laboratory Reagent Blank (LRB) to be subtracted from the LFB when calculating percent recovery; 

Method 200.5 does not. The LRB is the background concentration of the LFB and should be taken into 

account. Methods 200.7,200.8 and 200.9 require the sample background concentration to be subtracted 

from the LFM, regardless of the concentration. Method 200.5 only allows subtraction of the sample 

background concentration when the sample concentration is >2.2xMDL. Again, the background 

concentration of the sample should be subtracted, regardless of the concentration. Only subtracting the 

sample background concentration when it is >2.2xMDL implies quantitation with a high degree of 

certainty in a region of the calibration curve that is considered to have a high degree of uncertainty (See 

3.7 of this document). Consistency between the two ICP methods, as well as other metals analytical 

methods, being used for the same program is imperative 

Recommendation: In 2002, an EPA method validation study was conducted for Method 200.7, Revision 

5.0 Trace Elements in Water, Solids, and Biosolids by ICP-AES that incorporated the use of axial and 

radial torch technology. The data generated from this study would be better suited for the requirements of 

the NPDES program than the drinking water data used to develop Method 200.5. Methods 200.7 Rev. 4.4 

and Rev. 5.0 are more rugged and better suited for the complex and varied matrices of wastewater 

samples. HRSD suggests completing the remaining data reviews and statistical analyses of this validation 

study. The validation study was conducted using newer technology and is more reflective of the 

capabilities of more modern ICPs. 

Comment 169.1 

Judith R. Morgan 

American Council of Independent Laboratories 

We welcome this clarification. Use of the axial torch option is important in order to obtain the low 

detection and quantitation limits frequently required for wastewater analysis. 

Comment 171.1 

Lola Guerra 

Henrico County DPU 

Comment 2: Mercury, but not titanium, by Method 200.7 Rev 4.4 is approved. Why is titanium not 

included? 

Recommendation 2: Approve titanium by Method 200.7 Rev 4.4 

II.A.3 Method 525.2 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 92 - Lee Wolf, Columbia Analytical Services, Inc. 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 
2010 Methods Update Rule Response to Comments 12 March 2012 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Comment 171.1 - Lola Guerra, Henrico County DPU 

Summary of Comments: EPA proposed to substitute EPA Method 525.2 for Method 525.1 for the 

determination of certain pesticide active ingredients. Most commenters agreed with substituting the 

newer version of the method. A few commenters were concerned about the use of drinking water 

methods for wastewater analyses and suggested that other EPA methods (e.g., SW-846) might be better 

suited to wastewater matrices, or that EPA should revise and expand the 600-Series methods. One 

commenter questioned why the holding time was 30 instead of 40 days for methods 525.1 and 525.2. 

Response: EPA appreciates the comments in support of the inclusion of EPA Method 525.2 to Table IG 

as an additional method for use in measurement of pesticide active ingredients for which Method 525.1 

has been previously approved. EPA also appreciates comments received regarding the substitution of 

EPA Method 525.1 with EPA Method 525.2. At this time EPA will continue to list both EPA Method 

525.1 and EPA Method 525.2 as approved methods to provide additional flexibility in the selection of an 

appropriate method. 

EPA received multiple comments regarding the addition of SW-846 methods; however, the SW-846 

methods were not developed for use in EPA’s water monitoring programs and were not included in the 

proposal for approval at Part 136. The addition of these methods for use in EPA’s water monitoring 

programs falls outside of the scope of today’s rule. Additional comments were received regarding 

updating or expanding the 600-Series methods and these changes also fall outside of the scope of today’s 

rule, but may be included in a future rulemaking. 

EPA acknowledges that the extract holding times listed in Methods 525.1 and 525.2 are 30 days, whereas 

Table II specifies a 40-day extract holding time for the parameters in these two methods. As noted 

elsewhere in this document (see section II.F.1), Table II takes precedence over information provided in 

approved methods. Therefore, if you are using Method 525.1 and 525.2 for Clean Water Act compliance 

monitoring of a pesticide active ingredient listed in Table IH, you are to adhere to the extract holding time 

in Table II (e.g., 40 days). In contrast, if you are using these methods for monitoring compliance with 

Safe Drinking Water Act regulations, the extract holding time is not governed by Table II. It should be 

noted that the holding times specified in Table II are the maximum holding times – extract analyses 

should begin as soon as possible after sample collection. 

Original Comment Text: 

The following commenters supported the substitution of method 525.2 for 525.1 

Comment 79.1 Richard Burrows, TestAmerica Inc. 

Comment 91.1 Andrea Rex, Massachusetts Water Resources Authority 

Comment 92 Lee Wolf,Columbia Analytical Services, Inc. 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 113.1 Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 117.1 Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 169.1 Judith R. Morgan, American Council of Independent Laboratories 

Other comments: 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 
2010 Methods Update Rule Response to Comments 13 March 2012 

Comment: We welcome the addition of these methods, which provide options for many analytes of 

current environmental concern. 

EPA should substitute Method 525.2 for Method 525.1 since Method 525.2 is a newer method and its 

analytical scope is broader. Method 525.2 also contains more updated analytical and QC instructions. 

Since all of the compounds in Method 525.1 are included in Method 525.2, there is no reason to keep 

Method 525.1. Question: Why is the holding time after extraction 30 days instead of 40 days in these two 

methods? 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

Table IC and ID include the methods for non-pesticide and pesticide compounds respectively, Table ID 

now includes drinking water methods as approved for wastewater testing, Drinking water methods are not 

as applicable to wastewater analyses as SW-846 methods due to sample matrices, The 600 series methods 

were created with now obsolete technology and have never been updated, SW-846 methods are updated 

on a more regular basis and generally include more stringent calibration and quality control criteria, The 

600 series methods should either be replaced with SW-846 methods, or they should be revised to update 

the methods to current technological standards and quality control. 

Comment 171.1 

Lola Guerra 

Henrico County DPU 

Comment: Expand the 600 series list of organic method compounds to correlate with 8000 series. Current 

examples include xylene, MIBK, MEK, and 1, 2 diphenylhydrazine which are required for NPDES 

program monitoring and are listed under 8000 series but not the 600 series. Since these compounds are 

not listed in the 600 series, there is not an approved method for NPDES monitoring. Laboratories must 

use separate, non-approved methods. 

Recommendation: Several EPA 600 and 8000 series methods have long been known to be similar in 

application such as EPA methods 624 and 8260B, 625 and 8270D, 608 and 8081B. Considering 

equivalency of these methods, the scope of the 600 series list of organic analytes should be expanded to 

include the compounds in the 8000 series methods, provided that the QA/QC requirements of the more 

stringent methods are met. Monitoring requirements that allow only the use of 40 CFR sanctioned 

methods now includes some analytes that are not covered by the 600 series methods but are included in 

the similar 8000 series methods. Allowing expanding the scope of the 600 series methods will provide 

more flexibility for permittee to meet monitoring requirement using EPA sanctioned and approved 

methods. 

II.A.3.a Method 608.1 

List of Comments: 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 
2010 Methods Update Rule Response to Comments 14 March 2012 

Summary of Comments: Two commenters supported the addition of Method 608.1, while one 

commenter suggested that other methods, particularly those from the SW-846 methods manual were more 

appropriate and should be included. 

Response: EPA appreciates the comments in support of the addition of EPA Method 608.1 to Table ID. 

Regarding the SW-846 methods, see response in Section II.A.3. 

Original Comment Text: 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

Section II.A.3 a-j While we support the addition of some of the nonconventional pesticide methods, 

which have been in use for more than 10 years, to Tables ID and IG for general use, we believe the EPA 

is being too restrictive in its approach. The methods proposed for addition are those as published in the 

1992 publication, ‘‘Methods for the Determination of Non-conventional Pesticides in Municipal and 

Industrial Wastewater,’’ EPA 821–R–92–002, April 1992. While we appreciate and encourage the 

increased flexibility in considering other available method resources for general analytical use, we feel 

that the EPA is overlooking a far more comprehensive compendium of methods published in SW-846 as 

well as other drinking water methods. In a sense, we strongly the current exclusion of the SW-846 can be 

viewed as disingenuous to the philosophy of moving technology and methodologies forward. The SW846 methodologies are more technically advanced, are updated with reasonable frequency, and have been 

used successfully in a variety of matrices, including wastewaters, for many years. For example, how can 

the EPA consider approving methods 614 and 614.1 for organophosphorus pesticides, which have not 

been revised since 1992, yet not consider approving the more recent companion SW-846 method 8141B, 

which was updated as recently as 2007? We feel that it is fitting, given the EPA’s renewed focus on 

streamlining method approvals, that SW-846 methodologies as well as other approved drinking water 

methods (“500” series) be listed in Tables IC, ID, IF and IG and approved for use in support of Clean 

Water Act analyses. 

II.A.3.b Method 608.2 

List of Comments: 

Comment 114.1 - Z. Bernie A. Wilk, New Jersey Department of Environmental Protection 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Summary of Comments: One commenter supported the addition of Method 608.2, but suggested that 

other methods, particularly those from the SW-846 methods manual were more appropriate and should be 

included. Another commenter raised issues with the approval of Methods 515.1 and 515.2 for DCPA, 

which were actions taken by EPA in a previous rulemaking. 

Response: EPA appreciates the comment in support of the addition of EPA Method 608.2 to Table ID. 

Regarding the SW-846 methods, see response in Section II.A.3. 

EPA Methods 515.1 and 515.2 were approved for measurement of DCPA in a previous rule. These 

methods are appropriate for the determination of DCPA degradates, as the commenter stated and a 

footnote was added to Table IG for clarification. 

Original Comment Text: 

Comment 114.1 

Z. Bernie A. Wilk 

New Jersey Department of Environmental Protection 
2010 Methods Update Rule Response to Comments 15 March 2012 

The proposed rule dated Sept 23, 2010 indicates that EPA methods 515.1 and 515.2 among others will be 

approved methods for the analysis of DCPA. Discussions with EPA’s Drinking Water Program (D. 

Munch) indicate that these methods when performed as written are not appropriate for the analysis of the 

free DCPA but are only applicable to the analysis of the DCPA degradates (mono and diacids). The 

remaining methods do seem appropriate for the analysis of DCPA. Please review and clarify as 

appropriate. 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

While we support the addition of some of the nonconventional pesticide methods, which have been in use 

for more than 10 years, to Tables ID and IG for general use, we believe the EPA is being too restrictive in 

its approach. The methods proposed for addition are those as published in the 1992 publication, 

‘‘Methods for the Determination of Non-conventional Pesticides in Municipal and Industrial 

Wastewater,’’ EPA 821–R–92–002, April 1992. While we appreciate and encourage the increased 

flexibility in considering other available method resources for general analytical use, we feel that the EPA 

is overlooking a far more comprehensive compendium of methods published in SW-846 as well as other 

drinking water methods. In a sense, we strongly the current exclusion of the SW-846 can be viewed as 

disingenuous to the philosophy of moving technology and methodologies forward. The SW-846 

methodologies are more technically advanced, are updated with reasonable frequency, and have been 

used successfully in a variety of matrices, including wastewaters, for many years. For example, how can 

the EPA consider approving methods 614 and 614.1 for organophosphorus pesticides, which have not 

been revised since 1992, yet not consider approving the more recent companion SW-846 method 8141B, 

which was updated as recently as 2007? We feel that it is fitting, given the EPA’s renewed focus on 

streamlining method approvals, that SW-846 methodologies as well as other approved drinking water 

methods (“500” series) be listed in Tables IC, ID, IF and IG and approved for use in support of Clean 

Water Act analyses. 

II.A.3.c Method 614 

List of Comments: 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 187 - Peter Halpin, Caltest Analytical Laboratory 

Summary of Comments: Two commenters supported the addition of Method 614. One commenter 

suggested that other methods, particularly those from the SW-846 methods manual were more appropriate 

and should be included. A fourth commenter requested that this method also be allowed for the 

determination of chlorpyrifos even though this analyte is not specifically listed in the method. 

Response: EPA appreciates the comment in support of the addition of EPA Method 614 to Table ID. 

Regarding the SW-846 methods, see response in Section II.A.3. In response to the comment regarding the 

addition of chlorpyrifos to EPA Method 614, updating or expanding the 600-Series methods also falls 

outside of the scope of today’s rule. However, under the ATP program, any person wishing to use 

Method 614 for the measurement of chlorpyrifos or modify any 600-Series methods to add analytes not 

included in the approved method may apply for approval for use of an alternate test procedure. The 

performance of any proposed alternative method for a given analyte must be equivalent or better than the 

performance of the approved method for EPA to grant approval of an ATP. 
2010 Methods Update Rule Response to Comments 16 March 2012 

Original Comment Text: 

The following supported the addition of the new methods. 

Comment 132.1 Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Other comments: 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

Section II.A.3 a-j While we support the addition of some of the nonconventional pesticide methods, 

which have been in use for more than 10 years, to Tables ID and IG for general use, we believe the EPA 

is being too restrictive in its approach. The methods proposed for addition are those as published in the 

1992 publication, ‘‘Methods for the Determination of Non-conventional Pesticides in Municipal and 

Industrial Wastewater,’’ EPA 821–R–92–002, April 1992. While we appreciate and encourage the 

increased flexibility in considering other available method resources for general analytical use, we feel 

that the EPA is overlooking a far more comprehensive compendium of methods published in SW-846 as 

well as other drinking water methods. In a sense, we strongly the current exclusion of the SW-846 can be 

viewed as disingenuous to the philosophy of moving technology and methodologies forward. The SW846 methodologies are more technically advanced, are updated with reasonable frequency, and have been 

used successfully in a variety of matrices, including wastewaters, for many years. For example, how can 

the EPA consider approving methods 614 and 614.1 for organophosphorus pesticides, which have not 

been revised since 1992, yet not consider approving the more recent companion SW-846 method 8141B, 

which was updated as recently as 2007? We feel that it is fitting, given the EPA’s renewed focus on 

streamlining method approvals, that SW-846 methodologies as well as other approved drinking water 

methods (“500” series) be listed in Tables IC, ID, IF and IG and approved for use in support of Clean 

Water Act analyses. 

Comment 187 

Peter Halpin 

Caltest Analytical Laboratory 

With regard to adding an analyte, for years now our San Francisco Bay and Sacramento Delta regions 

have had toxicity problems with diazinon and chlorpyrifos. Chlorpyrifos is not a listed analyte in the 

CWA list of approved methods/analytes. Our regulatory agencies requested chlorpyrifos be included in 

the EPA 614 method. This method performs very well for that analyte, but is not specifically listed. It 

would be helpful for the Clean Water Act to allow for additional required analytes to be added to existing 

protocols when this can be demonstrated to be effective. 

Our extraction comments are based on our experience with the subjects we commented on, specifically: 

We have experience in solid phase extraction for methods 608, 614, 632, TPH-Diesel, and Pyrethroid 

pesticides. The current limitation is not the methods of solid phase extraction, but the suitability of the 

sample with regard to passing through the solid phase media when the sample particles for some samples 

clog the filter used. We have experience in running the EPA Method 617 compounds using the EPA 

Method 608 methylene chloride extraction for informational purposes. 

Our mass spectrometer comments are based on our experience using quadrapole mass spectrometers to 

reach the method reporting limits for EPA Methods 608, and 614. 

II.A.3.d Method 614.1 

List of Comments: 
2010 Methods Update Rule Response to Comments 17 March 2012 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Summary of Comments: Two commenters supported the addition of Method 614.1. One commenter 

suggested that other methods, particularly those from the SW-846 methods manual were more appropriate 

and should be included. 

Response: EPA appreciates the comment in support of the addition of EPA Method 614.1 to Table ID. 

Regarding the SW-846 methods, see response in Section II.A.3. 

Original Comment Text: 

The following commenters supported the addition of the new methods. 

Comment 132.1 Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Other comments: 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

Section II.A.3 a-j While we support the addition of some of the nonconventional pesticide methods, 

which have been in use for more than 10 years, to Tables ID and IG for general use, we believe the EPA 

is being too restrictive in its approach. The methods proposed for addition are those as published in the 

1992 publication, ‘‘Methods for the Determination of Non-conventional Pesticides in Municipal and 

Industrial Wastewater,’’ EPA 821–R–92–002, April 1992. While we appreciate and encourage the 

increased flexibility in considering other available method resources for general analytical use, we feel 

that the EPA is overlooking a far more comprehensive compendium of methods published in SW-846 as 

well as other drinking water methods. In a sense, we strongly the current exclusion of the SW-846 can be 

viewed as disingenuous to the philosophy of moving technology and methodologies forward. The SW846 methodologies are more technically advanced, are updated with reasonable frequency, and have been 

used successfully in a variety of matrices, including wastewaters, for many years. For example, how can 

the EPA consider approving methods 614 and 614.1 for organophosphorus pesticides, which have not 

been revised since 1992, yet not consider approving the more recent companion SW-846 method 8141B, 

which was updated as recently as 2007? We feel that it is fitting, given the EPA’s renewed focus on 

streamlining method approvals, that SW-846 methodologies as well as other approved drinking water 

methods (“500” series) be listed in Tables IC, ID, IF and IG and approved for use in support of Clean 

Water Act analyses. 

II.A.3.e Method 615 

List of Comments: 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 187 - Peter Halpin, Caltest Analytical Laboratory 

Summary of Comments: One commenter supported the addition of this method but also suggested that 

other methods, particularly those from the SW-846 methods manual are more appropriate and should be 

included. A second commenter noted concerns with the derivatization steps and hazardous reagents used 

in this method and suggested that as techniques become available which include an on-line automated 

derivatization step, it would be useful to have a path forward for using such techniques in CWA analyses. 
2010 Methods Update Rule Response to Comments 18 March 2012 

Response: EPA appreciates the comment in support of the addition of EPA Method 615 to Table ID. 

Regarding the SW-846 methods, see response in Section II.A.3. 

Regarding concerns about hazardous reagents used in this method, the inclusion of EPA Method 615 

provides an additional option when choosing a method for measurement of the compounds for which it is 

being approved. However, other methods are approved for measurement of these compounds and today’s 

rule does not impose a requirement for use of Method 615. 

Regarding the approval of methods that employ an on-line automated derivatization step for use in 

compliance monitoring under the requirements of the Clean Water Act, EPA welcomes applications for 

alternate or new methods under its ATP program. The commenter should submit information to EPA’s 

Alternate Test Procedure (ATP) program (see http://water.epa.gov/scitech/methods/cwa/atp/atp_index.cfm

to determine if the proposed changes are acceptable modifications or require additional validation.

Original Comment Text: 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

Section II.A.3 a-j While we support the addition of some of the nonconventional pesticide methods, 

which have been in use for more than 10 years, to Tables ID and IG for general use, we believe the EPA 

is being too restrictive in its approach. The methods proposed for addition are those as published in the 

1992 publication, ‘‘Methods for the Determination of Non-conventional Pesticides in Municipal and 

Industrial Wastewater,’’ EPA 821–R–92–002, April 1992. While we appreciate and encourage the 

increased flexibility in considering other available method resources for general analytical use, we feel 

that the EPA is overlooking a far more comprehensive compendium of methods published in SW-846 as 

well as other drinking water methods. In a sense, we strongly the current exclusion of the SW-846 can be 

viewed as disingenuous to the philosophy of moving technology and methodologies forward. The SW846 methodologies are more technically advanced, are updated with reasonable frequency, and have been 

used successfully in a variety of matrices, including wastewaters, for many years. For example, how can 

the EPA consider approving methods 614 and 614.1 for organophosphorus pesticides, which have not 

been revised since 1992, yet not consider approving the more recent companion SW-846 method 8141B, 

which was updated as recently as 2007? We feel that it is fitting, given the EPA’s renewed focus on 

streamlining method approvals, that SW-846 methodologies as well as other approved drinking water 

methods (“500” series) be listed in Tables IC,ID, IF and IG and approved for use in support of Clean 

Water Act analyses. 

Comment 187 

Peter Halpin 

Caltest Analytical Laboratory 

With regard to herbicide analyses, few labs want to provide the listed Method 615 method due to its 

hazards and high cost due to its complicated and time consuming nature. As techniques become available 

which include an on-line automated derivatization step, it would be useful to have a path forward for 

using in CWA analyses, as a modified method, providing of course all method QC was met for the matrix 

of concern at the concentrations of concern. 

II.A.3.f Method 617 

List of Comments: 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 
2010 Methods Update Rule Response to Comments 19 March 2012 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 187 - Peter Halpin, Caltest Analytical Laboratory 

Comment 194 - John Burnett, Baltimore County, MD 

Summary of Comments: Two commenters supported the inclusion of Method 617. One commenter 

suggested that other methods, particularly those from the SW-846 methods manual were more appropriate 

and should be included. Another commenter expressed the desire to use conventional extractions as 

broadly as their performance allows, rather than separate, different extractions as in the case of Method 

617 versus Method 608. A fifth commenter expressed concerns about the use of Method 617 in 

pretreatment samples with a high organic solids content (as opposed to final effluents), and for trifluralin 

in particular. 

Response: EPA appreciates the comments in support of the addition of EPA Method 617 to Table ID. 

Regarding the SW-846 methods, see response in Section II.A.3. 

In response to the comment regarding additional flexibility with respect to the use of the extraction 

solvent specified in EPA Method 608 with EPA Method 617, updating or expanding the 600-Series 

methods also falls outside of the scope of today’s rule. However, under the ATP program, any person 

may apply for approval for use of an alternate test procedure, including a change in extraction solvent, 

provided the alternative method results in equivalent or better performance for the analytes of interest 

compared to the approved method, see response in Section II.A.3.e for more details on the ATP program. 

In response to the comment regarding the use of EPA Method 617 for pretreatment monitoring, the 

inclusion of EPA Method 617 provides an additional option when choosing a method for measurement of 

the compounds for which it is being approved (e.g., trifluralin). However, because other methods are 

approved for measurement of these compounds, today’s rule does not impose a requirement for the use of 

Method 617. If other methods approved at Part 136 are more appropriate for a given application (such as 

for samples with high organic solids content), then those methods may be used. 

Original Comment Text: 

The following commenters supported the addition of the new methods. 

Comment 132.1 Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Other comments: 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

Section II.A.3 a-j While we support the addition of some of the nonconventional pesticide methods, 

which have been in use for more than 10 years, to Tables ID and IG for general use, we believe the EPA 

is being too restrictive in its approach. The methods proposed for addition are those as published in the 

1992 publication, ‘‘Methods for the Determination of Non-conventional Pesticides in Municipal and 

Industrial Wastewater,’’ EPA 821–R–92–002, April 1992. While we appreciate and encourage the 

increased flexibility in considering other available method resources for general analytical use, we feel 

that the EPA is overlooking a far more comprehensive compendium of methods published in SW-846 as 

well as other drinking water methods. In a sense, we strongly the current exclusion of the SW-846 can be 

viewed as disingenuous to the philosophy of moving technology and methodologies forward. The SW846 methodologies are more technically advanced, are updated with reasonable frequency, and have been 

used successfully in a variety of matrices, including wastewaters, for many years. For example, how can 

the EPA consider approving methods 614 and 614.1 for organophosphorus pesticides, which have not 

been revised since 1992, yet not consider approving the more recent companion SW-846 method 8141B, 
2010 Methods Update Rule Response to Comments 20 March 2012 

which was updated as recently as 2007? We feel that it is fitting, given the EPA’s renewed focus on 

streamlining method approvals, that SW-846 methodologies as well as other approved drinking water 

methods (“500” series) be listed in Tables IC,ID, IF and IG and approved for use in support of Clean 

Water Act analyses. 

Comment 187 

Peter Halpin 

Caltest Analytical Laboratory 

With regard to solvents called for in the methods, many of the same analytes are included in EPA 

methods 608 and 617. EPA Method 617 is proposed for general use in this update. However the Method 

617 requires a blend of methylene chloride and hexane, where Method 608 does not. We have extracted 

the analytes of the 617 list that are not in the 608 method, using the 608 extraction of methylene chloride 

only. We find good extraction comparable to our other 608 analytes. It would be helpful to be able to use 

conventional extractions as broadly as their performance allows, rather than separate, different extractions 

as in the case of 617 versus 608. Currently some of our clients are required by permits to use EPA 

Method 608. Other clients are required to use EPA Method 608 and additionally monitor for Perthane and 

Strobane (analytes from EPA Method 617). If EPA Method 617 is brought into the general use tables, 

then when analytes specific to that method are required, they would be required by that method. Even 

though Perthane and Strobane extract well in the EPA Method 608 methylene chloride extraction, unless 

EPA made a written allowance for the extraction change or adding of compounds to Method 608, clients 

would have to run two separate extractions and analyses to comply with their permit, even though only 

one extraction and analysis is required from the lab view. Combining analytes/methods where appropriate 

could offer significant cost savings to monitoring programs. Combining triazine pesticides with 

organophosphorus pesticides for example, is feasible for many analytes, but clarification that this would 

be acceptable would be useful. 

Our extraction comments are based on our experience with the subjects we commented on, specifically: 

We have experience in solid phase extraction for methods 608, 614, 632, TPH-Diesel, and Pyrethroid 

pesticides. The current limitation is not the methods of solid phase extraction, but the suitability of the 

sample with regard to passing through the solid phase media when the sample particles for some samples 

clog the filter used. We have experience in running the EPA Method 617 compounds using the EPA 

Method 608 methylene chloride extraction for informational purposes. 

Comment 194 

John Burnett 

Baltimore County, MD 

I am deeply concerned about the proposed wholesale adoption of methods for organic parameters found 

in EPA Method 617 as applicable to the sanitary sewer. They are not. There are many reasons for this 

concern, but a couple of primary reasons are: 

1. Failure to address high organic solids content of the samples. There is no provision in Method 617 

for any of the target analytes to account for the potential high organic solids that may be found. Many of 

the target parameters will have a much higher affinity for and will bind to the solids that can be found. 

This will result in artificially low analytical results as that portion of the parameter will not be accounted 

for or appear. This further complicates the possibility of pass through and/or sludge management issues 

for the POTW. 

2. Failure to recognize the extremely high probability of interferences due to the nature of the matrix 

itself. Wastewater contains a significant amount of chlorination (and some fluoridation). The bulk of this 

is due to the fact that it is a used drinking water. The electron capture detector is designed to identify 
2010 Methods Update Rule Response to Comments 21 March 2012 

chlorinated/fluoridated compounds. Add to the original level the amount of chlorine added by industrial 

process, cleaning solutions (bleach), etc, the level of chlorinated organic compounds makes the choice of 

detector untenable for many of the target parameters. 

3. Failure to recognize the impact of flora in the sanitary sewer on the holding time. I have conducted 

several studies in an effort to create a method for analysis of glycols in the sanitary sewer. The creatures 

in the system love it and it is devoured rather quickly. The holding time for extraction maybe as little as 

48 hours for some of the target analytes, others may indeed be as long as 14 days. To blindly accept 14 

days solely because that is what works in drinking waters that do not have the flora and fauna that exists 

in the sewer is foolish. 

4. Experience. As a pretreatment coordinator, I have had the challenging opportunity to examine 

one of the target analytes (trifluralin) first hand. We had an industry that was creating a product for use in 

“green” buildings to allow for the planting of rooftop gardens that would protect the building’s roof 

structure from root growth. Trifluralin is a root growth inhibitor. This particular company was 

incorporating it into a product that could be applied to a flat roof, which would protect the roof from roots 

damaging the roof. The company’s handling of the trifluralin brought the attention of our state’s OSHA, 

and they asked me for information on methods for trifluralin. Trifluralin in one of the target compounds 

listed in EPA Method 617. Trifluralin is also known to be very toxic to aquatic organisms. My question 

quickly became, is poor handling allowing any of the trifluralin to be washed into the company’s drains 

and thereby into the sewer? Method 617 did not work, for all of the reasons stated above. I was able to 

create an approach that did work well enough to convince myself that none of the trifluralin was entering 

the sewer.

II.A.3.g Method 619 

II.A.3.h Method 622 

II.A.3.i Method 622.1 

List of Comments: 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Summary of Comments: Two commenters supported the inclusion of Methods 619, 622 and 622.1. 

One commenter suggested that other methods, particularly those from the SW-846 methods manual were 

more appropriate and should be included. 

Response: EPA appreciates the comments in support of the addition of EPA Methods 619, 622, and 

621.1 to Table ID. Regarding the SW-846 methods, see response in Section II.A.3. 

Original Comment Text: 

The following commenters supported the addition of the new methods. 

Comment 132.1 Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Other comments: 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

Section II.A.3 a-j While we support the addition of some of the nonconventional pesticide methods, 

which have been in use for more than 10 years, to Tables ID and IG for general use, we believe the EPA 
2010 Methods Update Rule Response to Comments 22 March 2012 

is being too restrictive in its approach. The methods proposed for addition are those as published in the 

1992 publication, ‘‘Methods for the Determination of Non-conventional Pesticides in Municipal and 

Industrial Wastewater,’’ EPA 821–R–92–002, April 1992. While we appreciate and encourage the 

increased flexibility in considering other available method resources for general analytical use, we feel 

that the EPA is overlooking a far more comprehensive compendium of methods published in SW-846 as 

well as other drinking water methods. In a sense, we strongly the current exclusion of the SW-846 can be 

viewed as disingenuous to the philosophy of moving technology and methodologies forward. The SW846 methodologies are more technically advanced, are updated with reasonable frequency, and have been 

used successfully in a variety of matrices, including wastewaters, for many years. For example, how can 

the EPA consider approving methods 614 and 614.1 for organophosphorus pesticides, which have not 

been revised since 1992, yet not consider approving the more recent companion SW-846 method 8141B, 

which was updated as recently as 2007? We feel that it is fitting, given the EPA’s renewed focus on 

streamlining method approvals, that SW-846 methodologies as well as other approved drinking water 

methods (“500” series) be listed in Tables IC,ID, IF and IG and approved for use in support of Clean 

Water Act analyses. 

II.A.3.j Method 632 

List of Comments: 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 187 - Peter Halpin, Caltest Analytical Laboratory 

Summary of Comments: Two commenters supported the inclusion of Method 632. One commenter 

suggested that other methods, particularly those from the SW-846 methods manual were more appropriate 

and should be included. A fourth commenter expressed concerns about the solid-phase extraction 

procedure in the method when the sample particles for some samples clog the filter. 

Response: EPA appreciates the comments in support of the addition of EPA Method 632 to Table ID. 

Regarding the SW-846 methods, see response in Section II.A.3. 

The inclusion of EPA Method 632 provides an additional option when choosing a method for 

measurement of the compounds for which it is being approved. However, other methods are approved for 

measurement of these compounds, and today’s rule does not impose a requirement for use of Method 632. 

If another approved method is more appropriate for a given use (such as for samples that may clog the 

filter), then another approved method may be used. 

Original Comment Text: 

The following commenters supported the addition of Method 632. 

Comment 132.1 Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Other comments: 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

Section II.A.3 a-j While we support the addition of some of the nonconventional pesticide methods, 

which have been in use for more than 10 years, to Tables ID and IG for general use, we believe the EPA 

is being too restrictive in its approach. The methods proposed for addition are those as published in the 

1992 publication, ‘‘Methods for the Determination of Non-conventional Pesticides in Municipal and 
2010 Methods Update Rule Response to Comments 23 March 2012 

Industrial Wastewater,’’ EPA 821–R–92–002, April 1992. While we appreciate and encourage the 

increased flexibility in considering other available method resources for general analytical use, we feel 

that the EPA is overlooking a far more comprehensive compendium of methods published in SW-846 as 

well as other drinking water methods. In a sense, we strongly [sic] the current exclusion of the SW-846 

can be viewed as disingenuous to the philosophy of moving technology and methodologies forward. The 

SW-846 methodologies are more technically advanced, are updated with reasonable frequency, and have 

been used successfully in a variety of matrices, including wastewaters, for many years. For example, how 

can the EPA consider approving methods 614 and 614.1 for organophosphorus pesticides, which have not 

been revised since 1992, yet not consider approving the more recent companion SW-846 method 8141B, 

which was updated as recently as 2007? We feel that it is fitting, given the EPA’s renewed focus on 

streamlining method approvals, that SW-846 methodologies as well as other approved drinking water 

methods (“500” series) be listed in Tables IC,ID, IF and IG and approved for use in support of Clean 

Water Act analyses. 

Comment 187 

Peter Halpin 

Caltest Analytical Laboratory 

Our extraction comments are based on our experience with the subjects we commented on, specifically: 

We have experience in solid phase extraction for methods 608, 614, 632, TPH-Diesel, and Pyrethroid 

pesticides. The current limitation is not the methods of solid phase extraction, but the suitability of the 

sample with regard to passing through the solid phase media when the sample particles for some samples 

clog the filter used. 

II.A.4 Method 1614A 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 125.1 - John H. Phillips, Ford Motor Company 

Summary of Comments: Two commenters supported the inclusion of Method 1614A. Another 

commenter expressed concerns with the extent of method validation undertaken by EPA and with other 

technical aspects of the method. 

Response: Upon further evaluation of the data supporting the use of this test procedure and the peer 

review comments, EPA agrees with the commenter who stated that additional validation data are needed 

to fully characterize the performance of this method for various matrices and has decided not to include 

Method 1614A in today’s final rule. 

Original Comment Text: 

The following commenters supported the addition of the Method 1614A. 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Other comments: 

Comment 125.1 

John H. Phillips 

Ford Motor Company 

Method 1614A- This method is sensitive to interferences, especially to DeBDE. This method has not 

been fully validated, as only a single laboratory performance data is presented. The MDLs and MLs 
2010 Methods Update Rule Response to Comments 24 March 2012 

listed are not achievable for some congeners (BDE-47, 99 & 100 for example). An additional labeled 

internal standards and different injection recovery standards are needed. Sample dilution affects the 

functionality of isotope dilution with the addition of labeled standards. 

II.A.5 Method 1668C 

EPA proposed to approve Method 1668C, a high resolution gas chromatography - mass spectrometry 

procedure, for the analysis of PCB congeners. The proposal of this method resulted in a large number of 

detailed comments on a wide range of topics. EPA is continuing to evaluate the comments and this 

review will take more time than anticipated. Many comments refer to the quality of the supporting data 

and EPA wants to thoroughly review the concerns raised in light of the criticisms. Therefore, in order to 

prevent a delay in promulgation of other methods included in the Methods Update Rule, EPA has decided 

to postpone consideration of Method 1668C until a later date. The comments received in response to the 

proposed rule will be addressed at that time. 

II.A.6 Methods 1622 and 1623 

No comments regarding Methods 1622 and 1623 were received. EPA is finalizing these two methods as 

proposed. 

II.A.7 Bacteriological Methods 

List of Comments: 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 166.1 - Paul Wiegand, National Council for Air and Stream Improvement, Inc. 

Summary of Comments: One commenter noted that SM2540G for total, fixed, and volatile solids is not 

listed, but should be, in Table IB. A second commenter expressed concern that these methods may not 

apply or do not perform as well in industrial wastewaters as they do in POTW effluents. That commenter 

submitted a technical report on the subject. 

Response: The approved methods for solids assume total solids rather than fixed or volatile solids for 

assay of fecal coliforms or Salmonella in sewage sludge. EPA Methods 1680, 1681, and 1682 include the 

procedure to determine total solids in Section 12.4 for EPA Methods 1680, 1681 and in Section 12.5 for 

EPA Method 1682. Thus, a separate method such as SM 2540G to determine total solids is not required 

in Table IB. 

EPA thanks the second commenter for the comments regarding the applicability of the methods and for 

providing the technical report of a study on the subject. The methods listed as approved in 40 CFR part 

136 apply to discharge permits under the NPDES program, or to “Certifications issued by States pursuant 

to section 401 of the CWA, as amended: (136.1(c)).” In general, these would be discharges, not 

necessarily specific to any one type. A number of methods have been approved or are available for use in 

wastewater. Permittees have the option of using any approved method for the organisms of interest in the 

specific matrix unless the permit specifies otherwise. 

Original Comment Text: 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 
2010 Methods Update Rule Response to Comments 25 March 2012 

SM2540G, % total, fixed and volatile solids, is not listed in the updated Table IB. Because the biosolids 

procedures themselves are included in Table IA, Parameter #1, e.g., EPA 1680, 1681, it is requested that 

the SM 2540G be added to Table IB. 

Comment 166.1 

Paul Wiegand 

National Council for Air and Stream Improvement, Inc. 

When applied to pulp and paper final effluents, methods for Escherichia coli (E. coli) and enterococci 

produced widely varying results depending on which technique (membrane filtration, multiple tube most 

probably number, or enzyme substrate) was used. EPA should limit approval of E. coli and enterococci 

methods to only receiving waters, municipal wastewaters, and those wastewaters included in the 

validation studies conducted to support promulgation of the methods. NCASI is submitting Technical 

Bulletin No. 971 in support of this comment. 

In March 2007, EPA approved the use of several EPA membrane filtration methods for the analysis of 

Escherichia coli (E. coli) (Methods 1103.1 and 1603) and enterococci (Methods 1106.1 and 1600) in 

surface waters and wastewater matrices, and for fecal coliforms in sewage sludge (Method 1680). EPA 

proposes approval of revisions to all but EPA 1603 to correct technical errors. Multiple tube-most 

probably number (MT-MPN), and multiple tube or multiple well enzyme substrate methods are also 

approved for E. coli and enterococci measurements. More recently, water quality-based permit 

limitations are being proposed for pulp and paper wastewater discharges, although none of these methods 

have been validated using pulp and paper wastewaters. NCASI conducted a study to compare E. coli and 

enterococci measurements using multiple tube-most probably number, enzyme substrate, and membrane 

filtration tests (EPA Methods 1603 and 1600, respectively) in three pulp and paper final effluent samples 

at three contract laboratories (NCASI TB971, 2009). This study showed matrix-related dilution effects 

when measuring both E. coli and enterococci and high variability among the various test methods. There 

was no clear indication that one enterococci test method performed better than another when applied to 

pulp and paper wastewaters, but the results generated using EPA Method 1600 by membrane filtration 

showed elevated levels in all three wastewaters compared to other method types and other membrane 

filtration media. The application of any of the approved methods for source identification of E. coli or 

enterococci involving pulp and paper final effluents could result in misleading conclusions and 

inappropriate water quality-based permit limitations. 

II.A.8 Method 1627 

No comments regarding Method 1627 were received. EPA is finalizing this method as proposed. 

II.A.9 EPA Method 624 for Quantitation of Acrolein and Acrylonitrile 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica, Inc 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 92 - Lee Wolf, Columbia Analytical Services, Inc 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 98.1 - URS Corporation 

Comment 112.1 - Colin Elliot, King County Environmental Lab 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 123 - Vincent Sapienza, New York City Department of Environmental Protection 
2010 Methods Update Rule Response to Comments 26 March 2012 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Summary of Comments: Most commenters supported the use of Method 624 for the determination of 

these two analytes. Several commenters noted that different preservation methods might be required for 

these two analytes compared to the others in Method 624, and one commenter noted that there were no 

QC acceptance criteria in the method for these two analytes. One commenter expressed concern that 

adding these two analytes to the method stems from comments by a single laboratory rather than from 

multi-laboratory testing and the Agency should not offer a carte blanche approval. One commenter 

submitted the results from a holding time study that included these analytes. Another commenter 

recommended that Methods 624 and 625 be revised to incorporate acceptance criteria for additional 

analytes. 

Response: EPA appreciates comments received in support of the use of Method 624 for determination of 

acrolein and acrylonitrile. Changes to required preservation and holding time requirements for acrolein 

and acrylonitrile compounds were not proposed as part of this rulemaking. However, one commenter 

noted that the preservation and holding time requirements for these two analytes in Table II differ from 

the requirements for other Method 624 analytes. The current requirements in Table II date to 1984 and 

specify that samples for acrolein and acrylonitrile must be preserved at a pH in the range of 4 to 5. This 

pH range was based on concerns about degradation of these two analytes in strongly acidic samples (e.g., 

pH < 2). Footnote 10 to Table II currently states that pH adjustment is not required if acrolein will not be 

measured, but that samples for acrolein receiving no pH adjustment must be analyzed within 3 days of 

sampling. In contrast, samples analyzed by EPA Method 624 for most other volatile organic compounds 

are not preserved by adjusting the pH, and may be held for up to 14 days. Samples to be analyzed for the 

purgeable aromatic hydrocarbons (i.e., benzene, ethylbenzene, and toluene) are preserved at a pH of < 2, 

and may also be held up to 14 days. Thus, in the case where a permittee wanted to use EPA Method 624 

to measure acrolein or acrylonitrile in addition to other analytes included in Method 624, the sampler 

would have to take two different sets of samples, and perform two separate analyses. Commenters stated 

that EPA does not have a basis for requiring a different preservation and holding time for these two 

analytes and submitted data in support of their assertion that sample preservation be allowed at either a 

pH of 7 or a pH of 2. EPA reviewed these data but the Agency has concluded that these data are not 

sufficient or compelling to change the current preservation and holding time requirements for these 

analytes because the data are anecdotal rather than the result of a well-planned and properly documented 

stability study. As a result, EPA’s final rule retains the current preservation and holding time 

requirements for acrolein and acrylonitrile. 

EPA acknowledges that quality control (QC) acceptance criteria for acrolein and acrylonitrile do not 

appear in EPA Method 624 and has added a footnote to Table IC (footnote 4) indicating that the QC 

acceptance criteria from EPA Method 603 should be used when analyzing samples for acrolein and 

acrylonitrile using EPA Method 624 in the absence of QC acceptance criteria for these compounds in 

Method 624. Regarding the comment about granting carte blanche approval of this method for these two 

analytes, EPA agrees that caution must be exercised because EPA has not conducted an extensive multilab study. However, EPA supports this change because many laboratories have had experience with the 

use of Method 624 for the determination of these two analytes and the Agency desires to provide them the 

flexibility to use this method provided the laboratories can demonstrate acceptable performance. 

Therefore, as suggested by the same commenter, EPA has included language in footnote 4 to Table IC 

indicating that Method 624 may be used for quantitative determination of acrolein and acrylonitrile, 

provided that the laboratory has documentation to substantiate the ability to detect and quantify these 

analytes at levels necessary to comply with any associated regulations, and indicating that the use of 

sample introduction techniques in addition to simple purge-and-trap may be required. 

Footnote 5 to Table IC, regarding the use of EPA Method 625 for analysis of benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, and N-nitrosodiphenylamine, first appeared in 1984. The footnote 
2010 Methods Update Rule Response to Comments 27 March 2012 

is intended as guidance for permitting authorities and permittees when selecting methods. Although other 

methods may be preferred, a facility is still in compliance if it continues using EPA Method 625 as the 

quantitative method for these compounds if other analytical methods have not been established in the 

facility’s laboratory or Method 625 is specified in their permit. 

With regard to the question about why is not EPA revising Methods 624 and 625, changes to these 

methods are outside the scope of this rulemaking. 

Original Comment Text: 

The following commenters supported the addition of the analytes for Method 624. 

Comment 79.1 Richard Burrows, TestAmerica, Inc 

Comment 91.1 Andrea Rex, Massachusetts Water Resources Authority 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 112.1 Colin Elliot, King County Environmental Lab 

Comment 123 Vincent Sapienza, New York City Department of Environmental Protection 

Comment 169.1 Judith R. Morgan, American Council of Independent Laboratories 

Other comments: 

Comment 92 

Lee Wolf 

Columbia Analytical Services, Inc 

Approving method 624 for the determinative analysis of acrolein and acrylonitrile is a good proposal. 

But along with that, the preservation and holding time requirements in the current CFR MUR (2007) must 

be addressed. Currently the samples for acrolein and acrylonitrile must be preserved and pH 4-5, or 

analyzed within 3 days if not preserved. Our study shows that this is not necessary (data can be provided 

if desired). Also, for a “full” 624 analysis that includes acrolein and acrylonitrile and other volatiles, this 

also means that samplers must take two sets of samples and the lab must analyze the samples twice. This 

all represents added sample bottle, documentation, sampling, analysis, processing, and reporting costs that 

are unnecessary in consideration of data quality. The preservation and holding time for these analytes 

should be the same as other volatile organics by method 624. 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 

Comment: Table IC, Notes 4 & 5: EPA methods 624 and 625 may be used for additional compounds, 

including acrolein, acrylonitrile, benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, and Nnitrosodiphneylamine. This is a reasonable proposal; however, there are no published QC acceptance 

criteria in the methods for these compounds. Will the limits be published soon, or should a lab continue 

using the in-house historical limits for DOC, LCS and MS/MSD analyses or limits found in other 

approved methods for these analytes? Why isn’t the EPA revising methods 624 and 625 to include and 

address the changes? Additionally regarding Note 5: “....However, when they are known to be present, 

methods 605, 607, and 612, or method 1635 are preferred methods for these compounds”: How is 

“preferred” defined or to be interpreted from a regulatory Agency’s perspective? Additionally, is a 

permitted NPDES facility still in compliance if it continues using EPA method 625 as the quantitative 

method since other analytical methods may not be established in the facility’s laboratory or 625 is 

specified in their permit. 

Comment 98.1 

URS Corporation 
2010 Methods Update Rule Response to Comments 28 March 2012 

Table II should be revised from the draft version to include changes in preservation requirements for 

acrolein and acrylonitrile. It is difficult and burdensome to preserve samples in the field to the limited pH 

range specified (i.e., pH 4-5) for analysis of acrolein and acrylonitrile. Typically, analysis for acrolein and 

acrylonitrile is performed in conjunction with analysis of a larger list of volatile organic compounds (ex., 

the priority pollutant volatile list). In lieu of preserving the samples to a pH 4-5, another preservation 

option for acrolein and acrylonitrile is to collect an unpreserved sample and analyze within 3 days of 

collection. This option increases the analytical costs (laboratory analyzes a preserved and unpreserved 

sample if additional parameters are requested) as well as creates hardship on the laboratory to meet the 

accelerated hold time. Acrolein and acrylonitrile were included in a spiking study to assess preservation 

requirements for these compounds to alleviate these issues. 

Study Details: On behalf of DuPont, Lancaster Laboratories, Inc. of Lancaster, Pennsylvania, performed a 

volatile spiking study in preserved and unpreserved water samples. The compounds, acrolein, 

acrylonitrile, vinyl chloride, styrene, and 2-chloroethyl vinyl ether, were spiked at a concentration of 100 

ug/L into the following: 

 three preserved (with HCL to pH <2) deionized water samples 

 three unpreserved deionized water samples 

 three preserved (with HCL to pH <2) groundwater samples 

 three unpreserved groundwater samples 

Each of the 12 samples was analyzed every other day starting on Day 0 and ending on Day 16. With the 

exception of 2-chloroethyl vinyl ether in the preserved samples, acceptable recoveries (70-130%) were 

observed for all compounds in both matrices. As a result, we believe the preservation criteria for acrolein 

and acrylonitrile can be modified to read “Cool, ≤ 6°C18, 0.008% Na2S2O35, HCL to pH < 2” and the 

maximum holding time criteria be modified to read “14 days.” 2-chloroethyl vinyl ether, styrene, and 

vinyl chloride were also included in the spiking study to address an update to Table 4-1 of SW-846, 

Chapter 4, which calls for unpreserved samples for these three compounds. Since acceptable recoveries 

were observed in the preserved samples from Day 0 to Day 16 for acrolein, acrylonitrile, styrene, and 

vinyl chloride, we believe samples can be preserved with HCl to pH<2 and analyzed within 14 days. We 

do agree with EPA on submitting an unpreserved sample for the analysis of 2-chloroethyl vinyl ether. 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Section II.A.9 discusses the removal of footnote 4 for Method 624, We are in agreement with the removal 

of this footnote, EPA Method 8260B has been used for years to analyze acrolein and acrylonitrile with no 

confirmation, Since EPA Method 624 has the same technology and analytical procedures as EPA Method 

8260B, enough data has been generated over the years to support this. 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

Section II.A.9. While we believe that EPA method 624 can be optimized in a manner which allows the 

generation of quantitative analytical results for the compounds acrolein and acrylonitrile, we feel that 

offering a carte blanche approval at this time is premature. It appears from the summary that the removal 

of the screening restriction for these two analytes stems from comments made by a single laboratory, 

rather than a more rigorous multi-laboratory testing study. We do not deny that some laboratories are 

capable of producing quantitative results of acceptable quality for acrolein and acrylonitrile using EPA 

method 624. It is our experience, however, that this is only possible using specific modifications to the 
2010 Methods Update Rule Response to Comments 29 March 2012 

method, which should be required to be employed should a lab wish to use method 624 to produce 

quantitative results. 

 SW-846 method 8260B (1996), a much more recent version of this GC/MS method, clearly specifies that 

these two analytes are associated with poor purging efficiency. Method 8260 goes on to suggest that the 

use of azeotropic or vacuum distillation techniques is required to provide adequate response for these 

compounds. We note that neither of these sample introduction techniques is included as an “allowable 

modification” under 40 CFR Part 136.6 (b). 

If method 624 is to be allowed for general quantitative determination of these two analytes, we believe 

that performance criteria, including sample introduction technique, should be specified in a footnote to 

table IC. One suggestion would be to add the following language to the proposed revision to footnote 4 

in Table IC: Method 624 may be used for quantitative determination of Acrolein and Acrylonitrile, 

provided that the laboratory has documentation to substantiate the ability to detect and quantify these 

analytes at levels necessary to comply with any associated regulations. The use of sample introduction 

techniques in addition to simple purge and trap may be required. 

Section II.B New Standard Methods and New Versions of Approved Standard Methods 

EPA proposed to approve various new Standard Methods or new versions of approved Standard Methods. 

The proposal generated a large number of comments regarding those methods, and although this section 

of the original proposal did not include any subsections or other logical structural divisions, EPA has 

divided the comments received by topics, and presents the comment responses for each topic in 

subsections B.1 to B.10, below. 

II.B.1 General Support 

List of Comments: 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 107.1 - Patsy Root, IDEXX Laboratories 

Comment 108.1 - George Noguchi, U.S. Department of the Interior, U.S. Fish and Wildlife Service 

Comment 112.1 - Colin Elliot, King County Environmental Lab 

Comment 123 - Vincent Sapienza, Bureau of Wastewater Treatment, New York City Department of 

Environmental Protection 

Summary of Comments: Many commenters supported EPA’s proposal to limit the approved versions of 

Standard Methods to the most recent versions, although several were concerned about the resulting costs. 

One commenter expressed concern that listing the year published will lead to confusion about editions 

versus publication dates. 

Response: EPA thanks the commenters for their support. EPA has addressed the cost concerns in 

Section II.B.2 of this document. EPA has addressed the publication date confusion in Section II.B.3 of 

this document. 

Original Comment Text: 

The following commenters supported the proposal to limit the approved versions of Standard Methods to 

the most recent versions. 

Comment 91.1 Andrea Rex, Massachusetts Water Resources Authority 

Comment 107.1 Patsy Root, IDEXX Laboratories 

Comment 108.1 George Noguchi, U.S. Department of the Interior, U.S. Fish and Wildlife Service 

Comment 123 Vincent Sapienza, Bureau of Wastewater Treatment, New York City Department 

of Environmental Protection 
2010 Methods Update Rule Response to Comments 30 March 2012 

Other comments: 

Comment 112.1 

Colin Elliot 

King County Environmental Lab 

Comment: We agree that only the most recent version of a method should be approved for NPDES 

testing. We are concerned that listing only the year published will lead to confusion as to whether a 

particular SM edition # contains the most recent version. We would prefer that the most recent SM 

edition # be shown in 40 CFR 136.3 and that the year published be entered only for the on-line methods. 

II.B.2 Cost 

List of Comments: 

Comment 82 - LeeAnna Hutchings, Great Salt Bay Sanitary District Damariscotta, ME 

Comment 88.1 - Susan D. Hill, Wisconsin State Laboratory of Hygiene 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 95.1 - Robert B. Leventry, Butler County Water and Sewer Department Regulatory 

Compliance Team 

Comment 99.1 - Jennifer Marques, Linden Roselle Sewerage Authority 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 115 - L. Wentland, City of St. George, UT 

Comment 118 - Andrew G. Wendell, ClearWater Laboratory 

Comment 152.1 - James Matthews, On Line Environmental Inc (OLE) 

Comment 154.1 - Sharon Mertens, Milwaukee Metropolitan Sewerage District 

Comment 161.1 - Carol Batterton, Water Environment Association of Texas 

Comment 162.1 - Ed Saxon, South Carolina Water Quality Association 

Comment 177.1 - Novelle C. Stokes, South Central Wastewater Authority 

Summary of Comments: Many commenters objected to EPA’s proposal to limit the approved versions 

of Standard Methods to the most recent versions, based on the perceived cost for an on-line subscription 

to Standard Methods. Some commenters expressed concern that acceptance of the "most recent" version 

could mean "and not the older version anymore." 

Response: EPA refers readers to the discussion in section IV.A of the preamble to this rulemaking for 

additional information. 

“Standard Methods for the Examination of Water and Wastewater” (Standard Methods) is published by a 

consensus organization that is owned and managed by the three professional organizations (WEF, 

AWWA, and APHA) as a not-for-profit entity. There is no formal relationship between the consensus 

organization and EPA, and EPA as no direct managerial control over Standard Methods. EPA has no 

authority to require Standard Methods to provide free access to on-line methods. This also applies to 

other voluntary consensus standard bodies such as ISO, ANSI, ASTM, and AOAC. 

Publication of these methods is under the direct control of Standard Methods staff and their release to the 

general public occurs through either print or electronic format at the discretion of the Standard Methods 

staff. Charges for these methods, whether in print or electronic format, reflect the costs of the 

organization responsible for their publication. 

Dischargers may use any approved Part 136 method for compliance monitoring unless the method is 

specified in their discharge permit by the permitting authority, or the method is not sufficiently sensitive 
2010 Methods Update Rule Response to Comments 31 March 2012 

to comply with the permit limit. EPA is not requiring the use of any EPA-approved Standard Method in 

today’s rule. Electronic versions of a single method from Standard Methods On-Line generally cost $69. 

A subscription to Standard Methods On-Line costs $295 per year. However, such a subscription would 

allow one person in the laboratory to obtain all of the Standard Methods needed as a result of this 

rulemaking. The PDF files for the methods can be downloaded from the web site and saved “locally” to a 

computer or network at the laboratory. The local PDF files can be printed or accessed internally within 

the laboratory. Therefore, EPA does not agree with commenters that they will have to purchase an online subscription to Standard Methods, nor does EPA conclude that this change will present a significant 

financial burden to laboratories. 

Thus, EPA disagrees that more than one “seat” (subscription) would likely be required for small or large 

organizations. Further, given the timeframes involved in approval of new or revised methods for NPDES 

compliance monitoring, the subscription is not likely to need renewal for some time, since EPA generally 

updates methods at Part 136 approximately every 4-5 years. 

Regarding the concern that acceptance of the "most recent" version could mean "and not the older version 

anymore," see response in Section II.B.5. 

Original Comment Text: 

Comment 82 

LeeAnna Hutchings 

Great Salt Bay Sanitary District Damariscotta, ME 

Found on page 58029 it is being proposed that the most current edition of Standard Methods be the only 

one approved. To purchase an electronic version of the method or a copy of the book as often as it is 

published could be yearly. This would increase the financial burden to our 2 small facilities (being the 

book costs $250 and minimum online yearly access costs $295). Although newer editions have newly 

revised quality assurance and quality control procedures, the use of the data should be balanced against 

the need for greater accuracy. Newer QA/QC procedures do not always correspond to increased accuracy 

and even if the procedure increased accuracy minimally, would it justify the need to spend money on new 

procedures verses spending on a worthwhile expenditure such as the operation and maintenance our 

facilities? 

Comment 88.1 

Susan D. Hill 

Wisconsin State Laboratory of Hygiene 

Federal Register, 9/23/10, p. 58029: section B—many laboratories do not subscribe to Standard Methods 

On-line, and it would be financial hardship to do so. For our lab a minimum subscription (2-5 seats for 2 

years) would cost $678.00 every two years. Buying a printed book costs approximately $200.00, and is a 

much cheaper option. 

Comment 91.1 

Andrea Rex 

Massachusetts Water Resources Authority 

New Standard Methods. In addition to proposing a number of new or revised methods from the 

“Standards Methods” compendium, this section proposes to only approve the most recent version of a 

procedure from Standard Methods instead of approving versions from the 18th, 19th, 20th, or online 

compendia. While this is a considerable simplification it will result in a major effort and expense to 

laboratories when they need to purchase the most recent methods and ensure that the method being 
2010 Methods Update Rule Response to Comments 32 March 2012 

performed in their laboratory comports with the approved method. Overall this is probably a good change 

once laboratories go through this reconciliation process. 

Comment 95.1 

Robert B. Leventry 

Butler County Water and Sewer Department Regulatory Compliance Team 

The cost to purchase multiple "seats" for an online subscription to SM for our laboratory, operations and 

environmental staff would cost many times more than the single hardcopy edition we now share. Even if 

only one of our analysts subscribed to the online version, the subscription must be renewed every 1-2 

years which would essentially force us to pay for the same access multiple times versus a more cost 

effective hardcopy version that is approved and useful over many years. We found that hardcopy editions 

were currently used for this reason by all of the other local utility and commercial laboratories in our area 

that we contacted, including some who had subscribed in the past to the online version of Standard 

Methods. 

If 40CFR 136.3 changes to a method approval based on the publication year instead of the edition of SM, 

EPA needs to ensure that the regulated community has free or at least cost effective access to the 

methods. We suggest the solution for these concerns is for EPA to publish a cross reference chart to the 

currently approved online methods and make available the changes since the last approved hard copy 

edition. These references should be freely available on EPA's website. Alternatively, EPA could work 

with the Standard Methods Committee to make available to those having purchased hardcopy SM 

editions some cost effective way to access the updated online version of a method as approved in part 

136. This would allow all laboratories, whether they are local utilities such as ours or commercial labs, 

access to the information needed to meet Clean Water Act requirements. 

Comment 99.1 

Jennifer Marques 

Linden Roselle Sewerage Authority 

EPA is proposing to approve only the most recent version of a method published. Many of these methods 

will be from the 21st On-line edition of Standard Methods. As stated on the Standard Methods Committee 

website, www.standardmethods.org, access to the 21st on-line edition is by an annual subscription. 

Subscriptions are based on the number of seats that are needed. Each individual requiring access is 

considered one seat. The more seats required the greater the cost of subscription. The cost of one seat is 

$295.00 for a one year subscription. The requirement to subscribe on-line becomes a financial hardship 

on the small municipal laboratories especially when more than one seat is required per laboratory. 

It is also impractical and less accessible compared to the printed edition. Many of the municipal 

laboratories have limited or no internet access. Internet access may be only for the supervisor and not the 

laboratory technicians. Requiring the laboratory technicians to access the methods online would result in 

a need to purchase additional computers for the laboratories and provide internet connections to each 

computer. This imposes additional costs to the municipal labs at a time when everyone is being 

economically conservative. 

EPA approving the 21st edition printed compendium by Standard Methods would be the most practical 

and economically reasonable option at this time. 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 
2010 Methods Update Rule Response to Comments 33 March 2012 

There are many Standard Methods included in Tables IA, IB, and IH that are newer revisions than the 21" 

edition of Standard Methods and would require a subscription to Standard Methods to review the methods 

on-line. This is cost prohibitive for state certification programs and laboratories to review newly proposed 

methods. These methods should not be included in the proposed rule until the methods are made available 

in printed form for review or in a more cost effective manner. Also, there are still laboratories that do not 

have on-line access and would not be able to obtain these methods. Some examples of these methods are 

Fecal coliform, MPN by SM 9221 C E -2006, Total coliform, MPN by SM 9221 B -2006, E. coli by SM 

9223 B -2004, Trace Metals by ICP/MS by SM 3125 -2009, Hexavalent Chromium by SM 3500Cr 

C¬2009 and 3500Cr B -2009. 

Comment 115 

L. Wentland 

City of St. George, UT 

My concern is requiring labs, that run simple tests (like BOD, TSS, pH, TS, TDS, Turbidity, E. Coli), to 

have to use the most current version of Standard Methods will come at a cost of money to the taxpayer (of 

purchasing the new standards) and a cost of time (to revise the SOPs) to the lab. I do not see that the 

QA/QC will improve in relation to the cost involved. I prefer the EPA's practice of discarding methods as 

they become obsolete. 

Comment 118 

Andrew G. Wendell 

ClearWater Laboratory 

I am opposed to this change. While it may appear to streamline a reference for a given analytical method, 

I do not believe it is reasonable to expect every laboratory or wastewater facility to purchase a new 

version of Standard Methods on what would be potentially an annual basis. Where in most cases little (if 

any) of a given analyte’s source methodology would have changed, the onus of a lab or facility having to 

purchase the latest edition for the sake of owning the latest edition is both an inefficient use of resources 

as well as a source of potentially frivolous litigation over the semantics of which edition is used. This 

would also lead to confusion over when a given lab or facility must begin citing the new edition in lab 

reports, such as where a new edition becomes available but the lab has been certified using a previous 

edition for some time period that extends past the availability of the new edition. Another situation that 

could cause confusion is if a given method from a new edition of Standard Methods might not be 

considered to be acceptable by the EPA (due to decreased QA/QC method requirements, for example) this 

would either force the EPA to allow an undesirable method change, or still require a lab/facility to 

reference multiple or otherwise non-latest editions of Standard Methods which would violate the 

proposed regulation. It would be preferable for a laboratory or facility to refer to the most recent 

(approved) 40 CFR that outlines in table format which source method editions are considered acceptable. 

Comment 152.1 

James Matthews 

On Line Environmental Inc (OLE) 

We are also concerned about the requirement to use only the most recently approved methods approved 

by the Standard Methods Committee, as discussed on page 58028-9 of the proposed legislation. While 

we understand the desire and need for consistency, being able to only reference the most recent version of 

Standard Methods becomes problematic. As you may be aware, the State of South Carolina currently lists 

the method edition/version on the lab certification certificate issued by the state. The requirement to use 

only the most recently approved method would also require reissuance of the lab certificate for each 

revision. Would this require reapplication for certification for the laboratory with each revision as it is 

implemented? This could mean substantial backlogs for states issuing certifications. Additionally, once 
2010 Methods Update Rule Response to Comments 34 March 2012 

again smaller labs would be most adversely impacted by this requirement. In addition to more frequently 

revising lab standard operating procedures, the lab would also have to purchase printed versions of 

Standard Methods more frequently and/or subscribe to the on line version of Standard Methods. The 

proposed tracking requirements may force the need for each lab to implement a LIMS system or require a 

substantial increase in labor. For labs with limited budgets, this monetary commitment could further 

restrict how budget monies are distributed throughout the fiscal year. We would propose that you 

consider accepting the versions approved during the most recent five year period. This would require labs 

to stay abreast of current technology improvements and update their methods accordingly, as well as not 

create an undue financial and workload burden. 

Comment 154.1 

Sharon Mertens 

Milwaukee Metropolitan Sewerage District 

EPA is proposing to approve only the most recent version of a method published by the Standard 

Methods. This limitation will require labs to purchase the on-line version of Standard Methods, which is 

available only as an annual subscription costing a minimum of $404/year. This is a significant cost 

increase from the purchase of hard copy versions every few years when versions are updated. The 

concept of using the most recent version sounds like a good idea. We like to think that incorporating the 

latest technology and improvements is always a good thing. However, there are many times when the 

current method is perfectly adequate to meet the required specifications and there may be little, if any, 

improvement in data quality for the intended use. Method updates always require an investment by the 

laboratory. This includes the time required to review the new method, train analysts, validate the updated 

procedure, rewrite or update SOPs, benchsheets and other documentation. These may also require 

investment in new equipment. In many cases, these investments are fully justified by the added benefits 

of the new methods. However, where they are not, the laboratories should not be forced to change just for 

change sake. Cost and/or the market will drive labs to use the best available methods as appropriate. 

This should not be regulated. EPA should approve methods by reference and technology but not by 

version or date. EPA could and should encourage the use of the most recent version, however, the use of 

an earlier approved version should also be allowed if it meets the end use of the data. 

Comment 161.1 

Carol Batterton 

Water Environment Association of Texas 

EPA is proposing to revise how we identify approved methods that are published by the Standard 

Methods Committee. Currently in the tables at 136.3(a), EPA lists these methods in one or more columns 

as being in the 18th, 19th, 20th printed compendiums, or in the On-line editions published by the 

Standard Methods Committee. EPA identifies which versions are approved by the printed edition in 

which the method is published or, in the case of the electronic version of the method, by the last two 

digits of the year in which the method was published by the Standard Methods Committee (e.g., Standard 

Method 2320 B–97). In some cases, EPA has approved more than one version of a Standard Method. 

Approval of several versions of the same Standard Method has led to inconsistencies in how laboratories 

conduct these analyses especially in quality assurance/quality control (QA/QC) practices. For this reason, 

EPA is proposing to approve only the most recent version of a method published by the Standard 

Methods Committee with as few exceptions as possible by listing only one version of the method with the 

year of publication designated by the last four digits in the method number (e.g., Standard Method 2320 

B–1997). This change allows use of a specific method in any edition that includes a method with the same 

method number and year of publication." WEAT’s comment: Standard Methods is a compendium of 

methods with the general QC requirements stated in Part 1000 and section XX20 of each Part. Most 

organizations are aware that if you are using a method in the 21st edition of Standard Methods, you must 

follow the Quality Control requirements of the 21st edition. For consistency, most labs utilize the same 
2010 Methods Update Rule Response to Comments 35 March 2012 

edition of Standard Methods for all their methods. With switching to the new format, it may be more 

confusing for labs to determine which quality control procedures they are supposed to follow. The new 

requirement to use the most recent version of a method is practically forcing labs to subscribe to the online edition of Standard Methods as the most recent version of a method is usually on-line years before 

they are published in hardcopy. The least expensive subscription to on-line Standard Methods is 

$404/2years. This will be cost prohibitive for many of the small water and wastewater laboratories. 

Comment 162.1 

Ed Saxon 

South Carolina Water Quality Association 

Additionally, once again smaller labs would be most adversely impacted by the requirement to use only 

the most recently approved methods. In addition to more frequently revising lab standard operating 

procedures, the lab would also have to purchase printed versions of Standard Methods more frequently 

and/or subscribe to the online version of Standard Methods. The proposed tracking requirements may 

force the need for each lab to implement a L1MS system or require a substantial increase in labor. For 

labs with limited budgets, this monetary commitment could further restrict other critical needs for data 

generation and management throughout each fiscal year. SCWQA proposes that EPA consider accepting 

the versions approved during the most recent five year period. This would require labs to stay abreast of 

current technology improvements and update their methods accordingly, but not create an undue financial 

and workload burden. 

Comment 177.1 

Novelle C. Stokes 

South Central Wastewater Authority 

Comment: Newly revised Standard Methods are only available online via www.StandardMethods.org 

which requires a costly online membership. Annual membership fees start at $295 and increase based on 

the number of users needing access. Our 5 member laboratory would cost $495 per year just to have 

access to method texts and updates. As proposed, these method revisions would be approved as soon as 

released and therefore require immediate compliance within the laboratory. 

No other approved method source requires such outrageous fees for cited method texts. Why would the 

Agency indiscriminately approve methods from such a for-profit source? 

Recommendation: EPA should limit its approval of analytical methods to those that are available to the 

public free of charge. The idea that a municipal laboratory be required to purchase the rights to simply 

view an approved method is contrary to the Agency’s objective to encourage public participation in the 

fight to protect out natural resources. The agency’s apparent preferential endorsement of the Standard 

Methods Committee and vendors within the regulatory text implies a lack of impartiality. 

II.B.3 Version Confusion 

List of Comments: 

Comment 88.1 - Susan D. Hill, Wisconsin State Laboratory of Hygiene 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 95.1 - Robert B. Leventry, Butler County Water and Sewer Department Regulatory 

Compliance Team 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 124.1 - Thomas Tourje, Augusta County Service Authority 
2010 Methods Update Rule Response to Comments 36 March 2012 

Comment 134.1 - Josh Kathrinus, American Bottoms Regional Wastewater Treatment Facility 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 189.1 - William Ray, California State Water Resources Control Board 

Summary of Comments: Many commenters noted disconnects with the way that Standard Methods are 

identified in the hardcopy editions of the methods manual, in the on-line version at the Standard Methods 

web site, and in the tables of approved methods at 40 CFR 136. Commenters expressed concerns about 

the ability to unambiguously identify the approved version of a given method and the effects of the 

different method identification systems on various aspects of laboratory practice. Several commenters 

were concerned about the specific language in this section referring to “published” methods as opposed to 

“approved” methods. One commenter wanted the year tag to be reduced to the latter 2 digits for 

consistency with Tables IC and ID, 40 CFR part 141, and ASTM methods. 

Response: EPA recognizes that there are multiple meanings of the word “approved” and takes care to be 

clear and to distinguish those meanings in its rulemakings. For example, Standard Methods are identified 

by the year in which they were “approved” for publication by the Standard Methods consensus body (e.g., 

SM 3113-2004 was approved by the Standard Methods Committee in 2004). The year of approval by 

Standard Methods is retained until the method is reviewed (and potentially revised). Standard Methods 

may choose to update a chapter. If no change is made to the chapter, the method number remains the 

same, but the date changes (e.g., XXXX-2000 will change to XXXX-2011). Similarly, if any change is 

made to the method, the date also changes. The new approval date is shown in both the book format and 

the on-line format when Standard Methods "approves" the method. However, “approval” by that 

committee does not reflect any regulatory significance at part 136 or elsewhere. The Agency must 

propose any updated version of a Standard Method in the Federal Register and provide the opportunity for 

public comment on the updated version before the method is approved at part 136 for use in wastewater 

regulatory programs. 

If the version of a Standard Method that EPA has “approved” for use in compliance monitoring and listed 

in part 136 was “published” by Standard Methods at a later date than the version in the most recent hard 

copy edition of Standard Methods that you have, you may need to purchase that method from the on-line 

version of Standard Methods, at a cost of $69 per method. The hard copy edition generally lags and is not 

available as quickly as the on-line version. Methods may be purchased individually for less than the cost 

of a full subscription to the on-line service or of the most recently published print edition of Standard 

Methods. 

The Standard Methods committee has taken additional steps to clarify how Standard Methods are 

identified in various hardcopy editions and online. Methods will denote “EPA NPDES Approved” on the 

printed hardcopy and on-line version of the method. 

EPA also refers readers to section IV.A of the preamble to this rulemaking. 

Original Comment Text: 

Comment 88.1 

Susan D. Hill 

Wisconsin State Laboratory of Hygiene 

Federal Register, 9/23/10, p. 58029: section B—“EPA is proposing to approve only the most recent 

version of a method published by the Standard Methods Committee. . .by listing only one version of the 

method with the year of publication designated by the last four digits in the method number.” Do you 

really mean the year of approval by the Standard Methods Committee? An example of why this is 

confusing follows: in the 21st printed edition, published in 2005, method 3113 is published with a 
2010 Methods Update Rule Response to Comments 37 March 2012 

footnote that says, “Approved by Standard Methods Committee, 1999.” So would this method be 

designated 3113-1999 or 3113-2005? There is also an on-line version, 3113 approved in 2004, which I’m 

assuming would be designated 3113-2004. Without access to Standard Methods On-line, we have no way 

of knowing if 3113 published in the 21st edition in 2005 is OK to use. 

Table IB—SM 3113-1999 is approved for some parameters (e.g. Sb, Cd, Cr, Fe, Pb, Ag), while SM 3113-

2004 is approved for other parameters (e.g. As, Ba, Be, Co, Cu, Mn, Mo, Ni, Se, Tl, Vn). It is 

unreasonable to expect a lab to run two different versions of the same method for different parameters. It 

would be better to approve one version of SM 3113 for all applicable parameters. 

All places SM 3113 is listed in Table IB have been revised to list SM 3113-2004 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 

Comment: In Table IB, Standard Methods 5210B-2001 is listed as one of approved test procedures. 

However, in Standard Methods Online both 5210 BOD and 5210 BOD (20th Ed) are listed. Which online 

BOD method is approved in the 2010 MUR (or are both)? The approved BOD method is 5210-2001. 

Comment 95.1 

Robert B. Leventry 

Butler County Water and Sewer Department Regulatory Compliance Team 

BCWS commends the United States Environmental Protection Agency's efforts to gather stakeholder 

input for the revision of the rules. It is important that all views are considered by EPA when making 

regulatory changes so unintentional consequences can be avoided and workable solutions to 

implementation problems can be achieved. 

FR pages 58028 and 58029 In the preamble Section II B, EPA proposes to change the way in which 

approved methods published by the Standard Methods Committee are identified. BCWS is not opposed to 

this change however we do have the following concerns regarding the implementation of this proposal: 

Standard Methods (SM) hardcopy editions currently have the approval date printed as a footnote to either 

the section or the specific method which would allow us to determine the correct method as outlined in 

the proposed rule. However, since we do not have access to an online subscription to SM, in some cases 

we have no way to determine the differences between the proposed approved method referenced in SM 

online and the hardcopy version we are currently using. 

For example in table IA of the currently approved CFR part 136.3, the method for E. coli using MPN is 

9223 B in the 20'h edition of SM. This method has a reference to the original publication year of 1997. In 

the proposed rule, the approved version of the method is listed as the year 2004. Since SM 21" hardcopy 

edition also references the 1997 publication date, we assume that the reference to 2004 is for a SM online 

method to which we don't have access. 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

Section II.B, Tables IA, IB, and IH address the approved methods for inorganic and microbiological test 

procedures and more specifically the approval of only the most recent edition of Standard Methods, It is 

agreed that having multiple editions approved causes inconsistencies across the laboratory community. It 
2010 Methods Update Rule Response to Comments 38 March 2012 

also causes problems with the certification of laboratories since each method may vary between editions 

and we must evaluate laboratories according to the edition they are referencing. The approval of one 

approved Standard Method for each parameter will help solve the inconsistencies between laboratories 

and will aid in the certification of laboratories in being able to hold the laboratories to one approved 

method. Also, it is our understanding that when Standard Methods issues a new revision of a method, it 

contains improvements to the method. However, there are two comments we would like to make in 

regards to this change: 

a) The method should not be listed with a 4 digit year, e.g., 2006, Instead, the Standard Methods should 

be listed with the last two digits of the approval year, e.g., 06, This will provide consistency with Tables 

IC and ID for organics which only list the last two digits of the year. This will also provide consistency 

with the format of the SDWA (40 CFR Part 141) method listings as well as ASTM methods, 

b) There are instances where Standard Methods has rereleased a method without significant changes or 

improvements. An instance of this would be the phenol methods SM 5530B and D. The newly proposed 

2005 revisions do not significantly differ from the 2000 revisions. The 2005 revision is only available online whereas the 2000 method is available in the 21" Edition of Standard Methods. Releasing new 

revisions without significant changes or improvements unnecessarily increases costs to all laboratories 

and regulatory authorities when there is relatively no difference between the two revisions. 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

“EPA is proposing to approve only the most recent version of a method published by the Standard 

Methods Committee. . .by listing only one version of the method with the year of publication designated 

by the last four digits in the method number.” While we fully support the idea of approving only a single 

version/edition of any Standard Methods procedure, we equally feel that the proposal lacks clarity and 

needs to be more carefully considered. 

The proposal states that a Standard Methods Procedure would be identified by listing only one version of 

the method with the year of publication designated by the last four digits in the method number (e.g., 

Standard Method 2320 B–1997). If the proposal were as stated, it might be less confusing to users; 

however, it does not appear that the last 4 digits codified reflect the “year of publication”. In the example 

above, “1997” would indicate the year of publication. Since the 19th edition of Standard Methods was 

published in 1995, and the 20th edition published in 1998, there is no edition of Standard Methods 

associated with a publication date of 1997. Our assessment of the proposed rule suggests that the “year”, 

as discussed in rule, actually reflects the year in which a particular method was approved by the Standard 

Methods Committee, which is of no relevance to any end user. 

Since purchasing new methods, or on-line subscriptions, poses a significant financial burden to smaller 

regulated facilities, it seems reasonable that end users should be able to quickly ascertain whether the 

copy of a particular method they own in a published edition of Standard Methods reflects the identical 

method approved in 40 CFR Part 136. As an example, we offer the procedure for Total Suspended 

Solids, SM 2540D, which is referenced and utilized by nearly every regulated wastewater treatment 

facility in Wisconsin. The proposed rule would identify “2540 D–1997” as the solitary approved 

Standard Method procedure for this determination. A small lab owns hard copies of Standard Methods 

19th (published 1995) and 20th (published 1998) editions and wants to know if one of these is the same as 

“2540D-1997”. Only in the on-line edition would the analyst find the notation, “Approved by Standard 

Methods Committee, 1997“. If the on-line edition is compared to the version in the 20th edition, however, 

one finds they are identical. The analyst should then be able to utilize their existing version. 
2010 Methods Update Rule Response to Comments 39 March 2012 

In short, the proposed rule lacks clarity which could be resolved by publishing a table which lists, for a 

given Standard Method cited in 40 CFR Part 136, any version(s) of the method in a printed 

version/edition of Standard Methods deemed equivalent because revisions have not been made. In the 

example provided, printed versions of method 2540D found in either the 20th or 21st editions should be 

equivalent to the on-line method published in rule. 

Comment 124.1 

Thomas Tourje 

Augusta County Service Authority 

 “For this reason, EPA is proposing to approve only the most recent version of a method published by the 

Standards Method Committee......” 

Comment: Should this specify the most recent approved version of a method published by the Standards 

Method Committee? 

Recommendation: Include the word “approved” in the sentence. 

Comment 134.1 

Josh Kathrinus 

American Bottoms Regional Wastewater Treatment Facility 

Standard Methods (SM) online has several method versions listed for a single method. In addition, the 

version of the method is not viewable at the link, rather it is found in the footers of the pdf file after 

maneuvering through the SM website and downloading the pdf. This is true for BOD, temperature and 

chromium at least. This could be a cause for confusion as to what method is approved or if all are 

acceptable. Unapproved methods should not be part of the selection. 

Comment 164.1 

Mark Haley 

Hopewell Regional Wastewater Treatment Facility 

Approved methods are listed by publication date rather than Standard Method edition number. Some 

approved methods are currently not available in hard copy and only can be obtained online. 

Comment: The change to approval by publication date introduces several problems including unclear 

requirements, lack of traceability and complications relating to laboratory accreditation. Currently 

laboratories use, report data, and are accredited by SM method numbers, including the edition. Changing 

40CFR citations from edition number to publication date will impact data management systems, 

accreditation data bases, PT provider data reporting systems, and regulatory programs. 

Recommendations 

For Standard Methods, cite methods based on edition number and date and clearly associate the QA/QC 

section required for each method. Recommend to Standard Methods consensus body to include QA/QC 

requirements within cited methods. 

Comment 189.1 

William Ray 

California State Water Resources Control Board 
2010 Methods Update Rule Response to Comments 40 March 2012 

In all prior versions of 40CFR 136.3, methods from Standard Methods for the Examination of Water and 

Wastewater (Standard Methods) have been based on a print edition number. In this proposal, EPA 

intends to list methods from Standard Methods based on the year of approval by a Standard Methods 

committee. Finding methods by approval year is most efficacious when using the online portal to 

Standard Methods (www.standardmethods.org). However, most have not used Standard Methods online 

because of costs as the purchase price for 4 method sets is very near the cost of one print copy. 

Permitting authorities have not invested in online copies of methods and like others have invested in more 

than one print edition. Eventually both parties will have to decipher which approved method belongs in 

which print version. In addition, at least 2 dozen methods are not in any print version, some as new as 

2009. And one method for cadmium is the 1990 version, which is not available online and is found only 

in the 19th edition print version. 

II.B.4 Default Approval Concerns 

List of Comments: 

Comment 106.1 - Charles Boepple, Upper Occoquan Service Authority 

Comment 109.1 - Andre Brousseau, Maine Wastewater Control Association 

Comment 116.1 - Wendy Harding and Mala Burton, Joint Virginia Water Environment Association and 

Virginia American Water Works Association 

Comment 124.1 - Thomas Tourje, Augusta County Service Authority 

Comment 126.1 - Sterling Pierce, Maine Department of Environmental Protection 

Comment 171.1 - Lola Guerra, Henrico County DPU 

Comment 177.1 - Novelle C. Stokes, South Central Wastewater Authority 

Summary of Comments: Several comments expressed concern that EPA’s language about using the 

“most recent” version of a Standard Method would lead to default approval of any newly published 

Standard Methods without suitable review and public comment. 

Response: Approval of any method used for CWA regulatory compliance requires that the methods go 

through the formal rule-making process, including publication of a proposal in the Federal Register for 

public comment, as is the case with today’s rulemaking. This requirement applies to methods contained 

in Standard Methods (in print editions or the on-line version). EPA apologizes for any confusion in the 

language in the proposal, and states categorically that approval of a method by the Standard Methods 

Committee does not automatically imply approval by EPA for use in Clean Water Act compliance 

monitoring. 

The approved methods are those listed in Tables IA to IH of 40 CFR part 136.3. 

Original Comment Text: 

Comment 106.1 

Charles Boepple 

Upper Occoquan Service Authority 

Comment I: It is unclear whether EPA intends to automatically approve future updated versions of the 

methods once the Standard Methods committee approves a new version or if only the specific version 

listed in Table IA or Table IB is approved. Will laboratories need to change methods as each method is 

updated? 

Recommendation I: Please clarify whether the most recent version of a method is a) that method version 

which appears in Tables IA and IB of the September 23, 2010 proposed rule, or b) the most recent version 

of the method as published in future editions of Standard Methods. 
2010 Methods Update Rule Response to Comments 41 March 2012 

Comment 109.1 

Andre Brousseau 

Maine Wastewater Control Association 

It is our understanding from reading the proposal that EPA desires to approve any and all corrections and 

description revisions made to methods published in the "Standard Methods for the Examination of Water 

and Wastewater" before the time this proposed rule is final. 

Does EPA intend to pre-approve changes that have not been published in the Federal Register for public 

review and comment prior to EPA's adoption? 

Maine Wastewater Control Association (MWWCA) believes that unless a method is subject to full and 

thorough scientific rigor, peer review, and then "set in stone," precision, accuracy and repeatability will 

suffer. Will the most recently published hard cover edition of "Standard Methods for the Examination of 

Water and Wastewater," that will be available at the time the rule is final, be accepted as most current, 

where applicable according to method number and year, and other method references, including Quality 

Assurance and Control requirements? 

Many, if not most, municipal and publicly owned treatment works (POTWs) that do self-monitoring use 

methods published in "Standard Methods for the Examination of Water and Wastewater," as approved by 

the EPA in 40 CFR 136.3. MWWCA is concerned that the proposal by EPA, to require use of "current" 

methods, will give de facto approval to changes "republished" independently by the Standard Methods 

Committee, as published "online," even after the proposed rule is final. Will permittees and other 

laboratories performing permit required monitoring, using EPA approved "Standard Methods," be 

expected to purchase subscriptions to "Standard Methods Online" (at $295 per year per seat) to meet 

EPA's definition of current? 

If EPA is indeed planning to approve "online" versions of approved methods, as updated independently 

and without opportunity for public participation, such a rule would be in conflict with current federal 

policies and legal principles regarding public participation and freedom of assembly, and also be a great 

burden of cost to many small entities. Allowing use of independently updated methods would require 

expensive subscriptions to an online service or other types of constant vigilance in trying to determine 

what EPA has approved as "current." 

We believe that the EPA must assure the public's right to know by only approving methods and quality 

control and assurance requirements that are available on the day of publication of the final rule, and that 

this is clear in the final rule. MWWCA requests that, in the final rule, the EPA clearly state its intent 

regarding public access to decisions regarding any changes to 40 CFR 136, and that EPA should clearly 

define the term "current" as regards this rule. 

The need to know the most current method does not fall only on direct dischargers, but also on indirect 

dischargers subject to the National Pretreatment Program. While corrections of errors and changes in 

descriptions of methods and quality control may seem insignificant to the EPA, they may become very 

significant for pretreatment inspectors who must review laboratory reports submitted by significant 

industrial users, and who must also confirm that the correct method is being followed. How will these 

POTWs need to document that the most current method was used and that all necessary current quality 

control and assurance was done? As of today, pretreatment programs most often rely on the laboratory 

reported method for a parameter, and State certification of that laboratory for testing that parameter, to be 

sure the test was done in accord with 40 CFR 136. How will individual POTWs assure that laboratories 

are performing the most current method approved by EPA in 40 CFR 136, if the approval date is a 

moving target? How much information will have to be collected with each laboratory report of analysis 

to make sure the information submitted is "legally defensible"? MWWCA believes that EPA approval of 
2010 Methods Update Rule Response to Comments 42 March 2012 

any method changes past the day of the publication of the final rule would be an unacceptable regulatory 

and economic burden on the POTWs with pretreatment programs, and that this would severely impact 

effective enforcement of the Clean Water Act. 

Maine has authority to implement and enforce the Clean Water Act, as a NPDES delegated State. The 

Maine Department of Environmental Protection (DEP) is charged oversight of POTW laboratories doing 

the self-monitoring described above, and requires that the testing be done according to a selected method, 

as approved by the EPA in 40 CFR 136.3 when available, and that the laboratory has quality control and 

assurance measures necessary to validate its data. Major and selected minor permittees under the Maine 

Pollutant Discharge Elimination System (MEPDES) program are required to participate in the annual 

Discharge Monitoring Report-Quality Assurance (DMR-QA) study program. 

As discussed in another part of our comments, most municipal and publicly owned treatment works 

(POTWs) that do self-monitoring use methods published in "Standard Methods for the Examination of 

Water and Wastewater," as approved by the EPA in 40 CFR 136.3. MWWCA is concerned that the 

proposal by EPA, to require use of "current" methods, will give de facto approval to changes to quality 

control and assurance recommendations that are "republished" independently by the Standard Methods 

Committee, following publication of the final rule. If this is indeed EPA's intent, then MWWCA requests 

that EPA provide all affected parties, including small entity permittees and their laboratories, with 

sufficient time to find and incorporate these changes into their standard operating procedures. MWWCA 

believes that sufficient time is two years from the date of publication. 

Comment 116.1 

Wendy Harding and Mala Burton 

Joint Virginia Water Environment Association and Virginia American Water Works Association 

Proposed Change: “For this reason, EPA is proposing to approve only the most recent version of a 

method published by the Standards Method Committee......” 

Comment 1: It is unclear whether EPA intends to automatically approve future updated versions of the 

methods once the Standard Methods committee approves a new version or if only the specific version 

listed in Table IA or Table IB is approved. Will labs need to change methods as each method is updated? 

Recommendation 1: Please clarify whether the most recent version of a method is a) that method version 

which appears in Tables IA and IB of the September 23, 2010 proposed rule, or b) the most recent version 

of the method as published in future editions of Standard Methods . 

Comment 124.1 

Thomas Tourje 

Augusta County Service Authority 

Comment: It is unclear whether EPA intends to automatically approve future updated versions of the 

methods once the Standard Methods committee approves a new version or if only the specific version 

listed in Table IA or Table IB is approved. Will labs need to change methods as each method is updated? 

Please clarify whether the most recent version of a method is a) that method version which appears in 

Tables IA and IB of the September 23, 2010 proposed rule, or b) the most recent version of the method as 

published in future editions of Standard Methods. 

Recommendation: The EPA proposal to approve only the most recent version of a method published by 

the Standards Method Committee remains a confusing area and little appears to be resolved as methods 

from several SM Editions are still being cited. The cost in manpower, of researching and updating all 

SOPs to reflect one SM version amongst many is going to be significant. Please leave direct citing of the 

SM 18th - 21st Edition in table IB. 
2010 Methods Update Rule Response to Comments 43 March 2012 

Comment 126.1 

Sterling Pierce 

Maine Department of Environmental Protection 

Maine DEP understands from the review of this proposal that EPA desires to approve any and all 

corrections and description revisions made to the methods published in the “Standard Methods for the 

Examination of Water & Wastewater” before this rule is finalized. Will this be the only time that this will 

be done without a public review and comment period? Will the latest hardcover edition of Standard 

Methods be accepted as the most current compilation of the requirements of the various methods 

contained within, or will license holders and commercial laboratories be required to purchase a 

subscription to Standard Methods online in order to keep up with the most recently method 

modifications? 

Comment 171.1 

Lola Guerra 

Henrico County DPU 

Proposed Change: “For this reason, EPA is proposing to approve only the most recent version of a 

method published by the Standards Method Committee......” 

Comment 1: It is unclear whether EPA intends to automatically approve future updated versions of the 

methods once the Standard Methods committee approves a new version or if only the specific version 

listed in Table IA or Table IB is approved. Will labs need to change methods as each method is updated? 

Recommendation 1: Please clarify whether the most recent version of a method is a) that method version 

which appears in Tables IA and IB of the September 23, 2010 proposed rule, or b) the most recent version 

of the method as published in future editions of Standard Methods. 

Comment 177.1 

Novelle C. Stokes 

South Central Wastewater Authority 

Comment: It is unclear whether EPA intends to automatically approve future updated versions of the 

methods once the Standard Methods committee approves a new version or if only the specific version 

listed in Table IA or Table IB is approved. Will labs need to change methods as each method is updated? 

Recommendation: Please clarify whether the most recent version of a method is a) that method version 

which appears in Tables IA and IB of the September 23, 2010 proposed rule, or b) the most recent version 

of the method as published in future editions of Standard Methods. 

II.B.5 Quality Assurance/Quality Control (QA/QC) 

List of Comments: 

Comment 78 - Brenda Bamett, Quality Program Manager, REI Consultants, Inc. 

Comment 106.1 - Charles Boepple, Upper Occoquan Service Authority 

Comment 116.1 - Wendy Harding and Mala Burton, Joint Virginia Water Environment Association and 

Virginia American Water Works Association 

Comment 124.1 - Thomas Tourje, Augusta County Service Authority 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 177.1 - Novelle C. Stokes, South Central Wastewater Authority 
2010 Methods Update Rule Response to Comments 44 March 2012 

Summary of Comments: Commenters expressed concerns about deciding the appropriate QA/QC 

requirements that match the EPA-approved version of a Standard Method without identifying the edition 

of Standard Methods. Three of the commenters recommended that EPA continue to approve any version 

of a method in the 18th through 21st edition of Standard Methods. 

Response: In response to the concern about the applicable QA/QC requirements, beginning with the 

publication of the 20th edition of Standard Methods, the Standard Methods Committee included the 

quality control (QC) procedures which are similar to the QC procedures that have been included by EPA 

in methods published over the last two decades for use in compliance monitoring programs under the 

Clean Water Act and the Safe Drinking Water Act. These procedures are specified in Part 1000 of the 

Standard Methods compendium and include the “essential” quality control checks that have been added at 

40 CFR part 136.7 as part of this final rule (see Section II.I of this document). To improve consistency, 

laboratories performing any of the approved Standard Methods should adopt the QC procedures specified 

in the 20th or 21st edition of the hardcopy Standard Methods or in the on-line version of Standard 

Methods. These versions of Standard Methods contain similar QC procedures. Hence, EPA opted to 

approve the newer versions of these Standard Methods and withdraw approval of most older versions. 

EPA disagrees that approval of only these later versions will lead to confusion because the new approach 

clearly identifies the version of the standard approved under Part 136 by the year of approval (e.g., 

Standard Method 3113-2004) and no longer ties the method to a particular printing or edition of Standard 

Methods. 

Original Comment Text: 

Comment 78 

Brenda Bamett 

Quality Program Manager, REI Consultants, Inc. 

I feel the change to list the approved Standard Method followed by the year of publication to be very 

burdensome in deciding the appropriate QC to match with each method. Each version of Standard 

Methods has improved upon the QC/QA practices. But when the date of an approved method lists a date 

that does not specifically line up with a given edition of Standard Methods and which in some cases spans 

various editions - I personally am at a loss to determine which edition’s QC is required by my 

laboratories. I believe a preferred method would be to list the earliest edition that approved QC can be 

found in....for example instead of SM2320B-1997 use the notation SM2320B 20th edition which lets me 

know that 18th or 19th editions do not contain the prescribed QC, but I can use 20th, 21st or online and 

meet or exceed the EPA QC/QA requirement for that method. 

Comment 106.1 

Charles Boepple 

Upper Occoquan Service Authority 

Part 1000 of Standard Methods (which covers many QA/QC subjects) does not have an "approval date" 

tied to it. Since the methods in tables IA and IB include methods that were first released in either the 20th, 

21st, or on-line versions of Standard Methods, it is unclear as to which Part I000 is appropriate (e.g. 

4500-CI-B¬1997 first appeared in the 20th Edition). This would undoubtedly lead to laboratory confusion 

in implementation since there are potentially three different Part 1000 sections that could be applied. 

We recommend that EPA continue to allow the use of all currently approved versions of Standard 

Methods as listed in 40CFR136 (i.e. 18th -21st Editions) 

Comment 116.1 

Wendy Harding and Mala Burton 
2010 Methods Update Rule Response to Comments 45 March 2012 

Joint Virginia Water Environment Association and Virginia American Water Works Association 

Part 1000 of Standard Methods (which covers many QA/QC subjects) does not have an “approval date” 

tied to it. Since the methods in tables IA and IB include methods that were first released in either the 

20th, 21st, or on-line versions of Standard Methods, it is unclear as to which Part 1000 is appropriate (e.g. 

4500–Cl- B–1997 first appeared in the 20th Edition). This would undoubtedly lead to laboratory 

confusion in implementation since there are potentially three difference Part 1000 sections that could be 

applied. 

For example; Flame Metals Method 3111B for 18th edition (this is a method for 27 metals listed): 

Besides the overview given in Section 1020B, requirements for CCV, Matrix Spikes and LCS appear at 

the end of 3020, blanks are in 3030D, calibration curves are discussed in 3020 and again in 3111B 4 c 

(which supersedes 3020) and spike frequency is covered in 3111A 7 with recovery and precision limits in 

Table 3111: III. Paragraph 7 lists an acceptable recovery as 85-115% as in 3020; however the table 

which is from ASTM (with permission) gives specific ranges for each individual metal ranging from .4-

12.5%. Also, only 17 metals are listed. Additionally, other tidbits are scattered throughout the method 

section including modifiers (3111B 4 a), recommended concentration ranges for calibration (Table 3111: 

I), and standards preparation (3111 A 5 and 3111B 3 j). 

We recommend that EPA continue to allow the use of all currently approved versions of Standard 

Methods as listed in 40CFR136 (i.e. 18th -21st Editions). 

Comment 124.1 

Thomas Tourje 

Augusta County Service Authority 

Part 1000 of Standard Methods (which covers many QA/QC subjects) does not have an “approval date” 

tied to it. Since the methods in tables IA and IB include methods that were first released in either the 

20th, 21st, or on-line versions of Standard Methods, it is unclear as to which Part 1000 is appropriate (e.g. 

4500–Cl- B–1997 first appeared in the 20th Edition). This would undoubtedly lead to laboratory 

confusion in implementation since there are potentially three different Part 1000 sections that could be 

applied. \ 

We recommend that EPA continue to allow the use of all currently approved versions of Standard 

Methods as listed in 40 CFR Part 136 (i.e. 18th - 21st editions). 

Comment 132.1 

Paula Hogg 

Hampton Roads Sanitation District 

Approved methods are listed by publication date rather than Standard Method edition number. Some 

approved methods are currently not available in hard copy and only can be obtained through Standard 

Methods on-line. 

Comment: The change to approval by publication date introduces several problems including unclear 

requirements, lack of traceability and complications relating to laboratory accreditation. 

Currently laboratories use, report data and are accredited by Standard Methods (SM) method numbers, 

including the edition. Changing 40 CFR citations from edition number to publication date will impact 

data management systems, accreditation data bases, PT provider data reporting systems, and regulatory 

programs. Currently, all QC requirements are not included in individual methods and therefore are not 

always consistent with method publication dates. Therefore it is unclear which QA/QC requirements are 
2010 Methods Update Rule Response to Comments 46 March 2012 

to be followed. On-line Methods and QC sections are not advancing on the same timeline so method and 

QA/QC requirements are not aligned. 

Overall, moving to newer methods is supported but changing the way methods are cited will cause 

extensive confusion based on the way Standard Methods publishes methods. Currently, there is no clear 

mechanism to track publish date to source or clear requirements for QA/QC for all methods. 

Recommendation 

For Standard Methods, cite methods based on edition number and date and clearly associate the QA/QC 

section required for each method. Recommend to Standard Methods consensus body to include QA/QC 

requirements within cited methods. 

Comment 177.1 

Novelle C. Stokes 

South Central Wastewater Authority 

The Agency’s objective to reduce confusion and to improve local enforcement of method standards is 

commendable. However, taking the action described threatens to do just the opposite. EPA’s assumption 

that each successive modification of a particular Standard Method carries with it legitimate and justifiable 

QA/QC measures is presumptive and shortsighted. 

The necessity for standardized methodology both in the laboratory and between them is clear, however 

such consistency should be mandated in a more simplistic sense to avoid overly burdensome requirements 

which often force abandonment of a preferred method altogether. We recommend the Agency consider 

holistically listing minimum QA/QC components before each parameter table based on the testing type 

(Biological Methods, Inorganic Test Procedures, Non-Pesticide Organic Compounds, etc.). The 

determination that further quality control measures are needed would then be the responsibility of 

individual laboratories in conjunction with their own accrediting agency. 

II.B.6 Alternate Test Procedures (ATPs) 

List of Comments: 

Comment 106.1 - Charles Boepple, Upper Occoquan Service Authority 

Comment 116.1 - Wendy Harding and Mala Burton, Joint Virginia Water Environment Association and 

Virginia American Water Works Association 

Comment 124.1 - Thomas Tourje, Augusta County Service Authority 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 177.1 - Novelle C. Stokes, South Central Wastewater Authority 

Summary of Comments: Several commenters questioned the effects of specifying the most recent 

version of a Standard Method on any alternate test procedures that were previously tested and approved 

based on an older version of the Standard Method. Concerns ranged from the effects on commonly used 

vendor-developed ATPs, to the appearance of a contradiction in how Standard Methods and ATPs are 

handled. 

Response: Withdrawal of the earlier approved versions of Standard Methods is not intended to affect the 

acceptance of any vendor-developed methods that were previously determined to be acceptable versions 

of those methods. Such Standard Methods were not withdrawn due to technical deficiencies. Rather, the 

Standard Methods were revised to improve clarity, increase method flexibility (e.g., use of a different 

solvent), or improve QC procedures, but the underlying technology was not changed. Therefore, the basis 
2010 Methods Update Rule Response to Comments 47 March 2012 

for the original ATP approval is still valid and the vendor-developed methods determined to be acceptable 

version of those methods continue to be approved for Clean Water Act monitoring. 

Original Comment Text: 

Comment 106.1 

Charles Boepple 

Upper Occoquan Service Authority 

Comment 2: Will methods (e.g. Hach) that received EPA's ATP approval and are based on earlier 

versions of a Standard Method that will no longer be listed in 40CFR 136 continue to retain EPA 

approval for regulatory monitoring? 

Recommendation 2: Please confirm that the commercially available EPA ATP methods, which are based 

on earlier withdrawn methods, are still approved. 

Comment 116.1 

Wendy Harding and Mala Burton 

Joint Virginia Water Environment Association and Virginia American Water Works Association 

Comment 2: Will methods (e.g. Hach) that received ATP approval and are based on earlier versions of a 

Standard Method that will no longer be listed in 40CFR136 continue to retain EPA approval for 

regulatory monitoring? 

Recommendation 2: Please confirm that the commercially available ATP methods which are based on 

earlier, withdrawn methods are still approved. 

Comment 3: If commercially available methods approved under the ATP program and based on older 

methods are still approved, then why are those same older methods no longer allowed for use by 

laboratories? 

Recommendation 3: Please provide justification for what appears to be a contradictory method 

requirement imposed on the laboratory community. 

Comment 124.1 

Thomas Tourje 

Augusta County Service Authority 

Comment: It is unclear if previously approved ATPs linked to Standard Method Editions are still 

accepted. For example, are Hach methods previously given an accepted ATP and deemed equivalent to 

SM 18th Edition still approved although edition numbers are proposed to be removed with the publication 

of this MUR or methods are updated to a more recent version? 

Recommendation: Specifically list ATP methods separately as part of 40 CFR Part 136 as approved. 

Also, EPA should provide this list of approved ATPs on the EPA website and update it routinely as new 

methods are approved so that the regulated community will understand all the available methods for 

regulatory monitoring. 

Comment 132.1 

Paula Hogg 

Hampton Roads Sanitation District 
2010 Methods Update Rule Response to Comments 48 March 2012 

EPA has proposed significant changes in the Method Update Rule (MUR) regarding which editions of 

Standard Methods are approved for use. Some of the changes between the different editions of Standard 

Methods are significant, and are not necessarily improvements compared to earlier editions. The method 

approval process for Standard Methods, ASTM and EPA differ greatly. Acceptability or approval to 

changes or updates to vendor methods previously deemed "equivalent" to 40 CFR Part 136 methods is not 

addressed. 

Comment: The reliability of analytical methods to provide data that meets the required data quality 

objectives (DQOs) will vary between these standards setting bodies. EPA has a responsibility to take a 

systematic approach to adding and removing methods promulgated through 40 CFR Part 136 to ensure 

NPDES program DQOs are met given this scenario. In order to meet the needs of various regulatory 

programs, methods must be promulgated based on consistent data quality objectives and not solely on 

publication through a consensus standards setting body. Method approval by EPA must include: 1) 

defined DQOs of the programs required to use 40 CFR Part 136 methods and 2) evaluation of method 

suitability through a defined process which includes intra-laboratory and inter-laboratory validation data, 

peer review and laboratory comments, selectivity of the methods for the parameters in question, 

applicable linear dynamic range, defined sensitivity, and accuracy and precision criteria to ensure that any 

methods promulgated in 40 CFR Part 136 are appropriate for their intended uses. 

DQOs for 40 CFR Part 136 methods are not clearly defined. This is a significant deficiency in the current 

regulations, does not follow EPA's Agency Policy Directive No. FEM-2005-001, Ensuring the Validity of 

Agency Methods -Methods Validation and Peer Review Guidelines (2005) or FEM Document No. 2005-

01, Validation and Peer Review of U. S. [EPA] Chemical Methods of Analysis, and leaves the programs 

using these methods with unknown and, hence, unacceptable uncertainty in their effectiveness. 

Since methods have been updated to the latest version through this proposed MUR, it is unclear how this 

impacts vendor methods previously approved by EPA as equivalent to one listed in 40 CFR 136 (for 

example Lachat Methods for TKN, NH3). Often, these methods are updated by the vendors and it is 

unclear if these updated methods are still considered equivalent by EPA. 

Questions include: 

• Since the previous letters referenced older versions of the approved methods, will vendors need to 

obtain updated letters from EPA and have information and data required for flexibility? 

• What documentation will a laboratory need to have to demonstrate that the correct version of a 

vendor method is approved for Clean Water Act monitoring? 

Recommendations 

EPA must develop acceptance criteria for 40 CFR Part 136 methods to be promulgated based on Program 

specific DQOs. This goal can be accomplished in either of two approaches: I) EPA can generate this 

information after standard setting bodies have completed their internal processes of method development 

or 2) EPA can require standard setting bodies to collect or generate the required information before 

methods are promulgated. In either case, a documented, transparent, systematic approach to evaluate 

methods for 40 CFR Part 136 promulgation must be developed and provided to the public for comment. 

Recent versions of previously approved vendor methods (by EPA letter stating equivalency) need to be 

listed in 40 CFR Part 136. If a vendor makes changes to an EPA equivalent method, then EPA must 

require vendors to notify them of changes and provide supporting QA/QC and EPA should publish these 

methods in 40 CFR Part 136. As stated in 1.1, these QA/QC requirements must be based on regulatory 

program DQOs. 

Comment 164.1 
2010 Methods Update Rule Response to Comments 49 March 2012 

Mark Haley 

Hopewell Regional Wastewater Treatment Facility 

Significant changes have been proposed in the Method Update Rule (MUR) regarding which editions of 

Standard Methods (SM) are approved for use. Some of the changes between the different editions are 

significant and not necessarily improvements when comparing earlier editions to the most recent. 

Acceptability and I or approval to changes or updates to vendor methods previously deemed "equivalent" 

to 40CFR Part 136 methods is not addressed. 

Comment: Some of the changes between the different editions are significant and not necessarily 

improvements when comparing earlier editions to the most recent. Since methods have been updated to 

the latest version through this proposed MUR, it is unclear of how this impacts vendor methods 

previously approved by EPA as equivalent to one listed in 40CFR 136 (for example: Lachat Methods for 

TKN and NH3). Often, these methods are updated by the vendors and it is unclear if these updated 

methods are still considered equivalent by EPA. 

Questions include: 

• Since the previous letters referenced older versions of the approved methods, will vendors need to 

obtain updated letters from EPA and have information and data required for flexibility? 

• What documentation will a laboratory need to have to demonstrate that the correct version of a 

vendor method is approved for Clean Water Act monitoring? 

Recommendations 

• Allow all currently approved versions of Standard Methods as listed in 40CFR 136 (i.e. 18th 21 51 -

Editions) to remain approved and allow the continued use of said versions. 

• Previously approved vendor methods (by EPA letter stating equivalency) need to be listed in 40CFR 

Part 136. If a vendor makes changes to an EPA equivalent method, then EPA must require vendors to 

notify them of changes and provide supporting QA/QC and EPA should publish these methods in 

40CFR Part 136. 

Comment 177.1 

Novelle C. Stokes 

South Central Wastewater Authority 

Comment: Will methods (e.g. Hach) that received ATP approval and are based on earlier versions of a 

Standard Method that will no longer be listed in 40CFR136 continue to retain EPA approval for 

regulatory monitoring? 

Recommendation: Please confirm that the commercially available ATP methods which are based on 

previously approved Standard Method Versions that the Agency is proposing to withdraw are still 

approved. 

II.B.7 Biosolids Rule 

List of Comments: 

Comment 96.1 - Denise Paige, Tennessee Municipal League (TML) 

Comment 105 - Sandra Dudley, Water Authority of Dickson County 

Summary of Comments: Two commenters requested that the older Standard Methods (e.g., 18th
2010 Methods Update Rule Response to Comments 50 March 2012 

edition) specified for use in analysis of biosolids or sewage sludge at 40 CFR 503 be added to the tables, 

in order to allow facilities to remain in compliance with the Part 503 regulations. 

Response: Today’s rulemaking does not impose any new requirements or have any effect on methods 

approved for compliance with Part 503 regulations. The requirements for the biosolids regulations, 

including references to old versions of Standard Methods, are codified in Part 503. In addition, selected 

Part 136 methods for fecal coliform and Salmonella were approved for use in sewage sludge in 2007 (FR 

72:14220). EPA may revise the applicable sewage sludge/biosolids methods in a future Methods Update 

Rule. 

Original Comment Text: 

Comment 96.1 

Denise Paige 

Tennessee Municipal League (TML) 

Method Omission: 40 CFR 503.8 (EPA's Sewage Sludge Rule) mandates the use of test methods from the 

18th Edition of Standard Methods for the Examination of Water and Wastewater. The proposed rule, 

through the use of dates within the approved test method number removes the 18th Edition from the 

approved list. This will place local governments in a situation where full compliance is impossible. They 

will be in violation of 40 CFR 503 or 40 CFR 136. There needs to be very clear language amending 40 

CFR 503.S stating that 40 CFR 136 methods are to be used. 

Comment 105 

Sandra Dudley 

Water Authority of Dickson County 

Certain key analytical measurements appear to be omitted from the proposed rule. As an example, 

Standard Method 2540G, Total Solids for a Semi-Solid Material, is not in the approved list. The 40 CFR 

503 regulations require the use of this technique, specifically naming the test specified by the 18th Edition 

of the Standard Methods for the Examination of Water and Wastewater. WADC respectfully requests the 

addition of Method 2540G and other methods that are required by other state and federal regulations. 

II.B.8 Implementation Issues 

List of Comments: 

Comment 106.1 - Charles Boepple, Upper Occoquan Service Authority 

Comment 116.1 - Wendy Harding and Mala Burton, Joint Virginia Water Environment Association and 

Virginia American Water Works Association 

Comment 124.1 - Thomas Tourje, Augusta County Service Authority 

Comment 130.1 - Heather L. Beard, Richland County Utilities 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 162.1 - Ed Saxon, South Carolina Water Quality Association 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Summary of Comments: A number of commenters expressed concerns over the implementation 

schedule relative to the need for labs to run start-up tests, PT samples, revise SOPs, and relative to the 

certification or accreditation requirements in those states that require formal accreditation of wastewater 

laboratories. 

Response: Regarding the need to revise existing SOPs and analyze new performance testing (PT) 

samples, EPA notes that these activities should be occurring on a routine basis for the existing approved 
2010 Methods Update Rule Response to Comments 51 March 2012 

methods (e.g., any laboratory’s quality system requirements should require annual review of all SOPs, 

regardless of this rulemaking). Laboratories that are subject to state certification or accreditation 

requirements must meet those requirements, regardless of this rulemaking. EPA anticipates that such 

state programs will allow some time period for complete implementation of any method changes resulting 

from today’s action. Given the diversity of the state programs that exist, it would be impractical to 

specify a uniform implementation schedule that is perfect for all that are affected by it. 

Original Comment Text: 

Comment 106.1 

Charles Boepple 

Upper Occoquan Service Authority 

Comment 6: Many states have accreditation or certification programs; 14 states participate in the EPAsanctioned National Laboratory Accreditation Program. Certificates often indicate specific method 

numbers. Has EPA considered the impact of the proposed changes on national and state laboratory 

certification programs? State and national certification agencies may require laboratories to resubmit 

applications, repeat PT studies, perform new Demonstrations of Capability, MDL/PQL studies, etc. to 

maintain certification, which will be a significant economic burden on laboratories. 

Recommendation 6: Provide clear guidance to states and accrediting authorities regarding what should be 

required in this area for laboratories to implement updated methods. 

Comment 7: There is no implementation period specified in the proposed rule. It is unclear what may be 

required of laboratories to incorporate the new methods and any associated additional QC requirements 

(e.g. new PT samples, Demonstration of Capability, etc.). 

Recommendation 7: Laboratories should be given a 24-month implementation period to address changes 

listed in the final rule. This period would allow laboratories sufficient time for re-writing methods, 

personnel training, participation in appropriate PT studies, etc. 

Comment 116.1 

Wendy Harding and Mala Burton 

Joint Virginia Water Environment Association and Virginia American Water Works Association 

Comment 6: Many states have accreditation or certification programs; 14 states participate in the EPAsanctioned National Laboratory Accreditation Program. Certificates often indicate specific method 

numbers. Has EPA considered the impact of the proposed changes on national and state lab certification 

programs? State and national certification agencies may require laboratories to resubmit applications, 

repeat PT studies, perform new Demonstrations of Capability, MDL/PQL studies, etc. to maintain 

certification, which will be a significant economic burden on laboratories. 

Recommendation 6: Provide clear guidance to states and accrediting authorities regarding what should be 

required in this area for laboratories to implement updated methods. 

Comment 7: There is no implementation period specified in the proposed rule. It is unclear what may be 

required of laboratories to incorporate the new methods and any associated additional QC requirements 

(e.g. new PT samples, demonstration of capability, etc.). 

Recommendation 7: Laboratories should be given a 24-month implementation period to address changes 

listed in the final rule. This time frame is similar to that allowed by NELAP to implement changes in 

their standards. This period would allow laboratories sufficient time for re-writing methods, personnel 

training, participation in appropriate PT studies, and other quality assurance requirements. 
2010 Methods Update Rule Response to Comments 52 March 2012 

Comment 124.1 

Thomas Tourje 

Augusta County Service Authority 

Comments: Doesn’t this still lead to some approved methods coming from each of the 18th thru 21st 

additions, each with their own separate and differing QC requirements? Why are some methods 

published by Standard Methods showing approval for 20th Ed, while other methods show approval in the 

21st? Table IB (55) for TSS shows a reference to SM 2540D-1997, while SM 2540 D-2005 has been 

published for 5 years+. Why don’t you approve / cite SM 2540 D-2005? 

 How will this work with NELAC lab certification? If you have to use the most recent version of the 

method in Standard Methods, will labs have to resubmit their application, repeat PTs, etc. to maintain 

certification? Will there be a grace period once the MUR becomes a final rule? There is no 

implementation period specified in the proposed rule. It is unclear what may be required of laboratories 

to incorporate the new methods and any associated additional QC requirements (e.g. new PT samples, 

demonstration of capability, etc.). 

Recommendation: Please provide clear guidance to states and accrediting authorities regarding what 

should be required in this area for laboratories to implement updated methods. 

Comment: There is no implementation period specified in the proposed rule. It is unclear what may be 

required of laboratories to incorporate the new methods and any associated additional QC requirements 

(e.g. new PT samples, demonstration of capability, etc.). 

Recommendation: Laboratories should be given a 24-month implementation period to address changes 

listed in the final rule. This time frame is similar to that allowed by NELAP to implement changes in 

their standards. This period would allow laboratories sufficient time for re-writing methods, personnel 

training, participation in appropriate PT studies, and other quality assurance requirements. 

Comment 130.1 

Heather L. Beard 

Richland County Utilities 

We are also concerned about the requirement to use only the most recently approved methods approved 

by the Standard Methods Committee, as discussed on page 58028-9 of the proposed legislation. While 

we understand the desire and need for consistency, being able to only reference the most recent version of 

Standard Methods becomes problematic. As you may be aware, the State of South Carolina currently lists 

the method edition/version on the lab certification certificate issued by the state. The requirement to use 

only the most recently approved method would also require reissuance of the lab certificate for each 

revision. Would this require reapplication for certification for the laboratory with each revision as it is 

implemented? This could mean substantial backlogs for states issuing certifications. Additionally, once 

again smaller labs would be most adversely impacted by this requirement. In addition to more frequently 

revising lab standard operating procedures, the lab would also have to purchase printed versions of 

Standard Methods more frequently and/or subscribe to the on line version of Standard Methods. The 

proposed tracking requirements may force the need for each lab to implement a LIMS system or require a 

substantial increase in labor. For labs with limited budgets, this monetary commitment could further 

restrict how budget monies are distributed throughout the fiscal year. We would propose that you 

consider accepting the versions approved during the most recent five year period. This would require labs 

to stay abreast of current technology improvements and update their methods accordingly, as well as not 

create an undue financial and workload burden. 

Comment 132.1 
2010 Methods Update Rule Response to Comments 53 March 2012 

Paula Hogg 

Hampton Roads Sanitation District 

Comment: The change to approval by publication date introduces several problems including unclear 

requirements, lack of traceability and complications relating to laboratory accreditation. 

Currently laboratories use, report data and are accredited by Standard Methods (SM) method numbers, 

including the edition. Changing 40 CFR citations from edition number to publication date will impact 

data management systems, accreditation data bases, PT provider data reporting systems, and regulatory 

programs. Currently, all QC requirements are not included in individual methods and therefore are not 

always consistent with method publication dates. Therefore it is unclear which QA/QC requirements are 

to be followed. On-line Methods and QC sections are not advancing on the same timeline so method and 

QA/QC requirements are not aligned. 

Overall, moving to newer methods is supported but changing the way methods are cited will cause 

extensive confusion based on the way Standard Methods publishes methods. Currently, there is no clear 

mechanism to track publish date to source or clear requirements for QA/QC for all methods. 

Recommendation 

For Standard Methods, cite methods based on edition number and date and clearly associate the QA/QC 

section required for each method. Recommend to Standard Methods consensus body to include QA/QC 

requirements within cited methods. 

Standard Methods Section 1000 Proposed change/Issue Unclear if Section 1000 of Standard Methods is 

required. 

Recommendation: Requirements need to be clearly stated 

Comment 162.1 

Ed Saxon 

South Carolina Water Quality Association 

SCWQA is also concerned about the requirement to use only the most recently approved methods 

approved by the Standard Methods Committee, as discussed on page 58028-29 of the proposal document. 

While we understand the desire and need for consistency, a requirement to only reference the most recent 

version of Standard Methods becomes problematic. As you may be aware, the State of South Carolina 

currently lists the method edition/version on its lab certification certificate. The requirement to use only 

the most recently approved method would also require reissuance of the lab certificate for each revision. 

Would this require reapplication for certification for the laboratory with each revision as it is 

implemented? This requirement could mean substantial backlogs for states issuing certifications. 

Comment 164.1 

Mark Haley 

Hopewell Regional Wastewater Treatment Facility 

Approved methods are listed by publication date rather than Standard Method edition number. Some 

approved methods are currently not available in hard copy and only can be obtained online. 

Comment: The change to approval by publication date introduces several problems including unclear 

requirements, lack of traceability and complications relating to laboratory accreditation. Currently 

laboratories use, report data, and are accredited by SM method numbers, including the edition. Changing 
2010 Methods Update Rule Response to Comments 54 March 2012 

40CFR citations from edition number to publication date will impact data management systems, 

accreditation data bases, PT provider data reporting systems, and regulatory programs. Currently, all QC 

requirements are not included in individual methods, and since it is proposed only the most current 

methods / editions be used, this makes it unclear which QA/QC requirements (Pali 1000) are to be 

followed as there are three different sections which could be cited. 

Recommendations 

For Standard Methods, cite methods based on edition number and date and clearly associate the QA/QC 

section required for each method. Recommend to Standard Methods consensus body to include QA/QC 

requirements within cited methods. 

II.B.9 Method-specific Issues 

List of Comments: 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 112.1 - Colin Elliot, King County Environmental Lab 

Comment 116.1 - Wendy Harding and Mala Burton, Joint Virginia Water Environment Association and 

Virginia American Water Works Association 

Comment 124.1 - Thomas Tourje, Augusta County Service Authority 

Comment 151.1 - Aaren S. Alger, Pennsylvania Department of Environmental Protection 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 171.1 - Lola Guerra, Henrico County DPU 

Summary of Comments: Numerous method-specific comments were received, including many about 

the BOD method SM 5210 B and the ADMI color method versus SM 2120E. Other comments 

questioned the apparent omission of various microbiological methods and metals methods from the 

tables. 

Response: A typographical error appeared in the version of Table IB that was published in the proposed 

rule. This error caused Standard Method 3113B to be listed as 3113B-1999 in some places and as 

Method 3113B-2004 in other places. For today’s final rule, EPA has revised Table IB to correct this error 

by specifying Method 3113B-2004 consistently. Similar typographical errors occurred for the pH 

method, SM 4500H+

, which has been corrected to SM 4500H+B-2000; the turbidity method, which has 

been corrected from SM2130 to SM 2130B-2001; and the zinc method SM 3500 Zn, which has been 

corrected to SM 3500Zn B-1997. A number of other Standard Methods lacked specifics about which 

letter was associated with the method. This occurred in multiple lines throughout the table, all of which 

have been corrected. 

With regard to the various metals methods where commenters questioned the year citation, the dates in 

Table IB of the proposal are correct. The later dates are those on the most recent versions of these 

methods, as available from Standard Methods On-line. Specifically, SM 3112-2009, SM 3114-2009, SM 

3125-2009, and SM 3500-Cr B-2009 are correct as proposed. Likewise, the phenol method, SM 5530 

B/D-2005 is correct. Standard Methods approved these methods after publication of the 21st edition and 

will be published in the 22nd edition when it is published. In the meantime, the methods are available online. 

With regard to the microbiological methods in Table IA, Coliform (fecal) by SM 9221 C, E-2006, 

Coliform (total) by SM 9221 B-2006, E. coli by SM 9223 B-2004, and Fecal streptococci by SM 9230 B2007 and SM 9230 C-2007 are the latest available versions and are all correct as proposed. 

Similarly, for Table IH, E. coli by SM 9221 B.1-2006/9221F-2006, E. coli by SM 9213 D-2007, and 
2010 Methods Update Rule Response to Comments 55 March 2012 

Enterococci by SM 9230 B-2007 and SM 9230 C-2007 are the latest available versions and are correct as 

proposed. 

With regard to SM 5530 C not being listed in Table IB as an approved method for phenols, SM 5530 B 

and D were added to Table IB in the 2007 Methods Update Rule to replace EPA Methods 420.1 and 

420.2. Contrary to statements by a commenter, the chloroform extraction procedure option in EPA 

Method 420.1 was not previously approved. The description of parameter 48 in Table IB for Method 

420.1 previously read “Phenols, mg/L: Manual distillation, followed by Colorimetric (4AAP) manual....” 

Thus, the chloroform extraction procedure in Method 420.1 was not explicitly approved, and therefore 

SM 5530 C was not added to Table IB in the 2007 rule 72 FR 11199, or in the latest proposal. If a 

regulatory authority believes that the chloroform extraction procedure is necessary to achieve greater 

sensitivity for specific discharges, the regulatory authority has the ability to require its use for such 

discharges because such an approach is more stringent than the national requirements. 

With regard to the withdrawal of the ADMI color method SM 2120 E, and the retention of the NCASI 

ATP noted in footnote 18 of Table IB, EPA notes that this is an instance in which the previously 

approved Standard Method underwent substantive changes. When the 21st edition of Standard Methods 

was published, Standard Methods developed a new color procedure (spectrophotometric-single 

wavelength) that replaced the previous 20th edition version of SM 2120 C (which is not approved at 40 

CFR 136) and renumbered SM 2120 C as SM 2120 D. That new method caused SM 2120 D to be renumbered as 2120 E in the 21st edition. SM 2120 E in the 20th edition of Standard Methods included an 

“alternate method” (the weighted–ordinate spectrophotometric method) as well as the main ADMI 

procedure. With the 21st edition, the “alternate method” became SM 2120 F, but the main procedure in 

the earlier version of 2120 E was dropped. It was because of this change that EPA did not retain SM 

2120 E in the proposal. 

EPA is only approving SM 2120 B -2001 in today’s rule because the other versions of the Standard 

Method color methods were not proposed. In response to a comment stating that SM 2120 E is in some 

permits, permittees may continue to use this method unless the permitting authority specifies otherwise. 

EPA does not agree with many aspects of the multiple sets of nearly identical comments about SM 5210 

B for BOD. Specifically, EPA disagrees that the tighter pH adjustment is not necessary and notes that 

there are several other BOD methods approved in Table IB, including ASTM D888-09, AOAC 973.44, 

USGS I-1578-78, and a vendor-specific ATP. EPA does agree that SM 5210 B has extensive QC 

requirements, but notes that the QC requirements in the most recent version of the method were the result 

of careful deliberations by a group of experts and approved by the consensus group responsible for 

Standard Methods. Those experts found the change in the pH range from 6.5 - 7.5 to the narrower 7.0 - 

7.2 range relevant for performance of the seed organisms. 

EPA disagrees that the latest version of SM 5210 B-2001 requires calculation of the relative percent 

difference (RPD) across samples from different dilutions. An electronic search of the method found no 

occurrences of either “RPD” or “relative percent difference” in the entire text of 5210 A through 5210 D. 

The reporting section of SM 5210B-2001 states “Samples showing large differences between the 

computed BOD for different dilutions, for example, greater than 30%, may indicate the presence of a 

toxic substance or analytical problems. When the effect becomes repetitive, investigate to identify the 

cause.” However, the 30% metric is the “percent difference,” not the RPD, and uses a different 

calculation than the RPD. Moreover, the text cited above states that differences greater than 30% “may” 

indicate problems, and if they occur repeatedly, the analyst should investigate the cause. EPA agrees with 

Standard Methods that such comparisons are useful, but disagrees with the commenters that the intent is 

to treat the results from the different dilutions as “replicates.” 
2010 Methods Update Rule Response to Comments 56 March 2012 

With regard to the method blank acceptance criterion comments, EPA is approving SM 5210 B-2001, and 

withdrawing approval for the 20th edition version. Thus, the method blank acceptance criterion from SM 

5210 B-2001 is the only one that is acceptable. 

EPA does not have a specific position with regard to reporting BOD results with failing dilution water 

blanks, but acceptable GCA results. As noted in the method, the analyst should identify (e.g., “flag”) 

samples where any of the QC parameters in the method are not met. Such information should allow the 

permittee and/or the regulatory authority to assess the impacts of the QC issues on the results for specific 

samples relative to the permit requirements. 

Finally, regarding the comment about why SM 9221 for E. coli is not listed (in Table IA), EPA thanks the 

commenter for noting this typographical error. The method has been added to Table IA. 

Original Comment Text: 

The following commenters had the same (following) comment regarding QC requirements for BOD 

method SM 5210B-2001. 

Comment 116.1 Wendy Harding and Mala Burton, Joint Virginia Water Environment Association 

and Virginia American Water Works Association 

Comment 124.1 Thomas Tourje, Augusta County Service Authority 

Comment 164.1 Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 171.1 Lola Guerra, Henrico County DPU 

Comment 4: The only approved BOD method is SM 5210 B-2001 (21st edition & on-line) which has 

extensive QC requirements. The QC requirements listed in SM5210B-1988 (18th edition) and SM 

5210B-1997 (20th edition) are more appropriate. For example, in the 2001 method, the pH of the sample 

must be adjusted between 7.0 -7.2; however, in the 1988 and 1997 method versions the pH of the sample 

must be adjusted to 6.5 - 7.5. Tightening of the pH range to 7.0 -7.2 is not necessary to provide the proper 

environment for the microbiological component of the seed. The 2001 BOD method version also requires 

calculation of RPD on different dilutions of the same sample. Sample dilutions cannot be used as a 

measure of precision as they are not duplicate measurements. Duplicates should be required in order to 

measure precision and analyst observation on dilution differences can be used to determine potential toxic 

effects or analytical errors. The RPD calculation could become an issue on samples with low BOD 

concentrations. A sample that had different dilutions reading 8 mg/L and 12 mg/L would have to be 

flagged as being either toxic or an analytical error. Another problem with the RPD calculations can occur 

when analyzing industrial samples that contain large amounts of solids. It is possible to have variability 

between dilutions that is not due to toxicity or analytical error but simply due to sample matrix effects. 

Recommendation 4: Recommend to Standard Methods that they address this issue and revise method 

accordingly. List SM 5210B-1997 as an approved EPA method until SM 5210B-2001 has been updated. 

Other comments: 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 

Comment: Additionally, regarding the BOD methods, what is the method blank acceptance criteria since 

the two online methods have different written QC requirements? What is the USEPA position on 

reporting BOD results with a dilution blank outside of 0.0¬0.2 mg/L but with acceptable GGA results? 

Please clarify. 

Comment 112.1 

Colin Elliot 
2010 Methods Update Rule Response to Comments 57 March 2012 

King County Environmental Lab 

In Table IE some of the Trace metals by SM 3113 have the 2004 revision listed whereas some have the 

1999 revision listed. Specifically, Aluminum, Antimony, Arsenic, Barium, Beryllium, Cobalt, Copper, 

Gold, Manganese, Molybdenum, Nickel, Selenium, Thallium, Tin, and Vanadium are listed with the 2004 

revision. Cadmium, Chromium, Iron, Lead, and Silver are listed with the 1999 revision. There should 

only be one revision for all metals. 

In Table IB, Parameter #48 Phenols, SM 5530B and D are approved for Phenols but not SM 5530C, the 

chloroform extraction method. Is this an oversight, or is EPA planning to remove the Standard Methods 

chloroform extraction as an approved method for phenol determinations? The chloroform extraction 

procedure is still included in EPA Method 420.1. Please state why SM 5530C, the chloroform extraction 

procedure, is not included as an approved method. 

EPA is proposing to remove the ADMI color method SM 2120E. This method is listed on many NPDES 

permits and EPA does not propose an alternative ADMI method. Is this removal an error? The footnote 

references the NCASI method which is not equivalent to SM 2120E. Will NPDES permits be allowed 

modifications to move from the ADMI method to an alternative procedure? This issue will need to be 

addressed if the removal of the ADMI method is not an error. An alternative must be provided to NPDES 

permit holders. 

The following comments are in regards to missing letter references to Standard Methods: Table IB -pH by 

SM 4500H+ is missing the "B". Table IB - All metals by Standard Methods SM3113 are missing the "B". 

Table IB - Mercury by SM 3112 is missing the "B". Table IB - All metals by Standard Methods 8M 3120 

are missing the "B". Table IB - Turbidity by SM 2130 is missing the "B". Table IB - Zinc by SM 3500Zn 

is missing the "B" 

Comment 116.1 

Wendy Harding and Mala Burton 

Joint Virginia Water Environment Association and Virginia American Water Works Association 

Proposed Change: Addition and deletion of chemical and biological methods 

Comment 1: Color (ADMI) is approved but Standard Methods deleted. Why was the Standards Methods 

color procedure deleted? The ADMI method is not peer-reviewed and, due to the age of document, may 

be difficult to obtain now or in the future. 

Recommendation 1: Approve the Standard Methods procedure for color. 

Comment 151.1 

Aaren S. Alger 

Pennsylvania Department of Environmental Protection 

Table IA -Biological Methods for Wastewater and Sewage Sludge 

Coliform (fecal) by SM 9221 C E-2006. The version of SM 9221 in the 21st edition is dated 2001. 

Coliform (total) by SM 9221 B-2006. The version of SM 9221 in the 21st edition is dated 2001. 

E. coli by SM 9223 B-2004. The version of SM 9223 in the 21st edition is dated 1997. 

Fecal streptococci by SM 9230 B-2007 and SM 9230 C-2007. The version of SM 9230 in the 21st edition 

is dated 1993. 

Table IH -Microbiological Methods for Ambient Water 

E. coli by SM 9221 B.1-2006/9221F-2006. The version of SM 9221 in the 21st edition is dated 2001. 

E. coli by SM 9213 D-2007. The version of SM 9213 in the 21st edition is dated 1997. 
2010 Methods Update Rule Response to Comments 58 March 2012 

Enterococci by SM 9230 B-2007 and SM 9230 C-2007. The version of SM 9230 in the 21st edition is 

dated 1993. 

Table IB -Inorganic Test Procedures 

Metals by SM 3113-2004 (AA furnace). The version of SM 3113 in the 21st edition is dated 1999. (Note 

that there are 5 metals where the approved version is SM 3113-1999, as in the 21st edition. These metals 

are Cd, Cr, Fe, Pb, and Ag.) 

Metals by SM 3125-2009 (ICP/MS). The version of SM 3125 in the 21st edition is dated 1997. 

Mercury by SM 3112-2009 (CVAA). The version of SM 3112 in the 21st edition is dated 1999. 

Arsenic by SM 3114-2009 (AA gaseous hydride). The version of SM 3114 in the 21st edition is dated 

1997. 

Chromium, hexavalent by SM 3500-Cr B-2009 (colorimetric). The version of SM 3500-Cr in the 21st 

edition is dated 2001. 

Phenols by SM 5530 B/D-2005. The version of SM 5530 in the 21st edition is dated 2000 

Comment 171.1 

Lola Guerra 

Henrico County DPU 

Comment 1: Color (ADMI) is approved but Standard Methods deleted. Why was the Standards Methods 

color procedure deleted? The ADMI method is not peer-reviewed and, due to the age of document, may 

be difficult to obtain now or in the future. 

Recommendation 1: Approve the Standard Methods procedure for color. 

Comment 3: Why is E. coli Method 9221 not listed (in Table IA)? 

Recommendation 3: Include E. coli Method 9221. 

II.B.10 Other Comments 

List of Comments: 

Comment 166.1 - Paul Wiegand, National Council for Air and Stream Improvement, Inc. 

Summary of Comments: One commenter raised concerns that were not readily characterized in the 

other subsections regarding the Standard Methods. Specifically, the commenter is concerned that VCSB 

methods, such as Standard Methods, approved by EPA at 40 CFR 136 may not be subjected to the same 

level of validation as required of applicants to the ATP program, and states that EPA make available all of 

the validation data for any VCSB methods it proposes to approve. 

Response: EPA disagrees that it is necessary to subject all Standard Methods or other VCSB methods to 

extensive validation. Standard Methods are revised from time to time to improve clarity (i.e., editorial 

corrections) or to provide additional quality control (QC) instructions. Thus, most Standard Methods 

proposed for this rulemaking are not new, in that they do not use different analytical techniques or 

instrumentation than the previously approved versions of those Standard Methods. In those instances in 

which EPA does propose to approve a new VCSB method, it often works with the developer of the 

method and the VCSB to ensure that validation efforts are appropriate for wastewater matrices subject 

to the Clean Water Act. EPA encourages the method developer or the VCSB to make available relevant 

study plans, validation data and reports for any new method under consideration, or in readily available 

published references. EPA will continue to evaluate the validation study data available for any newly 
2010 Methods Update Rule Response to Comments 59 March 2012 

developed methods considered for rulemaking in the future and make a determination on the adequacy of 

the available data for wastewater program application. 

As with methods developed by EPA, it is not practical or possible to validate every method in 

wastewaters representing every potential discharger subject to the Clean Water Act. Therefore, in 

considering new methods from any source, EPA examines the available validation data for representative 

wastewater matrices, just as it does for ATP applicants. EPA finds that ATP applications often represent 

vendor-specific methods with wide application across regulated industrial categories, or industry-specific 

requests for alternatives. In those instances, EPA is able to more directly influence the extent of the 

validation effort and makes data submitted directly to EPA available in the record as appropriate. 

Original Comment Text: 

Comment 166.1 

Paul Wiegand 

National Council for Air and Stream Improvement, Inc. 

EPA is proposing adoption of a number of methods without providing any data showing that these 

methods will perform as required on the types of wastewaters regulated in the NPDES program. Methods 

adopted by EPA should be subject to the same level of validation required in the Alternate Test Procedure 

Program. 

It is understood that EPA proposes addition of numerous methods that were developed by voluntary 

consensus organizations (e.g., ASTM and Standard Methods) under the authority and requirements of the 

National Technology Transfer Act. The Act requires EPA to adopt all suitable methods developed by 

consensus organizations but does not release EPA from the responsibility of determining that the 

consensus methods meet the testing requirements under 304(h) of the Clean Water Act. If EPA evaluates 

a candidate consensus method and finds that it does not meet the performance requirements required for 

NPDES permit application and compliance testing, it is not obligated to adopt the method and need only 

communicate the basis for that decision to the Office of Budget and Management annually. 

In the current proposal, EPA has not provided any data that verify that the proposed consensus methods 

perform as required on the types of wastewaters regulated in the NPDES program. If a regulated entity or 

other interested organization (e.g., an instrument manufacturer) requests approval for the use of an 

alternate test procedure, EPA has established strict validation requirements that must be met before an 

approval can be granted. EPA currently proposes to fully incorporate methods that have previously been 

approved for nationwide use, and in so doing has effectively set a minimum method validation 

requirement. Thus EPA has failed to apply the same level of validation required in its own Alternate Test 

Procedure Program to the consensus methods. EPA should provide its rationale and make available the 

related data used for determining that these methods meet the required performance criteria and/or subject 

them to the same level of validation required in the ATP program. Those data should be noticed for 

public review and comment before incorporating a consensus method into 40 CFR Part 136. 

Section II.C New ASTM Methods and New Versions of Approved ASTM Methods 

List of Comments: 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 166.1 - Paul Wiegand, National Council for Air and Stream Improvement, Inc. 

Summary of Comments: One commenter expressed concerns about potential confusion for dischargers 

as a result of all of the newly added methods for cyanide. Another commenter expressed concerns about 
2010 Methods Update Rule Response to Comments 60 March 2012 

newly added cyanide methods, as well as the process that EPA uses in evaluating the suitability of VCSB 

methods for use in wastewater discharges from the variety of industries subject to NPDES regulations. 

Response: EPA approved new cyanide methods to allow dischargers and their laboratories to address 

potential positive and negative interferences in different wastewater dischargers. Given the wide range of 

discharges subject to NPDES regulations, it is not possible for EPA to require or recommend specific 

methods or practices for specific types of discharges. Dischargers and their laboratories must 

communicate with their regulated authority regarding the nature of the samples to be analyzed. 

Information about the regulatory permit limits for any pollutant, historical data for those pollutants, and 

whether or not the pollutant is used in or produced by the regulated process should be included in such 

communications. Cyanide is not appreciably different than other regulated pollutants. 

Regarding the process EPA uses to evaluate VCSB methods relative to specific industry wastewaters, 

EPA refers readers to the response to II.B.10 above. Today’s rule does not require the use of a specific 

new or existing method for a given industry’s discharge. Rather, today’s rule provides additional options 

to select an appropriate method for compliance monitoring. No existing regulatory limits on the pulp and 

paper industry (or any other industry) were developed using these newly approved methods. Today’s rule 

simply broadens the range of approved methods in order to allow any discharger to produce acceptable 

results for cyanide in their wastewater. All of the newly approved methods include QC tests and 

acceptance criteria that can and should be used by laboratories and dischargers to gauge the performance 

of these methods in a given sample matrix (i.e., industry discharge). If the method is properly carried out 

and the supporting QC data indicate acceptable performance, then EPA will accept the method results for 

that sample. The commenter’s implied alternative, e.g., testing every approved method on every 

regulated industry’s wastewater, is impractical. 

Original Comment Text: 

Comment 91.1 

Andrea Rex 

Massachusetts Water Resources Authority 

This section proposes a number of new or revised methods from ASTM, mostly for various forms of free, 

available, and total cyanide using a variety of instrumental approaches. As mentioned later, cyanide 

testing is complicated due to the number of potential positive and negative interferences and the various 

ways to try to address these interferences. By significantly expanding the number of approved cyanide 

methods, and the additional language on method modifications, permittees have new options but it is not 

obvious which method might be useful for any given discharge. 

Comment 166.1 

Paul Wiegand 

National Council for Air and Stream Improvement, Inc. 

It is understood that EPA proposes addition of numerous methods that were developed by voluntary 

consensus organizations (e.g., ASTM and Standard Methods) under the authority and requirements of the 

National Technology Transfer Act. The Act requires EPA to adopt all suitable methods developed by 

consensus organizations but does not release EPA from the responsibility of determining that the 

consensus methods meet the testing requirements under 304(h) of the Clean Water Act. If EPA evaluates 

a candidate consensus method and finds that it does not meet the performance requirements required for 

NPDES permit application and compliance testing, it is not obligated to adopt the method and need only 

communicate the basis for that decision to the Office of Budget and Management annually. 

In the current proposal, EPA has not provided any data that verify that the proposed consensus methods 

perform as required on the types of wastewaters regulated in the NPDES program. If a regulated entity or 
2010 Methods Update Rule Response to Comments 61 March 2012 

other interested organization (e.g., an instrument manufacturer) requests approval for the use of an 

alternate test procedure, EPA has established strict validation requirements that must be met before an 

approval can be granted. EPA currently proposes to fully incorporate methods that have previously been 

approved for nationwide use, and in so doing has effectively set a minimum method validation 

requirement. Thus EPA has failed to apply the same level of validation required in its own Alternate Test 

Procedure Program to the consensus methods. EPA should provide its rationale and make available the 

related data used for determining that these methods meet the required performance criteria and/or subject 

them to the same level of validation required in the ATP program. Those data should be noticed for public 

review and comment before incorporating a consensus method into 40 CFR Part 136. 

EPA proposes adoption of a variety of analytical methods for determinations of total, available, and free 

cyanide that have not been validated for specific wastewaters such as those from pulp and paper 

manufacturing. EPA should limit the scope of each method approval to those wastewater matrices for 

which method validation and detection limits studies have been conducted, or clearly establish the 

guidelines for determining the applicability of each analytical approach. NCASI is submitting NCASI 

File Report No. WC-05.01 in support of this comment. 

The new methods proposed for free cyanide are intended to capture that portion of cyanide that would 

most likely be present at the pH and temperature of ambient waters by eliminating procedural steps that 

disassociate weak and strong metal cyanide complexes. However, these new free cyanide methods use 

the same determinative steps as methods for determining available cyanide or total cyanide and will be 

prone to the same matrix interferences that are commonly found in pulp and paper matrices. 

Furthermore, EPA intends to modify footnotes to the sample preservation and holding time requirements 

in Table II to increase flexibility with regard to preservation and sample treatments to address 

interferences. Therefore, pulp and paper industry dischargers may have to conduct extensive detection 

limit and method validation studies if their NPDES permitting authorities implement monitoring 

requirements for total, available, or free cyanide in order to select the “most sensitive method” applicable 

to their specific wastewater discharges. Given that industrial discharge limits may be imposed based on 

water quality determinations conducted in ambient waters, the applicability and performance of each 

methodology in a given wastewater will be important when establishing permit limitations. Therefore, 

EPA should limit the scope of each method approval to those wastewater matrices for which method 

validation and detection limits studies have been conducted or clearly establish the guidelines for 

determining the applicability of each analytical approach. 

The proposed and currently approved methods for total, available, and free cyanide employ a wide range 

of sample preparation techniques, various measures to address interferences, several determinative steps, 

and varied detection limits, but have not been validated using pulp and paper matrices. NCASI studies to 

evaluate and compare some of the methods approved in the 2006 update showed highly variable total and 

available cyanide results. For example, NCASI’s study confirmed that cyanide amenable to chlorination 

(CATC) methodologies are not appropriate for pulp and paper wastewaters, as noted in Standard Methods 

4500-CN-G. Furthermore, treatment steps to eliminate interferences and different sample preservatives 

were noted to have significant effects on sample variability and detection limits for a variety of methods 

when applied to pulp and paper wastewaters. Although it appears that sulfide interferences up to 50 mg/L 

have been addressed in at least one of the revised flow injection and amperometric detection methods 

(ASTM D6888), the proposed sulfide removal reagent has not been evaluated when applied to pulp and 

paper wastewaters. 

The new micro distillation and ion chromatography procedures being proposed for approval were not 

included in NCASI’s evaluations, so extensive additional work would be needed to demonstrate 

equivalence with the current distillation procedures, determine detection limits, assess potential 

interferences, and evaluate performance using these techniques in pulp and paper wastewaters. 
2010 Methods Update Rule Response to Comments 62 March 2012 

 

Based on prior NCASI studies and the wide variety of options available for conducting total, available, 

and free cyanide measurements, it will be incumbent on the regulated entity to ensure that its laboratory 

has the proper documentation to demonstrate equivalence in its wastewater if the laboratory opts to use 

micro distillation procedures, establish wastewater-specific detection limits, and validate method 

performance. Therefore, EPA should more clearly establish guidelines for the applicability of each 

analytical approach or limit applicability to specific wastewater matrices. 

II.C.1 ASTM D2036-09 

II.C.2 ASTM D6888-09

II.C.3 ASTM D7284-08

II.C.4 ASTM D7511-09e2

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Summary of Comments: Three commenters supported the addition of these methods. 

Response: EPA appreciates the commenters’ support and it is including these methods in the final 

rulemaking. 

Original Comment Text: 

The following commenters supported the addition of the new methods. 

Comment 79.1 Richard Burrows, TestAmerica Inc. 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 169.1 Judith R. Morgan, American Council of Independent Laboratories 

II.C.5 Add free cyanide in Table IB and allow use of Method OIA 1677-09 and ASTM Methods 

D4282-02 and D7237-10

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 95.1 - Robert B. Leventry, Butler County Water and Sewer Department Regulatory 

Compliance Team 

Comment 153.1 - Debbie Webster, Central Valley Clean Water Association 

Comment 169.1 - Judith R. Morgan - American Council of Independent Laboratories 

Summary of Comments: Three commenters supported the addition of this method. A fourth 

commenter supported the addition and provided a detailed discussion of the issues that might be resolved 

with the use of this method. A fifth commenter was supportive, but expressed concerns about the 

timetable for the change. 

Response: EPA appreciates the commenters’ support and it is including the method in the final 

rulemaking. EPA also appreciates the thoughtful presentation of issues associated with total cyanide 

measurements and the relevance of ASTM D7365-09a and sodium hydroxide preservation of samples. 

In response to the comments, EPA is revising the entries in Table II for parameters 23 and 24 as follows: 
2010 Methods Update Rule Response to Comments 63 March 2012 

Parameter Number/Name Container 1 Preservation 2, 3

Maximum Holding 

Time 4

23-24. Cyanide, total or available 

(or CATC), and free 

P, FP, G Cool, ≤6 °C18 , NaOH to pH>10 5, 

6

, reducing agent if oxidizer 

present 

14 days 

With regard to a timetable for implementation of new methods, EPA cannot prevent state or local 

regulatory authorities from requiring immediate implementation. Moreover, the inclusion of a new 

parameter and associated methods in 40 CFR Part 136 does not imply a requirement for a permit 

limitation or monitoring under CWA. The permitting authority is responsible for setting requirements for 

specific parameters and the associated methods. New permit requirements set by the permitting authority 

address the timetable for implementation for a new method and parameter, which generally happens when 

a permit is reissued. 

Original Comment Text: 

The following commenters supported the addition of the new methods. 

Comment 79.1 Richard Burrows, TestAmerica Inc. 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 169.1 Judith R. Morgan , American Council of Independent Laboratories 

Other comments: 

Comment 95.1 

Robert B. Leventry 

Butler County Water and Sewer Department Regulatory Compliance Team 

FR pages 58030 and 58031 In the preamble Section II C 5, EPA proposes to add methods for free cyanide 

analysis which has not previously been included as a parameter in the tables. 

Some of our NPDES permits specify using method 4500 Cn I from various editions of SM until EPA 

promulgates a method for free cyanide. Generally, Ohio EPA makes these kinds of changes with the next 

permit cycle which allows time for both the utility and the laboratory to prepare for the change. However, 

with the wording in some of our permits it appears to require an immediate switch to the new method 

upon promulgation. This may not allow local laboratories enough time to implement a new method and 

all associated QA/QC. BCWS requests that USEPA provide clear guidance to states allowing time for 

transitions such as this where a new parameter required under the CWA is added to part 136. 

Comment 153.1 

Debbie Webster 

Central Valley Clean Water Association 

On behalf of the member agencies of the Central Valley Clean Water Association (CVCWA), we would 

like to share our support for proposed amendments related to cyanide test procedures. As explained in 

greater detail below, we specifically endorse proposed amendments to include “free” cyanide analytical 

procedures in Table IB 

In California, the Policy for Implementation of Toxics Standards for Inland Surface Waters, Enclosed 

Bays, and Estuaries of California (SIP) establishes procedures for the development of effluent limitations 

for pollutants such as cyanide. In the arid Central Valley of California, many POTWs discharge effluent 

to seasonal streams that often provide little to no dilution for prolonged periods of time. Through the SIP 

procedure, these POTWs discharging to effluent dominated water bodies often receive average monthly 

effluent limits for cyanide as low as 4.1 μg/L. Consistent compliance with this limitation is problematic, 

and numerous Central Valley POTWs employing secondary and tertiary treatment systems with chlorine 
2010 Methods Update Rule Response to Comments 64 March 2012 

or UV disinfection technologies have been affected. These POTWs almost universally utilize acid 

distillation procedures with amperometric or spectrophotometric detection to measure total cyanide (i.e., 

EPA methods 335.2, 335.4, and 9010B, Standard Method 4500-CN) as a NPDES permit required means 

of measuring compliance. As U.S. EPA is aware, total cyanide measurements derived from such acid 

distillation based methods are prone to interference and bias, particularly in complex matrices such as 

POTW effluent. 

The attached document Problems Associated with Using Current EPA Approved Total Cyanide 

Analytical Methods for Determining Municipal Wastewater Treatment Plant NPDES Permit Compliance, 

prepared on behalf of CVCWA member agencies by local experts familiar with POTW cyanide 

compliance issues, was presented to the Central Valley Regional Water Quality Control Board on May 

26, 2010. In this document, evidence independently generated by several POTWs strongly suggests that 

the use of sodium hydroxide as a preservative can lead to positive bias in total cyanide measurements. 

For POTWs that have not been granted dilution credit, small errors in cyanide measurement can lead to 

effluent limit violations and water quality objective exceedances. Sodium hydroxide-related bias is 

recognized by experts in cyanide analytical chemistry, and as U.S. EPA is aware through its proposed 

inclusion of ASTM D7365-09a, it is recommended as an appropriate mitigation of this interference to 

omit preservation with sodium hydroxide, provided cyanide’s stability can be demonstrated through a 

properly conducted hold-time study. 

Allowing for the omission of sodium hydroxide in cyanide stable matrices currently is not codified in the 

40 CFR 136. Formal reference to ASTM D7365-09a in the footnotes to Table II would significantly 

improve upon the preservation and stabilization of cyanide samples. But inclusion of the ASTM standard 

practice may not be the ultimate solution necessary to fully address the cyanide compliance and cyanide 

interference issues facing our many member agencies. For this reason we fully support the proposal to 

include “free” cyanide analytical methods in the battery of approved methods for NPDES compliance 

monitoring as well the language modifications to the Table II introduction that gives the local permitting 

authority the discretion to approve the use of alternative cyanide sample handling and preservation 

procedures. As presently stated in the footnotes to Table II, “There may be interferences that are not 

mitigated by approved procedures,” including the latest procedures detailed in ASTM D7365-09a. For 

this reason, we strongly support the regulatory flexibility afforded by dealing with the local permitting 

authority in developing analytical fixes where interference and bias is involved. Furthermore, the 

possibility of utilizing an analytical method that measures the portion of cyanide that is truly bioavailable 

is needed and, therefore, we support inclusion of the proposed “free” cyanide procedures. 

Although our CVCWA membership is limited to the Central Valley of California, we are aware that our 

issues with total cyanide analysis and cyanide compliance are not unique. Studies documenting the 

problems associated with total cyanide analysis on a national scale are published in the scientific 

literature, as well in professional and trade publications. We applaud U.S. EPA’s efforts to address these 

cyanide issues, and support the cyanide-related changes in the proposed rule. 

(EPA did not include attachment 153.2 due to its length.) 

II.C.6 ASTM D888-09

List of Comments: 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 120.1 - David N. Speis, Environmental Laboratory Advisory Board (ELAB) 
2010 Methods Update Rule Response to Comments 65 March 2012 

Summary of Comments: One commenter noted that the dissolved oxygen method is not sufficient to 

determine BOD or COD, and that EPA needs to make this clear in the table. A second commenter noted 

that there are other ASTM dissolved oxygen methods that might also be added. 

Response: EPA disagrees with the first commenter because the method is clearly applicable to dissolved 

oxygen measurements in conjunction with BOD and CBOD analyses, as described in the method. As a 

result of this commenters’ input, in today’s final rule, EPA added language to the end of footnote 63 in 

Table IB to clarify that Part 136 allows the use of Hach Method 10360 to measure dissolved oxygen when 

performing the methods approved in Table IB for measurement of biochemical demand (BOD) and 

carbonaceous biochemical oxygen demand (CBOD). In response to the addition of other ASTM methods 

noted by the second commenter, EPA may consider other ASTM dissolved oxygen methods in a future 

rulemaking. 

Original Comment Text: 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

ASTM Method D888-09 is listed as an approved biochemical oxygen demand (BOD) and carbonaceous 

biochemical oxygen demand (CBOD) method in Table IB. This is a dissolved oxygen procedure, and 

does not contain the required QC or procedures for performing BOD analyses. As such, it should only be 

listed as a procedure for Dissolved Oxygen, and not BOD and CBOD. If the intent was to use this method 

in conjunction with the BOD method, then this should be stated in a footnote. 

Comment 120.1 

David N. Speis 

Environmental Laboratory Advisory Board (ELAB) 

Additional methods that are of particular interest to many wastewater laboratories are the acceptance of 

the ASTM D888-09 Part C luminescence-based detection method for dissolved oxygen and the use of the 

associated Alternate Test Procedures utilizing the Luminescence Measurement of Dissolved Oxygen. 

II.C.7 ASTM D7573-09 

No comments were received regarding ASTM D7573-09. EPA is including this method in today’s 

rulemaking. 

II.C.8 ASTM D7065-06

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica, Inc. 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 116.1 - Wendy Harding and Mala Burton, Joint Virginia Water Environment Association and 

Virginia American Water Works Association 

Comment 125.1 - John H. Phillips, Ford Motor Company 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 166.1 - Paul Wiegand, National Council for Air and Stream Improvement, Inc. 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Comment 180 - Philip Yee, The Dow Chemical Company 
2010 Methods Update Rule Response to Comments 66 March 2012 

Summary of Comments: Several commenters supported the inclusion of ASTM D7065-06. Other 

commenters expressed concern that the ASTM procedure uses the same instrumentation and materials as 

Method 625, and thus Method 625 also should be approved for these analytes. Two other commenters 

expressed concerns about ASTM D7065-06 and the lack of validation data for specific industry 

wastewater matrices. One commenter also noted the lack of holding time and preservation requirements 

for the analytes in question. One commenter expressed concern that one of the surrogates described in the 

method is sometimes a target analyte.

Response: EPA thanks those commenters’ supporting the inclusion of this method in the Methods 

Update Rule. However, EPA disagrees that expanding Method 625 to include the five analytes covered by 

ASTM D7065-06 offers the “benefits” mentioned by the commenters. Absent a requirement for analysis 

of the five new analytes in every sample, laboratories would incur costs for buying and maintaining 

standards for analytes they may never need to report. Further, any existing standard operating procedures 

(SOPs) would need to be revised to include these analytes, the “most stringent method QA/QC” cited by 

one commenter, and other considerations relevant to these analytes. The effort required to revise such 

SOPs is roughly equivalent to that of creating a new SOP for ASTM D7065-06. Thus, EPA concludes 

that little or no cost savings would result from adding these analytes to Method 625. Furthermore, 

expanding the applicability of Method 625 to additional analytes is outside the scope of today’s 

rulemaking. If a laboratory/permittee wishes to use Method 625 for these analytes, they may request an 

approval for a specific application through the ATP program, provided that QA/QC criteria from the 

approved method are met. See response in Section II.A.3.e for ATP details. 

Method D7065-06 has been tested by eight laboratories using reagent water and substitute wastewater 

prepared according to ASTM D5905. Substitute wastewater may be used for laboratory testing where a 

reproducible mixture simulating municipal wastewater is required. To provide a more rugged evaluation 

of a test method's ability to measure analytes and the precision of the test method under more demanding 

conditions, it is necessary to utilize a matrix more complex than reagent water. Substitute wastewater is 

intended to be used as a material to be spiked with analytes or interferents of interest to evaluate the 

performance of test methods. 

Utilization of substitute wastewater as a matrix in interlaboratory validation studies allows inclusion of 

performance statistics for this matrix in the precision and bias section of ASTM test methods. Users of 

test methods will be able to evaluate their application of test methods in this matrix against published 

results. 

As noted earlier in this document in response to comments on Section II.C of the proposal, it is 

impractical to expect EPA to test every method in every industry’s wastewater. EPA has established 

procedures to validate test methods in a representative number of matrices when the method may be 

approved for nationwide use. This approach strikes a balance of challenging the method in a range of 

matrix types to determine the expected performance of the method in various matrices without requiring 

onerous testing. If there are any concerns with the method for a specific matrix, the laboratory should 

evaluate the method for that matrix or use a different method that may be more appropriate for that 

matrix. 

With regard to the difficulties in making measurements at the “part-per-quadrillion” levels cited by one 

commenter, EPA notes that neither the method nor the proposal suggests that such low-level 

measurements are intended by this method. The “reporting ranges” in Table 1 of the published method 

cover low part-per-billion levels in water (e.g., μg/L). 

Information on sample preservation and holding times was inadvertently not included in Table II. In 

response, EPA will add the following information to Table II for these analytes, based on the discussion 

in Section 10 of ASTM D7605-06: 
2010 Methods Update Rule Response to Comments 67 March 2012 

Parameter Number/Name Container 1 Preservation 2, 3

Maximum Holding 

Time 4

Table IC - Alkylated phenols: 

 114 -118. Alkylated phenols 

G Cool, < 6 oC, H2SO4 to pH < 2 28 days until extraction, 

40 days after extraction 

With regard to the use of n-nonylphenol (n-NP) as a surrogate compound, EPA notes that the concern is 

not significantly different from that in other methods for organic parameters that employ surrogates. The 

method lists two surrogate compounds, including n-NP. In the event that n-NP is a target analyte, under 

40 CFR part 136.6, the laboratory has the flexibility to not spike n-NP into every sample as a surrogate. 

In instances where n-nonylphenol is an analyte of interest, the discharger would need to relay that 

information to the laboratory in any event, so that the laboratory could utilize the allowed flexibility to 

add the analyte as a target, rather than as a surrogate. 

Original Comment Text: 

The following commenters supported the addition of this new method. 

Comment 79.1 Richard Burrows, TestAmerica, Inc. 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 169.1 Judith R. Morgan, American Council of Independent Laboratories 

Other comments: 

Comment 116.1 

Wendy Harding and Mala Burton 

Joint Virginia Water Environment Association and Virginia American Water Works Association 

This method is equivalent to EPA 625. However, 625 is not referenced for these compounds, requiring 

laboratories to use a separate method, SOPs, accreditation application, method validation, thus incurring 

significant additional costs to maintain capability. Furthermore, additional hazardous waste is generated. 

These additional costs are passed onto data users in both sampling and analytical fees. 

Recommendation: The proposed method is equivalent to EPA Method 625 with regard to sample 

extraction and determinative technique. In addition to the inclusion of the proposed ASTM method to 

the Method Update Rule, EPA should to allow for the use of EPA method 625 for the determination of 

the five chemicals listed in the proposed ASTM D7065-06 method as long as the requirement of the most 

stringent method QA/QC are met, thus expanding the scope of Method 625. 

Comment 125.1 

John H. Phillips 

Ford Motor Company 

ASTM D7065, This method is sensitive to interferences that can drastically affect surrogate recoveries 

and can produce biased data. Para-n-nonylphenol should be replaced with a different surrogate, because 

it is sometimes a target analyte. 

Comment 132.1 

Paula Hogg 

Hampton Roads Sanitation District 

This method is equivalent to EPA 625. However, 625 is not referenced for these compounds requiring 

laboratories to use a separate method, develop a separate SOP, apply for both methods for accreditation, 

analyze PT samples by both of these methods and perform duplicate method validation, thus incurring 

significant additional costs to maintain capability for two identical methods. These additional costs are 
2010 Methods Update Rule Response to Comments 68 March 2012 

passed onto data users in both sampling and analytical fees. Furthermore, adding these compounds to 

EPA method 625 can reduce the generation of hazardous waste. 

Recommendation 

The proposed method is equivalent to EPA Method 625 with regard to sample extraction and 

determinative technique. HRSD is requesting EPA, in addition to the inclusion of the proposed ASTM 

method to the Method Update Rule, list EPA Method 625 for these compounds, thus expanding the scope 

of method 625. Again, development of DQOs for these compounds would allow laboratories to use the 

most efficient and applicable approach for analyses. 

Comment 166.1 

Paul Wiegand 

National Council for Air and Stream Improvement, Inc. 

The proposed inclusion of these methods for general use is inappropriate because they have not been 

validated for use with certain wastewaters such as those from pulp and paper manufacturing. EPA should 

limit approval of their use to only matrices for which validation studies have been conducted. 

 EPA proposes approval and listing of ASTM D7065-06 in Table IC. The method states that it has been 

investigated for use with surface waters and waste treatment effluent samples and is applicable to these 

matrices. It has not been evaluated or validated for use in pulp and paper industrial wastewaters and 

therefore should not be approved for use in these matrices until validation studies have been conducted. 

Comment 180 

Philip Yee 

The Dow Chemical Company 

The Federal Register proposal further stated that this method has been multi-laboratory validated for use 

with surface water and waste treatment effluent samples and is applicable to these matrices. 

Dow is concerned that Method ASTM D7065-06 does not utilize validated data. Dow recommends data 

validation for Method ASTM D7065-06. Page 10 of Method ASTM D7065-06 states: “This method has 

been tested by eight laboratories using reagent water and Practice D5905 substitute wastewater.” 

Obviously, “tested” is very different from “validated”. After careful review of the related Single 

Laboratory Data, Method ASTM D7065-06 Tables 7 through 12 (pp. 10-12), it is not clear how testing 

was performed. It appears each laboratory analyzed one analyte only in multiple replicates which is 

definitely not sufficient for data validation. The cited statistical performance would put this method into 

the semi-quantitative category at this time: Roughly 63-68% recovery with a relative (SINGLE) standard 

deviation of 8% (Table 6). Non validated data will result in numerous difficulties for the regulated 

community to utilize this method and evaluate corresponding test results. Dow believes the data 

validation step must include looking for all analytes of interest in the real world matrices at or near 

proposed reporting limit for each analyte. 

For Method ASTM D7065-06, there are no sample preservation and holding time guidelines. Dow 

recommends that sample preservation and holding time guidelines be validated and established. 

Another challenge of this method is the complex and vast requirements that one would need to prepare 

and maintain a laboratory environment to analyze samples at the part per quadrillion level, as presented in 

the method document. Section 5 contains many lengthy required processes required to maintain the 

laboratory for this level. This would be prohibitively expensive for many in the regulated community. 
2010 Methods Update Rule Response to Comments 69 March 2012 

Finally, Dow is concerned that the value of testing at these low part per quadrillion levels may not yield 

meaningful results. The value of testing at these low levels should be re-examined by EPA in that the 

toxicity data may not indicate that these levels would be of concern for environmental monitoring. 

II.C.9 ASTM D7574-09 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica, Inc. 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 166.1 - Paul Wiegand, National Council for Air and Stream Improvement, Inc. 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Comment 180 - Philip Yee, The Dow Chemical Company 

Summary of Comments: Three commenters were supportive of the addition of these methods. Two 

other commenters expressed concerns about the lack of validation data for specific industry wastewater 

matrices. 

Response: EPA thanks the commenters who expressed support for this method. This method has been 

tested by a single laboratory in several environmental waters, and may be useful for many applications. 

However, EPA has decided to postpone approval of the method for general use until completion of a full 

inter-laboratory validation study designed to fully characterize the performance of this method across 

multiple laboratories and matrices. EPA will provide an opportunity to comment on this method again if 

EPA considers it for approval at part 136 in a future rulemaking. As mentioned earlier (see response to 

comment II.C.8), EPA does not test every method in every matrix. 

Original Comment Text: 

The following commenters supported the addition of the new methods. 

Comment 79.1 Richard Burrows, TestAmerica, Inc. 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 169.1 Judith R. Morgan, American Council of Independent Laboratories 

Other comments: 

Comment 166.1 

Paul Wiegand 

National Council for Air and Stream Improvement, Inc. 

The proposed inclusion of these methods for general use is inappropriate because they have not been 

validated for use with certain wastewaters such as those from pulp and paper manufacturing. EPA should 

limit approval of their use to only matrices for which validation studies have been conducted. 

EPA proposes addition of ASTM D7574-09 for determination of BPA in environmental waters to Table 

IC. This method specifically states that it has “been investigated for use with surface water and secondary 

and tertiary POTW effluent samples therefore, it is applicable to these matrices only.” As with the 

previous proposed method, it has not been evaluated or validated for use in pulp and paper industrial 

wastewaters. 

Comment 180 

Philip Yee 

The Dow Chemical Company 
2010 Methods Update Rule Response to Comments 70 March 2012 

Similar to Method ASTM D7065-06, there is no sample preservation and holding time guidelines for 

Method ASTM D7574-09. Dow recommends that sample preservation and holding time guidelines be 

validated and established. 

II.C.10 ASTM D7485-09 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica, Inc. 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 166.1 - Paul Wiegand, National Council for Air and Stream Improvement, Inc. 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Summary of Comments: Three commenters were supportive of the addition of these methods. One 

other commenter expressed concerns about the lack of validation data for specific industry wastewater 

matrices. One commenter noted the proposal listed aquatic life criteria referred to in the proposal were 

only for saltwater, not freshwater and saltwater. 

Response: EPA thanks the commenters who expressed support for this method. This method has been 

tested by a single laboratory in several environmental waters, and may be useful for many applications. 

However, EPA has decided to postpone approval of the method for general use until completion of a full 

inter-laboratory validation study designed to fully characterize the performance of this method across 

multiple laboratories and matrices. EPA will provide an opportunity to comment on this method again if 

EPA considers it for approval at part 136 in a future rulemaking. With respect to the comment about 

validation data for specific industry wastewater matrices, see response to comment II.C.8. 

EPA agrees that the aquatic life criteria cited in the proposal were for saltwater organisms (e.g., an acute 

criterion of 7.0 ppb and a chronic criterion of 1.7 ppb) and thanks the commenter for noting this error. 

The corresponding freshwater criteria are higher (28 and 6.6 ppb, respectively), and the method would be 

appropriate for measurements in those ranges. At such time as EPA decides to promulgate this method, it 

will ensure that the criteria are correctly cited. 

Original Comment Text: 

The following commenters supported the addition of the new methods. 

Comment 79.1 Richard Burrows, TestAmerica, Inc. 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 169.1 Judith R. Morgan, American Council of Independent Laboratories 

Other comments: 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 

It is our understanding on the EPA website that the limits (7 & 1.7 ppb) are only for Saltwater Aquatic 

Life criteria, not for both Freshwater and Saltwater. Thus, should “Freshwater and” should be deleted? 

Please clarify. 

Comment 166.1 

Paul Wiegand 

National Council for Air and Stream Improvement, Inc. 
2010 Methods Update Rule Response to Comments 71 March 2012 

The proposed inclusion of these methods for general use is inappropriate because they have not been 

validated for use with certain wastewaters such as those from pulp and paper manufacturing. EPA should 

limit approval of their use to only matrices for which validation studies have been conducted. 

EPA proposes addition of ASTM D7574-09 for determination of BPA in environmental waters to Table 

IC. This method specifically states that it has “been investigated for use with surface water and secondary 

and tertiary POTW effluent samples therefore, it is applicable to these matrices only.” As with the 

previous proposed method, it has not been evaluated or validated for use in pulp and paper industrial 

wastewaters. 

 

EPA proposes addition of ASTM D7485-09 for determination of nonylphenol, p-tert-octylphenol, 

nonylphenol monoethoxylate, and nonylphenol diethoxylate in environmental waters to Table IC. This 

method has been investigated and is applicable for environmental waters, including seawater. The 

method states that environmental waters shall refer to water tested using the method. This method has not 

been validated for use in pulp and paper industrial wastewaters and therefore should not be approved for 

use in these matrices until a validation study has been conducted. 

II.C.11 Do not add ASTM D7066-04 or ASTM D7575-10 in Table IB

List of Comments: 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 129 - Anonymous Public Comment 

Comment 181.1 - Joe Boyd, Environmental Express 

Summary of Comments: Two commenters disagreed with EPA’s decision not to add one or both of 

these methods. A third commenter recognized EPA’s rationale for not including these methods, but 

offered suggestions for how the methods might be incorporated into part 136. 

Response: As noted in the proposal, EPA did not propose to include ASTM D7066-04 or ASTM D7575-

10 in Table IB for the method-defined parameter “oil and grease” or “hexane-extractable material.” 

Therefore, adding those methods to Part 136 is outside the scope of today’s rule. EPA recently published 

a Notice of Data Availability (NODA) on new data for one of these methods, specifically for ASTM 

Method D7575-10, and requested comment on whether the Agency should approve this method for the 

measurement of oil and grease (see 76 FR 77742, December 14, 2011). The Agency will make a decision 

on the approval or disapproval of this method once it reviews the public comments received in response 

to the NODA and will publish the final decision of its consideration of this method in a future Federal 

Register notice. Today’s final rule does not include ASTM D7066-04 or ASTM D7575-10. 

Original Comment Text: 

Comment 91.1 

Andrea Rex 

Massachusetts Water Resources Authority 

For oil and grease, this section explicitly DOESN’T propose for approval ASTM method D7575-10, 

which is based on solid phase extraction using a membrane and quantitation by infrared absorption of the 

membrane. We had occasion to try this method out with the method developer (OSS) and found it to be 

simple yet elegant. It worked well on method detection limit and precision and accuracy samples, but we 

weren’t able to do a larger study comparing the method to the approved method. We share the concern 

expressed by EPA about representative sampling—10 mL portion versus the entire contents of a 1-L 

sample. We suggest that an alternative would be to collect the sample directly on the membrane in the 

field. Clearly, any method based on solid phase extraction doesn’t lend itself well to solid samples. 
2010 Methods Update Rule Response to Comments 72 March 2012 

Comment 129 

Anonymous Public Comment 

As an individual who has performed both the previous freon method as well as the n-hexane method I 

have been exposed to these dangerous fumes. I read your documentation for why this specific method 

ASTM D7575 was not chosen as a viable alternative to EPA 1664 based on the fact that all oil and grease 

sampling techniques require an organic solvent. This breakthrough in the measurement of oil and grease 

should be adopted and the rationale that the method doesn't include a solvent is not in the best interest of 

science or the environment. 

Comment 181.1 

Joe Boyd 

Environmental Express 

The EPA has decided not to include ASTM method D7575-10 in Table IB mainly due to the fact that this 

method does not use the solvent n-hexane in the determination of oil & grease. Methods that are 

currently listed in Table IB (EPA 1664B, SM 5520B-2001, and SM 5520F-2001) do indeed list n-hexane 

as the solvent to use for extraction. However, all three of these methods reference “oil & grease” as a 

method defined parameter based on the use of hexane as the extraction solvent. This makes the analytes 

of interest “hexane extractable material”, or HEM rather than “oil & grease”. While both “HEM” and 

“oil & grease” can be construed as method defined analytes, HEM is much more specific in that the name 

itself implies that the analytes of interest must be extractable using hexane. “Oil & grease”, however, is a 

broader term and does not limit itself to any specific type of extraction. One must understand that no 

matter what extraction procedure is employed, the analytes of interest will always be a method defined 

parameter as the term “oil & grease” is truly indefinable. The continued use of the term “oil & grease” in 

Table IB for Parameter 41, however, leads to some confusion and brings into question the reasoning 

behind the EPA’s decision to limit the measurement of this parameter to hexane extractable material. 

Environmental Express, Inc. does not specifically endorse the product created by Orono Spectral 

Solutions Inc. (OSS) used in ASTM method D7575-10, however we would ask that the EPA continue to 

look at products that can make various analyses “greener”. The supporting data provided by OSS does 

seem to indicate an equivalent option for the determination of the parameter “oil & grease” and eliminates 

the risks created by the use of n-hexane. While ASTM method D7575-10 does not lead to the analyte of 

interest as HEM, it does provide an alternative extraction technique to determine “oil & grease”. The 

EPA has already demonstrated that it is willing to alter the definition of the end analyte of interest for the 

parameter of “oil & grease” by moving from Freon® to n-hexane, creating HEM. The EPA should keep 

the spirit of this philosophy alive in the move to greener methodologies and reconsider it’s stance on 

ASTM D7575-10. 

Section II.D Alternate Test Procedures (ATPs) 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica, Inc. 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 101.1 - NYSDEC, New York State Department of Environmental Conservation 

Comment 106.1 - Charles Boepple, Upper Occoquan Service Authority 

Comment 116.1 - Wendy Harding and Mala Burton, Joint Water Environment Association and Virginia 

American Water Works Association 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 
2010 Methods Update Rule Response to Comments 73 March 2012 

Comment 171.1 - Lola Guerra, Henrico County DPU 

Summary of Comments: Commenters were generally supportive of the approval of the specific ATPs 

listed in the proposal. However, several commenters were concerned that the approvals were limited to 

specific vendors, rather than to the technique, e.g., luminescent determination of dissolved oxygen. 

Several commenters suggested that EPA publish a list of all approved ATPs for all parameters. Other 

commenters raised concerns about the status of previously approved ATPs relative to the changes in 

approval for various versions of Standard Methods and ASTM methods. 

Response: EPA appreciates the comments in support of the approval of these alternate test procedures 

(ATPs). With respect to the concern that EPA is approving methods limited to specific vendors, EPA 

approves test methods, not the specific technologies (i.e., equipment). Methods being approved for 

measurement of dissolved oxygen using luminescent-based sensor technology include methods developed 

by vendors and submitted as ATPs, as well as ASTM Method D888-09 (C), which does not specify the 

use of equipment from a specific manufacturer. Where specific vendors are mentioned, those vendors 

developed methods that include use of their equipment and submitted them for approval as ATPs. The 

use of equivalent equipment is not prohibited and falls within the flexibility allowed at 40 CFR Part 

136.6. 

Methods approved as ATPs for nationwide use are proposed and promulgated in the Federal Register. 

These methods are then listed in the tables of approved methods at 40 CFR Part136 or in industry-specific 

effluent limitation guidelines. 

Withdrawal of older versions of VCSB methods such as Standard Methods or ASTM methods does not 

affect the status of alternative methods (ATPs) for which letters have been issued stating that the methods 

are acceptable versions of the VCSB methods. Where older versions of VCSB methods have been 

withdrawn, the newer versions are equivalent to the older versions. Therefore, methods that were 

determined to be acceptable versions of the older methods are acceptable versions of the newer versions. 

Further, updated versions of test methods that have been reviewed, and for which letters were issued 

stating that they are acceptable versions of an approved method, fall within the flexibility allowed at part 

136.6. These methods do not require that new performance data be generated if the changes are merely 

editorial (e.g., clarifications) and do not affect the performance of the method. However, in cases where 

the updated method includes changes in the chemistry of the method, such as changes to buffers, data 

must be available from the vendors that document that the methods meet the requirements specified in 

part 136.6. 

Original Comment Text: 

The following commenters supported the addition of the new ATP methods. 

Comment 79.1 Richard Burrows, TestAmerica, Inc. 

Comment 91.1 Andrea Rex, Massachusetts Water Resources Authority 

Comment 101.1 NYSDEC, New York State Department of Environmental Conservation 

Comment 117.1 Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 169.1 Judith R. Morgan, American Council of Independent Laboratories 

The following commenters had the same (following) comment regarding the inclusion of Luminescence 

based measurements for Dissolved Oxygen. 

Comment 106.1 Charles Boepple, Upper Occoquan Service Authority 

Comment 116.1 Wendy Harding and Mala Burton, Joint Water Environment Association and 

Virginia American Water Works Association 

Comment 171.1 Lola Guerra, Henrico County DPU 
2010 Methods Update Rule Response to Comments 74 March 2012 

Comment: We applaud the inclusion of Luminescence based measurements for Dissolved Oxygen. We 

assume that although specific manufacturers of the LDO technology were mentioned by name, those that 

were not (e.g. SKALAR, YSI, Orion) are also acceptable? 

Recommendation 1: Include the phrase "or equivalent" when mentioning trade names so that it is clear 

that products from other manufacturers using the same technology are also acceptable. 

Recommendation 2: Provide an inclusive list of all approved ATP methods and their effective publication 

dates. EPA should provide this list of approved ATPs on the EPA website and update it routinely as new 

methods are approved so that the regulated community will understand all the available methods for 

regulatory monitoring. 

Other comments: 

Comment 132.1 

Paula Hogg 

Hampton Roads Sanitation District 

Comment/Recommendation HRSD supports the approval of Optical Probes for DO measurement by 

multiple methods when supported by QA/QC data. 

It is unclear if previously approved ATPs linked to Standard Method Editions are still accepted. For 

example - are Hach methods previously given an accepted ATP and deemed equivalent to SM 18th 

Edition still approved although edition numbers will be removed with the publication of this MUR or 

methods are updated to a more recent version? 

Recommendation: Specifically list ATP methods separately as part of 40 CFR Part 136 as approved. 

Comment 164.1 

Mark Haley 

Hopewell Regional Wastewater Treatment Facility 

Significant changes have been proposed in the Method Update Rule (MUR) regarding which editions of 

Standard Methods (SM) are approved for use. Some of the changes between the different editions are 

significant and not necessarily improvements when comparing earlier editions to the most recent. 

Acceptability and/or approval to changes or updates to vendor methods previously deemed "equivalent" 

to 40CFR Part 136 methods is not addressed. 

Comment: Some of the changes between the different editions are significant and not necessarily 

improvements when comparing earlier editions to the most recent. Since methods have been updated to 

the latest version through this proposed MUR, it is unclear of how this impacts vendor methods 

previously approved by EPA as equivalent to one listed in 40CFR 136 (for example: Lachat Methods for 

TKN and NH3). Often, these methods are updated by the vendors and it is unclear if these updated 

methods are still considered equivalent by EPA. 

Questions include: 

• Since the previous letters referenced older versions of the approved methods, will vendors need to 

obtain updated letters from EPA and have information and data required for flexibility? 

• What documentation will a laboratory need to have to demonstrate that the correct version of a 

vendor method is approved for Clean Water Act monitoring? 

Recommendations 
2010 Methods Update Rule Response to Comments 75 March 2012 

• Allow all currently approved versions of Standard Methods as listed in 40CFR 136 (i.e. 18th 21 51 -

Editions) to remain approved and allow the continued use of said versions. 

• Previously approved vendor methods (by EPA letter stating equivalency) need to be listed in 40CFR 

Part 136. If a vendor makes changes to an EPA equivalent method, then EPA must require vendors to 

notify them of changes and provide supporting QA/QC and EPA should publish these methods in 

40CFR Part 136. 

Comment : For example, are previously approved ATP HACH methods (deemed equivalent to SM 18th 

Edition) still approved I) although edition numbers will be removed with the publication of this MUR or 

2) as methods are updated to a more recent version? 

Recommendations: List ATP methods separately as part of 40CFR Part 136 as approved and/or specify 

any previously approved ATPs using SM editions which may no longer be listed, but are still approved 

for use. 

II.D.1 Hach Method 10360 

List of Comments: 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 118 - Andrew G. Wendell, ClearWater Laboratory 

Comment 177.1 - Novelle C. Stokes, South Central Wastewater Authority 

Summary of Comments: Commenters were supportive of the inclusion of Hach Method 10360, but 

several were concerned that its approval for BOD and CBOD was misleading, since this technique is only 

for the determination of dissolved oxygen as a part of the BOD or CBOD measurement. One commenter 

suggested that the generic technique be approved, and not the methods from specific vendors. 

Response: EPA appreciates comments received in support of the approval of these alternate test 

procedures. EPA will clarify the intent to allow the use of Hach Method 10360 and other luminescent 

based sensor methods for measurement of dissolved oxygen in conjunction with the methods approved 

for measurement of biochemical demand (BOD) and carbonaceous biochemical oxygen demand (CBOD) 

by revising footnote 63 of Table IB to the following: “Hach Method 10360, ‘Luminescence Measurement 

of Dissolved Oxygen in Water and Wastewater and for Use in the Determination of BOD5 and cBOD5, 

Revision 1.2 dated November, 2011.’ Available from Hach Company, 5600 Lindbergh Drive, Loveland, 

CO 80539, Telephone: 970–669–3050. This method may be used to measure dissolved oxygen when 

performing the methods approved in Table IB for measurement of biochemical oxygen demand (BOD) 

and carbonaceous biochemical oxygen demand (CBOD).” With respect to approval of the generic 

technique rather than methods from specific vendors, as mentioned earlier in response to II.D, EPA does 

not require the use of specific equipment. EPA approves the method, not the technology. 

Original Comment Text: 

The following commenters supported the addition of the new methods. 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 118 Andrew G. Wendell, ClearWater Laboratory 

Comment 177.1 Novelle C. Stokes, South Central Wastewater Authority 

Other comments: 

Comment 113.1 

Susan E. Butts 
2010 Methods Update Rule Response to Comments 76 March 2012 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

The Hach LDO method 10360 is described in footnote 63 of Table IB as approved for BOD and CBOD 

analysis. This is a dissolved oxygen procedure, and does not contain the required QC or procedures for 

performing BOD analyses. As such, it should only be listed as a procedure for Dissolved Oxygen, and not 

BOD and CBOD. If the intent was to use this method in conjunction with the BOD method, then this 

should be stated in a footnote. 

Comment 177.1 

Novelle C. Stokes 

South Central Wastewater Authority 

Recommendation: Efforts should be made to reduce the number of direct references to individual vendors 

and more emphasis placed on critical review of the methodology. Vendor names are mentioned when 

approving methods developed by vendors and submitted for approval as alternate test procedures. 

II.D.2 In-Situ Incorporated’s Method 1002-8-2009 

II.D.3 In-Situ Incorporated’s Method 1003-8-2009 

II.D.4 In-Situ Incorporated’s Method 1004-8-2009 

No comments were received for these methods. EPA is adding these methods as proposed. 

II.D.5 Mitchell Method M5271 

II.D.6 Mitchell Method M5331 

List of Comments: 

Comment 166.1 - Paul Wiegand, National Council for Air and Stream Improvement, Inc. 

Summary of Comments: One commenter expressed concern about the approval of these turbidity 

methods because they do not apply to colored wastewaters. 

Response: Methods M5271 and M5331 have the same limitations as the approved EPA Method 180.1, 

Revision 2.0. The applicable range of 0-40 NTU is the same in all three methods. EPA Method 180.1, 

Revision 2.0 also lists color as an interference. Approval of these methods for general use is intended to 

give the regulated community additional options when choosing approved methods for use in compliance 

monitoring. Approval does not impose a requirement for use of these methods since other methods are 

approved for use. 

Original Comment Text: 

Comment 166.1 

Paul Wiegand 

National Council for Air and Stream Improvement, Inc. 

The proposed inclusion of these methods for general use is inappropriate because they are not suitable for 

use with colored wastewaters such as those from some pulp and paper mills. EPA should clearly state the 

limitations for their use. 

EPA proposes Mitchell Methods M5271 and M5331 for measuring turbidity in wastewater for nationwide 

use. M5271 is titled “Determination of Turbidity by Laser Nephelometry” and M5331 is titled 

“Determination of Turbidity by LED Nephelometry.” Both methods specifically state (Section 1.0 of 

each) that they cover determination of turbidity in drinking, ground, surface, and any colorless water with 
2010 Methods Update Rule Response to Comments 77 March 2012 

a turbidity of less than 40 NTU. These methods are not suitable for determination of turbidity in colored 

wastewaters and should not be approved for this purpose. 

Section II.E Clarifications and Corrections to Previously Approved Methods 

II.E.1 Immediate Filtration of Samples for Orthophosphate 

List of Comments: 

Comment 82 - LeeAnna Hutchings, Great Salt Bay Sanitary District, Damariscotta, ME 

Comment 88.1 - Susan D. Hill, Wisconsin State Laboratory of Hygiene 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 106.1 - Charles Boepple, Upper Occoquan Service Authority 

Comment 109.1 - Andre Brousseau, Maine Wastewater Control Association 

Comment 112.1 - Colin Elliott, King County Environmental Lab 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 116.1 - Wendy Harding and Mala Burton, Joint Virginia Water Environment Association and 

Virginia American Water Works Association 

Comment 118 - Andrew G. Wendell. ClearWater Laboratory 

Comment 123 - Vincent Sapienza, Bureau of Wastewater Treatment, New York City Department of 

Environmental Protection 

Comment 124.1 - Thomas Tourje, Augusta County Service Authority 

Comment 126.1 - Sterling Pierce, Maine Department of Environmental Protection 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 134.1 - Josh Kathrinus, American Bottoms Regional Wastewater Treatment Facility 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 166. 1- Paul Wiegand, National Council for Air and Stream Improvement, Inc. 

Comment 177.1 - Novelle C. Stokes, South Central Wastewater Authority 

Comment 177.1 - Novelle C. Stokes, South Central Wastewater Authority 

Comment 180 - Philip Yee, Dow Chemical Company 

Summary of Comments: Some commenters supported the clarification of the requirement for 

immediate filtration of samples for orthophosphate. Other commenters viewed this as a burdensome new 

requirement. Many commenters questioned its application to composite samples. Some commenters 

asked where this clarification would be placed in part 136. 

Response: The proposed clarification of the requirement for immediate filtration of samples to be 

analyzed for orthophosphate was prompted by an email inquiry that was received by EPA on November 

9, 2009. The inquiry asked about manual grab samples collected and then combined to make a 24-hour 

composite sample for NPDES permit compliance and included three specific questions. 

The first question asked if each grab sample must be filtered within 15 minutes of collection, or if 

filtration may be delayed until sometime after the final manual grab sample is obtained. EPA’s response 

at that time was that each grab sample must be filtered within 15 minutes of collection, as indicated in 

Table II at 40 CFR Part 136.3. 

The second question asked if filtration may be delayed until the final grab sample is obtained and whether 

or not the 15-minute filtration requirement applied to the individual grab samples or to the composite 

sample. EPA’s response was that filtration may not be delayed until the final grab sample is collected and 

that each grab sample must be filtered upon collection. 
2010 Methods Update Rule Response to Comments 78 March 2012 

Finally, the third question asked how long the grab samples could be held prior to combining them to 

make a composite sample. EPA’s response was that the grab samples may be held for compositing up to 

the 48-hour holding time prior to beginning analysis. 

In summary, EPA’s November 2009 response to the three-part question was: 

• Each grab sample must be filtered within 15 minutes of collection to prevent orthophosphate 

formation. 

• Filtration may not be delayed until the final grab sample is collected; each grab sample must be 

filtered upon collection. 

• However, the filtered grab samples may be held for compositing up to the 48-hour holding time. 

EPA notes that the requirement to filter samples immediately upon collection is based upon research 

conducted by the United States Geological Survey (USGS) on grab samples to be analyzed for 

orthophosphate. The purpose of the immediate filtration requirement in orthophosphate measurements is 

to ensure that the form of phosphorus measured is the dissolved, or bio-available, form of 

orthophosphorus (i.e., that which passes through a 0.45-micron filter), hence the requirement to filter the 

sample immediately upon collection. This filtration excludes any particulate forms of phosphorus that 

might hydrolyze into orthophosphorus in a slightly acidic sample during the allowed 48-hour holding 

time. 

EPA proposed the clarification to make the information in EPA’s November 2009 responses more widely 

available. As noted in many of the comments, the clarification applies to grab samples and does not 

address samples collected using an automatic sampler. Therefore, permitting authorities should consider 

the filtration issue when allowing the use of automated equipment to collect 24-hour composite samples, 

as well as considering any potential compliance impacts on the final orthophosphate results if samples are 

not filtered until a 24-hour composite sample is collected. EPA has not considered the application of this 

method to compositing at this time. 

In response to comments, EPA has added a footnote to Table II in part 136 in the final rule regarding the 

immediate filtration requirement (footnote 24), " The immediate filtration requirement in orthophosphate 

measurement is to assess the dissolved or bio-available form of orthophosphorus (i.e., that which passes 

through a 0.45-micron filter), hence the requirement to filter the sample immediately upon collection (i.e., 

within 15 minutes of collection)." 

Original Comment Text: 

The following commenters had the same (following) comment regarding whether or not sample filtration 

applies to 24 hour composite samples. 

Comment 106.1 Charles Boepple, Upper Occoquan Service Authority 

Comment 116.1 Wendy Harding and Mala Burton, Joint Virginia Water Environment Association 

and Virginia American Water Works Association 

Comment 124.1 Thomas Tourje, Augusta County Service Authority 

Comment 171.1 Lola Guerra, Henrico County DPU 

Comment: There is confusion regarding interpretation of this requirement in regard to composite samples. 

Lem Walker (EPA) has verbally indicated that the rule applies to grab samples only, not 24-hr composite 

samples pulled with an auto-sampler. He acknowledged that filtering of the individual increments of a 24-

hr composite sample would not be practical or possible. 

Recommendation: Please clarify that 24-hr composite samples would only need to be filtered within 15 

minutes of the end of the composite sample period. 
2010 Methods Update Rule Response to Comments 79 March 2012 

Other comments: 

Comment 82 

LeeAnna Hutchings 

Great Salt Bay Sanitary District, Damariscotta, ME 

The nutrient criteria as of yet has not passed in Maine, our facilities are not requirement [sic] to test for 

orthophosphate. It is likely that many facilities will have it in future permits (ours are due for review 

now). The clarification will require each aliquot (grab) of the composite be filtered within 15 minutes of 

collection prior to compositing the 24-hour sample. The definition of a composite as defined in the 

conditions attached to our permit. “Composite sample means a sample consisting of a minimum of eight 

grab samples collected at equal intervals during a 24 hour period (or a lesser period as specified in the 

section on monitoring and reporting) and combined proportional to the flow over that same time period.” 

We have 5 full time employees including our office manager to run a water co., two treatment facilities, 

maintain11 pump stations and 40 miles of pipe. We do not have the money or man power for three shifts, 

so the grab sample can be filtered within 15 minutes of collection prior to compositing on phosphorus 

monitoring days? 

Comment 88.1 

Susan D. Hill 

Wisconsin State Laboratory of Hygiene 

Section E.1—this paragraph in the summary clarifies the purpose of the immediate filtration requirement 

in orthophosphate measurements, but where will this information be documented in the new revision of 

40 CFR part 136? 

Comment 91.1 

Andrea Rex 

Massachusetts Water Resources Authority 

Clarifications and Corrections to Previously Approved Methods. We applaud EPA for restating that field 

filtration is required for ortho-phosphate samples because some of our laboratory’s clients have been 

reluctant to take this on. 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 

Orthophosphate 

Comment: Each grab sample must be filtered within 15 minutes of collection to prevent orthophosphate 

formation. However, the filtered grab samples may be held for compositing up to the 48-hour holding 

time. This is a reasonable proposal. 

Comment 109.1 

Andre Brousseau 

Maine Wastewater Control Association 

The EPA proposes to clarify, and thus require, immediate filtration upon collection of each sample, 

including each separately collected aliquot of a composite sample, for analysis of orthophosphate. 

MWWCA finds this an unreasonable and egregious regulatory burden on permittees subject to the Clean 

Water Act. 
2010 Methods Update Rule Response to Comments 80 March 2012 

If it is the EPA's intent to require immediate filtration, then EPA should also require that orthophosphate 

be done on grab samples only. In 40 CFR 403.12, EPA has stipulated that for compliance by Industrial 

Users with applicable Pretreatment Standards and Requirements, grab samples must be used for pH, 

cyanide, total phenols, oil and grease, sulfide, and volatile organic compounds. MWWCA believes EPA 

should apply the same discretion in tins case and require only grabs samples for orthophosphate. 

EPA's s proposed clarification would make it impossible to collect an automatic flow-proportional 

composite sample for orthophosphate and impractical to collect an automatic 24-hour time-proportional 

composite sample. There is no current technology for automatically filtering 96 separate aliquots of a 

composite sample every fifteen minutes. Even if technology were available, POTWs and other permittees 

would need to collect at least two separate composite samples; one for orthophosphate and the second for 

other permit composite sample requirements. Purchase of additional "high tech" samplers to collect one 

additional parameter would be an economic hardship for many small treatment plants. 

To require permittees to do manual sampling for 24 hour composites would be a significant cost and 

regulatory burden to small entities and municipalities, as well as larger entities and municipalities, 

because most POTWs rely on automatic samplers, and most POTWs do not have operators or laboratory 

personnel available 24 hours per day to collect samples by hand EVERY FIFTEEN MINUTES. POTWs 

would also be required to invest in equipment to collect at least two separate flow-proportional 

composites, where only one is now required. Again, MWWCA believes that EPA should require that only 

grab samples be taken for orthophosphate. 

Inability to collect a 24-hour composite by automatic sampler would also make it impossible or 

impractical to assess and compare the orthophosphate data with other permit parameters, such as TSS or 

BOD. Therefore, it may be necessary for EPA to clarify, that when it is necessary to collect a sample for 

comparison with other composite parameters, the permittee should analyze for total phosphorous. 

Comment 112.1 

Colin Elliott 

King County Environmental Lab 

Comment: This change will eliminate the ability to collect Orthophosphate samples as continuous 

composites since the composite would exceed the filtration holding time. The requirement to filter 

Orthophosphate samples within 15 minutes should be described in Table II (as a footnote) in a similar 

manner to dissolved metals. 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

The summary of the orthophosphate filtration clarification located in Section E.1 of the discussion cannot 

be clearly found in the proposed rule. The summary provides enough information to describe the change, 

but the rule itself is not clear and needs to reflect what is written in the section E.1 of the summary. 

Comment 118 

Andrew G. Wendell 

ClearWater Laboratory 

I am opposed to this change. Where many facilities are required to analyze for dissolved orthophosphate 

on a composite effluent sample, and where a composite sample may consist of 8 up to 96 (at a frequency 

of 1 every 15-minutes) sub-samples, this requirement has many onerous and counter-productive facets: 1) 
2010 Methods Update Rule Response to Comments 81 March 2012 

my biggest concern is that every sub-sample handled has the potential for contamination and thusly 

broadens the potential for error and lessens accuracy in terms of measuring a true orthophosphate value, 

2) the cost of individually filtering 8 to 96 samples could range from a couple hundred dollars up to or 

even exceeding $1000 per sample (compared to about $50/sample), 3) for facilities that collect samples 

on a flow-paced basis, an employee would almost have to be dedicated to the purpose of watching the 

flow and sampler so that when a sample was collected (not always predictably) they would be instantly 

available to filter the sample, 4) in many cases, a facility would be required to staff personnel over a 24-

hour period for the sake of filtering each sub-sample aliquot (whether it is flow-paced or not), 5) the cost 

in time and dollars would likely be extremely high compared to the ‘gain’ of data when comparing 

dissolved orthophosphate results in the proposed regulation vs. simply filtering the composite sample 

once at the end of the composite period, especially when you consider the enormous increase in the 

potential for error due to contamination as I mention in my comment #1. 

Comment 123 

Vincent Sapienza 

Bureau of Wastewater Treatment, New York City Department of Environmental Protection 

EPA is clarifying the purpose of the immediate filtration requirement in orthophosphate measurements, 

which is to assess the dissolved or bioavailable form of orthophosphorus (i.e., that which passes through a 

0.45 micron filter), hence the requirement to filter the sample immediately upon collection. This filtration 

excludes any particulate forms of phosphorus that might hydrolyze into orthophosphorus in a slightly 

acidic sample during the allowed 48 hour holding time. Each grab sample must be filtered within 15 

minutes of collection to prevent orthophosphate formation. Specifically, filtration may not be delayed 

until the final grab sample is collected; each grab sample must be filtered upon collection. However, the 

filtered grab samples may be held for compositing up to the 48-hourholding time. 

NYCDEP does not agree with this proposal as there is no significant tangible gain to be realized by 

requiring labs to filter the samples within 15 minutes after the sample collection. EPA's concern is based 

on the theory that, in the absence of filtration during the holding time of 48 hours, particulate forms of 

phosphorus may hydrolyze into Ortho-P in slightly acidic samples. This theory has virtually no merit 

when tested in actual samples. Our comparison study indicates that the difference is analytically 

insignificant as more than 99%ofthe samples for NPDES compliance have pH values between6.8 and 7.2. 

This clarification would mean that, since grab samples must be filtered within 15 minutes of sample 

collection, treatment plants would not be able to use auto-samplers for sample collection for reporting of 

Ortho-P. Auto samplers allow us to get more representative influent and effluent samples and reduce the 

numbers of sample bottles received by process labs. In addition, if the permittee must also report results 

for Total Phosphorus and other parameters, samples can be collected using an auto-sampler. Under the 

circumstances, if we need to establish a correlation between Ortho-P and Total Phosphorus results, we 

will be unable to do so because there will be two different composite samples. We ask that EPA 

reconsiders this position because the requirement will provide no real gain to the science and analysis. 

Comment 126.1 

Sterling Pierce 

Maine Department of Environmental Protection 

The EPA is proposing to require that samples scheduled for the analysis of orthophosphate, be filtered 

immediately after collection of each sample, including each aliquot of a composite sample. This will be 

overly burdensome on the permit holders currently required be their permits to obtain a composite sample 

for orthophosphate. Maine DEP has been requiring licensee’s to obtain composite samples for 

orthophosphate as part of their required monitoring. This new clarification / requirement would be overly 

burdensome on the license holder because there is no automated technology for sample filtration that 

could be combined with the use of the composite sampler. 
2010 Methods Update Rule Response to Comments 82 March 2012 

 

The proposed requirement would make it impossible to collect a flow proportioned composite sample for 

orthophosphate that could be compared to other operational parameters such as total suspended solids or 

biochemical oxygen demand using an automatic composite sampler. The only way to collect a 

comparable composite sample would be to collect and filter an aliquot for the orthophosphate analysis 

each time the automatic sampler collected an aliquot for the BOD and TSS analysis. Since very few of 

the wastewater facilities in Maine are staffed on a 24-hour basis, the collection of a representative 

composite sample for orthophosphate analysis is, at best, onerous and, in reality, impossible. 

Comment 132.1 

Paula Hogg 

Hampton Roads Sanitation District 

Immediate filtration for orthophosphate is required for grab samples and filtered grab samples may be 

held for compositing for up to 48 hours, which is the sample holding time. 

Comment 

It is unclear if this requirement is suggesting that only grab samples can be collected for orthophosphate 

analyses or if individual grab samples must be collected and filtered immediately upon collection in order 

to complete a composite sample. 

Typically, a composite sample consists of individual aliquots (either flow weighted or timed) and the 

sample is not complete until the end of the compositing period. If the rule is implying individual filtration 

of each aliquot, technology does not exist for in-line filtration of individual aliquots in cases where 

autosamplers are employed. Is it the intent of this requirement to preclude the collection of samples using 

automated equipment and to require manual collection and filtration? Manual collection and filtration of 

multiple grabs will increase the potential for error and increase the risk of sample contamination due to 

the number of times the sample must be handled throughout the collection period. Furthermore, data to 

support this requirement has not been provided. 

While reasoning states that conversion of particulate forms of phosphorous into orthophosphate occurs in 

slightly acidic conditions, the term "slightly" acidic is not defined and there is no data presented to 

support this change. 

Recommendation: Recommend filtration at the end of composite period as currently required. Clarify 

the statement in the MUR to allow use of automated sampling equipment for composite sampling with 

filtration at the end of the composite period. 

Comment 134.1 

Josh Kathrinus 

American Bottoms Regional Wastewater Treatment Facility 

The preamble is unclear whether the requirement for a 0.45 micron filter for testing ortho-P applies to all 

methods approved for ortho-P, or only the methods solely used for ortho-P. Also, we could not find in 

Section 136.3 the language is that states the 0.45um filtration is required. 

Comment 164.1 

Mark Haley 

Hopewell Regional Wastewater Treatment Facility 

Comment: It is unclear if this requirement is suggesting that only grab samples can be collected for 

orthophosphate analyses, or if individual grab samples must be collected and filtered immediately upon 

collection in order to complete a composite sample. 
2010 Methods Update Rule Response to Comments 83 March 2012 

Typically, a composite sample consists of individual aliquots (either flow weighted or timed) and the 

sample is not complete until the end of the compositing period. If the rule is implying individual filtration 

of each aliquot, technology does not exist for in-line filtration of individual aliquots in cases where 

autosamplers are employed. Is it the intent of this requirement to preclude the collection of samples using 

automated equipment and to require manual collection and filtration? Manual collection and filtration of 

multiple grabs will increase the potential for error and increase the risk of sample contamination due to 

the number of times the sample must be handled throughout the collection period. Furthermore, data to 

support this requirement has not been provided. While reasoning states that conversion of particulate 

forms of phosphorous into orthophosphate occurs in slightly acidic conditions, the term "slightly" acidic 

is not defined and there is no data presented to support this change. 

Recommend filtration at the end of composite period as currently required. Clarify the statement in the 

MUR to allow use of automated sampling equipment for composite sampling with filtration at the end of 

the composite period. 

Comment 166. 1 

Paul Wiegand 

National Council for Air and Stream Improvement, Inc. 

The proposed clarification to require filtration of effluents within 15 minutes of sample collection for 

analysis of bioavailable phosphorus is impractical and no data supporting this requirement were provided. 

EPA should provide the data or change this requirement to a more reasonable period such as one hour. 

Section E1 of the proposal states that “EPA is clarifying the purpose of the immediate filtration 

requirement in orthophosphate measurements, which is to assess the dissolved or bio-available form of 

orthophosphorus (i.e., that which passes through a 0.45 micron filter), hence the requirement to filter the 

sample immediately upon collection.” EPA proposes that “each grab sample must be filtered within 15 

minutes of collection to prevent orthophosphate formation.” This requirement may be difficult to comply 

with in situations where the laboratory is located remotely from the sampling location. As the majority of 

approved orthophosphate methods require filtration of 50 mL of sample, such facilities would be required 

to carry filtration equipment, including vacuum sources, into the field and perform the filtration upon 

collection. Many wastewaters, including those from the pulp and paper industry, would be difficult to 

filter to this degree using field sampling techniques such as syringe filters. 

Comment 177.1 

Novelle C. Stokes 

South Central Wastewater Authority 

Comment: Typically NPDES permits are issued with requirements for 24 hr composite sampling of 

Orthophosphate. Treatment plants using both manual and automated sampling equipment currently 

preserve and analyze Orthophosphate samples as defined in Table II based on a single sample quantity. 

The proposed language would force the manual collection and immediate filtration of multiple grab 

samples (as little as 4 and as many as 96 individual samples) throughout the composite period. 

Regardless of the operator time required to meet such an excessively stringent requirement, this 

modification would increase the potential for sampling error and risk of sample contamination. 

Recommendation: Reissue all current NPDES permits to define a 24 hour Orthophosphate composite 

sample as “an average of 4 (or more) individual sample aliquots collected during a 24 hour period.” For 

example, each of the 4 grabs collected during the composite period would be analyzed separately and the 

results averaged for compliance reporting. 

The proposed revision reduces the comparability of Orthophosphate data with historical records and other 

parameters collected by automatic sampling equipment. 
2010 Methods Update Rule Response to Comments 84 March 2012 

Recommendation: Grant an exemption to permittees currently using automatic sampling equipment as 

technology does not currently exist for in-line filtration of samples. 

Comment 180 

Philip Yee 

The Dow Chemical Company 

Dow is concerned that the requirement for immediate filtration upon sample collection of orthophosphate 

samples would result in an excessive burden to the regulated community. The immediate filtration 

requirement would require the purchase and maintenance of field filtration equipment. This requirement 

would result in significant ongoing costs to the regulated community. Subsequently, Dow recommends 

that this requirement be eliminated. 

II.E.2 Correct missing citations for microbial methods applicable to ambient water monitoring 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica, Inc. 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 107.1 - Patsy Root, IDEXX Laboratories 

Comment 112.1 - Colin Elliott, King County Environmental Lab 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Summary of Comments: Commenters supported the corrections, but several suggested other methods 

that should be added to the list of those approved for ambient monitoring. One commenter asked why 

some methods previously listed as approved were not so listed in the proposal. 

Response: EPA thanks the commenters for supporting the corrections. Standard Method 9223B has not 

been added to Table IH because it was not validated in ambient water. Standard Methods 9230 B-2007 

and 2930 C-2007 were included in Table IH for ambient waters in the proposal and are included in the 

final ruling. EPA’s Alternate Test Procedures program may be used to evaluate new and alternate 

methods which require method validation data to demonstrate comparability and thus suitability of such 

methods. See response in section II.A.3.e for more details on the ATP program. 

Regarding the comment on the non-listing of approved methods in the proposal, see response in Section 

II.F. 

Original Comment Text: 

The following commenters supported the correction addition of the new methods. 

Comment 112.1 Colin Elliott, King County Environmental Lab 

Comment 132.1 Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 Mark Haley, Hopewell Regional Wastewater Treatment Facility 

The following commenters had the same (following) comments regarding the addition of method 9223B 

for total coliform analysis, and the addition of SM 9230-2007. 

Comment 79.1 Richard Burrows, TestAmerica, Inc. 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment: We suggest that method 9223B should be included for total coliform analysis. It is faster than 

the 9221B method, allowing results to be generated in a timely manner. 
2010 Methods Update Rule Response to Comments 85 March 2012 

Comment: Standard Methods method 9230-2007 should be included here 

Other comments: 

Comment 107.1 

Patsy Root 

IDEXX Laboratories 

Page 58039: Commend EPA on the separation of methods for wastewater and ambient water; the addition 

of Table IH adds much clarity for Ambient water methods versus Wastewater methods 

Comment 164.1 

Mark Haley 

Hopewell Regional Wastewater Treatment Facility 

Why were some methods approved in the previous MUR not listed in the Proposed MUR? 

We recommend EPA implement a systematic approach to evaluate new methods requiring method 

validation data to demonstrate suitability of method

Section II.F Changes to Required Containers, Preservation Techniques, and Holding 

Times in Table II 

List of Comments: 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 104 - Nilda Cox, MWH Global 

Summary of Comments: One commenter supported the changes to Table II for BOD in particular. 

Another commenter was concerned about other Part 136 tables that were not cited in Table II. 

Response: EPA appreciates the comment in support of the addition of the language stating that the 

instructions in Table II take precedence over information in specific methods or elsewhere. However, this 

information was added in a previous rule and is not a new requirement under today’s rulemaking. Thus, 

the applicable holding time for BOD continues to be 48 hours, as specified in Table II. 

As is common practice in the Federal Register, the version of Table II that appeared in the proposed rule 

only listed those parameters for which changes were being proposed. No changes were proposed to the 

required sample containers, preservation techniques and holding times for the parameters listed in the 

tables that were not included in the proposal. The final rule includes the complete Table II. 

Original Comment Text: 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 

Comment: According to the proposed rule, Table II specifies the 48 hours BOD holding time while part 

136 method recommends 24 hours. In this instance, EPA proposes that Table II instructions take 

precedence. This change is long overdue and welcome. 

Comment 104 

Nilda Cox 

MWH Global 
2010 Methods Update Rule Response to Comments 86 March 2012 

Table II (58066) - "Required Containers, Preservation Techniques and Holding Times", the proposed 

MUR does not have the following Tables and Footnotes found in previous CFR versions: 

Table IB- Inorganic tests, Metals 

Table IC- Organic Tests 

Table ID- Pesticides Tests 

Table IE- Radiological tests 

II.F.1 Table II takes precedence over other instructions, unless approved by permitting authority 

List of Comments: 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 101.1 - NYSDEC, New York State Department of Environmental Conservation 

Comment 107.1 - Patsy Root, IDEXX Laboratories 

Comment 108.1 - George Noguchi, U.S. Department of the Interior, U.S. Fish and Wildlife Service 

Comment 109.1 - Andre Brousseau, Maine Wastewater Control Association 

Comment 112.1 - Colin Elliott, King County Environmental Lab 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Summary of Comments: Commenters generally supported the clarification that Table II takes 

precedence over other instructions. However, commenters were generally opposed to the proposed 

changes that would allow permitting authorities to approve changes to the Table II requirements. Among 

the concerns raised are the burden that this requirement would impose on the permitting authorities to 

review and approve changes, as well as the likelihood that such changes would present a burden for 

laboratories that work across states, and the inconsistency that would likely result from the issuance of 

such variances by the permitting authorities. Some commenters stated support for the applicability of 

ATP-style documentation for holding time changes. One commenter suggested that Table II should be 

updated to be consistent with SW-846 preservation requirements. 

Response: EPA appreciates the comments in support of the language stating that the instructions in 

Table II take precedence over information in specific methods or elsewhere. However, this information 

was added in a previous rule and is not a new requirement under today’s rulemaking. 

In response to comments received on the proposed language leaving the nature, timing, and extent of the 

required documentation for approval of a change request for Table II parameters to the discretion of the 

permitting authority, EPA has reconsidered this proposed change and has removed the proposed language 

from the final rule. The revised language may be found in section 136.3(e) of the rule. 

Regarding updating Table II for consistency with SW-846 preservation requirements, EPA strives to be 

consistent with other preservation and holding time requirements but these requirements may be different 

for the various Agency programs because the matrices of concern are different. 

EPA also refers readers to section III.I of the preamble for today’s rulemaking for additional information 

regarding Table II requirements. 

Original Comment Text: 

Comment 91.1 

Andrea Rex 

Massachusetts Water Resources Authority 
2010 Methods Update Rule Response to Comments 87 March 2012 

We applaud EPA for clearly stating that the required containers, preservation techniques, and holding 

times in Table II take precedence over the instructions in the approved methods. We endorse the language 

that will allow a party to submit documentation to a permitting authority to support the use of an 

alternative to Table II requirements. However, in our experience permitting authorities are very reluctant 

to approve any deviations from Table II. Moreover, if a change is being proposed to improve the ability to 

preserve the integrity of a sample, it may be difficult or impossible to demonstrate that the modified 

procedure is better than a faulty approved procedure. 

Comment 101.1 

NYSDEC 

New York State Department of Environmental Conservation 

NYSDEC opposes EPA’s revision to the introductory text to Table II at 136.3(e). The proposed language 

allows permittees to solicit their regulating authority for permission to use alternate containers, 

preservation, and holding times to those found in Table II. The proposed language also charges the 

permitting authority to determine the nature, timing and extent of supporting documentation needed to 

grant permission. The inclusion of this language will impose an unnecessary and costly burden on 

permitting agencies in maintaining proper sampling conducted in compliance with the NPDES/SPDES 

programs. 

Specific reasons to omit the proposed language include: 

The proposed language places all the burden of establishing review criteria and maintaining a program for 

allowing alternative procedures for required containers, preservation and holding times on the permitting 

authority. NYSDEC has neither the staff nor fiscal resources to accept this additional responsibility. 

The proposed language will open Table II up for challenges to its credibility. We are often challenged by 

permittees to “show” where it is required that they follow specific procedures. Having a definitive Table 

II included in 40 CFR 136 allows challenges to be quickly and effectively resolved. 

Without a standard set of criteria by which to allow alternatives, the proposed changes will lead to 

inconsistencies in collecting samples, which subsequently affect monitoring data. Consistency in 

sampling protocols is a critical component to maintaining comparability of data for Clean Water Act 

programs. 

Decentralizing the authority to grant alternatives to established procedures will eliminate a central 

repository of analytical information. By having each permitting authority receive and determine what 

alternatives are allowable any progress towards developing new allowable techniques will be hindered. 

Maintaining one standard process for the approval of alternate procedures, whether it is holding times or 

method analysis provides simplicity and consistency. Introducing a separate pathway for seeking 

permission to use an alternative technique will be confusing and burdensome to both the regulated 

community and the regulating agency. 

NYSDEC recommends that the introductory language clarifies how to resolve conflicts between 

instructions in an approved method and what is published in 40 CFR 136 by simply stating that 

“Information in this table takes precedence over instructions provided in specific methods or elsewhere.” 

If EPA believes that it is necessary to provide the opportunity for a regulated party to seek an alternative 

to the specifics in Table II then it should follow the same guidance as declared in 40 CFR 136.4 and 136.5 

application and approval for alternative test procedures. 

Comment 107.1 

Patsy Root 
2010 Methods Update Rule Response to Comments 88 March 2012 

IDEXX Laboratories 

Page 58034: Since EPA is proposing revisions to Table II at 136.3(e) in order to resolve conflicts between 

instructions in the Table versus instructions in the method source(s) (example given includes 48 and 24 hr 

hold time for BOD), EPA should confirm which source takes precedence. 

Comment 108.1 

George Noguchi 

U.S. Department of the Interior, U.S. Fish and Wildlife Service 

The Department agrees with revising of the text to allow a party to submit documentation to their 

permitting or other authority that supports use of an alternative approach; so long as the alternative 

approach does not alter the integrity of the submitted sample. 

Comment 109.1 

Andre Brousseau 

Maine Wastewater Control Association 

EPA is proposing revisions to 40 CFR 136.3 (e) to clarify how to resolve conflicts. In the discussion on 

page 58034, EPA notes that the Table II instructions specify a 48 hour holding time for BOD samples, 

while some Part 136 methods recommend 24 hours. EPA indicates that the 40 CFR 136 Table II. 48-

hours holding time takes precedence over holding times recommended in the approved methods. Later in 

the discussion, EPA proposes to revise introductory text to Table II as follows: "Information in this table 

takes precedence over instructions provided in specific methods or elsewhere unless a party documents 

the acceptability of an alternative to the Table II instructions. The nature, timing and extent of the 

required documentation (i.e., how to apply and review as well the amount of supporting data) are left to 

the discretion of the permitting authority (State Agency or EPA Region)." 

The EPA seems to be saying its Table II holding time for BOD takes precedence, unless other authorities 

say otherwise. How will this be reviewed and enforced? How will it benefit effective enforcement of the 

Clean Water Act? 

The Maine DEP, by a Guidance Document sent to permittees by individual letter, considers a BOD result 

as valid only if the sample is analyzed within 6 hours of collection by an onsite laboratory, or within 24 

hours of collection by an off-site laboratory, unless the Maine DEP has granted a variance. In effect, this 

sets multiple holding times in conflict with Table II. The Maine DEP would be the State Agency 

responsible for clarifying conflicts with Table II. If the proposed rule change to 40 CFR 136. (e) becomes 

final, will the Maine DEP Guidance Document be sufficient documentation for requiring alternative 

holding times and variances for BOD? 

If not, would the EPA proposal require Maine DEP to document its policy for the various BOD holding 

times (6 hours, 24 hours or variance to individual permittees) in order to be in compliance with 40 CFR 

136? Will individual POTWs with pretreatment programs be required to refer significant industrial users' 

laboratories to the Maine DEP Guidance Document and instruct them to obtain any necessary variances 

from Maine DEP? 

Comment 112.1 

Colin Elliott 

King County Environmental Lab 

Conflicts between Table II and the Reference Method 
2010 Methods Update Rule Response to Comments 89 March 2012 

Comment: We agree that Table II should have precedence over the reference method. Allowing 

alternatives and providing flexibility on the level of documentation will be helpful. The current version 

specifies using the Alternate Test Procedure to document alternatives. This format doesn’t always work 

well for document holding time or storage condition validations. 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

Section II.F.1 discusses proposed changes in language in 136.3 about the preservation and holding time 

table. EPA is proposing to add the language "Information in this table takes precedence over instructions 

provided in specific methods or elsewhere unless a party documents the acceptability of an alternative to 

the Table II instructions. The nature, timing, and extent of the required documentation (i.e. how to apply 

and review as well as the amount of supporting data) are left to the discretion on the permitting authority 

(State Agency or EPA Region) or other authority and may rely on instructions, such as those provided for 

method modifications at 136.6. Thus an alternate sample container, preservation, and/or holding time may 

be considered at the discretion of the permitting authority or other authority." 

This office disagrees with this change. This provides an opening for inconsistencies across state agencies 

and poses a problem for laboratories to adhere to state requirements when analyzing samples for multiple 

states. It also leaves a lot of room for interpretation as to what containers, preservations, and holding 

times are acceptable. In some cases, it may put the decisions in the hands of regulatory authorities that do 

not have the experience to make the decision, e.g. the permitting group may be different than the 

laboratory certification group. If EPA is going to allow the preservation and holding times to be at the 

discretion of the permitting authority, what would be the point of having a table of criteria? If EPA wishes 

to allow this, then EPA must specify the guidelines and procedures for states to approve any changes. 

Specifically, guidelines for the minimum criteria needed to make this decision, e.g. changes to 

preservations and holding times must come from a published and reliable source. This change would 

work against the National Environmental Laboratory Accreditation Program in their pursuit to reduce the 

inconsistencies between states and EPA program certification requirements for laboratories. 

Another inconsistency across EPA programs is the preservation of Vinyl Chloride, Styrene, and 2-

Chloroethylvinyl ether. SW-846 specifies that if samples are to be analyzed for these compounds, the 

samples must be collected unpreserved and analyzed within seven days. The preservation table should be 

updated to be consistent with SW-846 preservation requirements. 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

We support the development of a single set of protocols regarding required sample containers, chemical 

and thermal sample preservation, and analytical holding times. To that end, it would seem that one 

approach to consider would be that the EPA only approve those methods which direct users to the Table 

II in 40CFR Part 136.3 for sample handling and preservation information. It is confusing for any analyst 

to try to resolve discrepancies between method and federal rules. 

 

While this provision in the proposed rule injects flexibility into the sample handling process, it also 

facilitates the erosion of consistency, conformity, and the quality of data being generated. Consequently 

we cannot support this aspect of the rule proposal. 
2010 Methods Update Rule Response to Comments 90 March 2012 

While it is quite possible to envision scenarios developing in which deviations from recognized sample 

handling protocols can or do occur, decisions regarding the use of the associated data are best left to the 

end users of the data. The proposed rule creates a system in which regulatory authorities make different 

decisions regarding sample handling protocols separately and distinctly from one another. Arguably, this 

has the potential to affect the consistency and quality of Clean Water Act data generated by individual 

states. 

Many would argue that data quality and sample integrity begin with the collection and preservation of the 

sample itself. Regulatory bodies do not—and should not—have the authority to allow the use of alternate 

analytical methodologies. Subsequently, we would propose that any suggested modifications to sample 

handling and preservation requirements be handled in the same manner as modifications to the analytical 

procedures, i.e., the ATP process. Rather than having individual regulatory authorities make decisions 

regarding modification to sample preservation or holding times, they should be submitted to a national 

authority. 

II.F.2 E. coli and Enterococcus Holding Times 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica, Inc. 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 100 - Carol Bell, City of Winston-Salem, North Carolina 

Comment 101.1 - New York State Department of Environmental Conservation 

Comment 106.1 - Charles Boepple, Upper Occoquan Service Authority 

Comment 107.1 - Patsy Root, IDEXX Laboratories 

Comment 110.1 - Laurie Curra, Texas Commission on Environmental Quality 

Comment 112.1 - Colin Elliott, King County Environmental Lab 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 116.1 - Wendy Harding and Mala Burton, Joint Virginia Water Environment Association and 

Virginia American Water Works Association 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 120.1 - David N. Speis, Environmental Laboratory Advisory Board (ELAB) 

Comment 124.1 - Thomas Tourje, Augusta County Service Authority 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Comment 171.1 - Lola Guerra, Henrico County DPU 

Summary of Comments: The majority of the commenters supported the changes and clarifications to 

the holding times for E. coli and Enterococcus. Two commenters were also concerned with a potential 

inconsistency between footnotes 4 and 22 to Table II. One commenter did not support that change, 

claiming it was too restrictive and difficult to meet in cases where laboratories are not nearby the facility 

collecting the sample. 

Response: EPA appreciates the comments in support of the changes and clarifications. Regarding the 

potential inconsistency between footnotes 4 and 22, EPA is deleting the text that reads “(e.g., samples 

analyzed for fecal coliforms may be held up to 6 hours prior to commencing analysis)” from Footnote 4 

so that the footnotes are consistent. 

As stated in the proposal preamble, in 2006, EPA conducted a nationwide holding time study for fresh 

and marine ambient waters (see proposal docket item EPA-HQ-OW-2010-0192-0035) and concluded 
2010 Methods Update Rule Response to Comments 91 March 2012 

that, on a nationwide basis, the Agency was unable to justify extending the holding time for Escherichia 

coli or Enterococcus in these water matrices. The alternate test procedure program (40 CFR part 136.4) 

allows permittees to apply to the Regional Coordinator or permitting authority in the Region where the 

discharge occurs for approval of an alternate test procedure (in this case, the extension of the holding 

time) if, among other requirements, they are able to provide comparability data for the performance of the 

proposed alternate test procedure compared to the performance of the approved test procedures. See 

response in section II.A.3.e for more details on the ATP program. 

Original Comment Text: 

The following commenters supported the revised Footnote for holding time. 

Comment 79.1 Richard Burrows, TestAmerica, Inc. 

Comment 91.1 Andrea Rex, Massachusetts Water Resources Authority 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 101.1 New York State Department of Environmental Conservation 

Comment 106.1 Charles Boepple, Upper Occoquan Service Authority 

Comment 110.1 Laurie Curra, Texas Commission on Environmental Quality 

Comment 112.1 Colin Elliott, King County Environmental Lab 

Comment 116.1 Wendy Harding and Mala Burton, Joint Virginia Water Environment Association 

and Virginia American Water Works Association 

Comment 120.1 David N. Speis, Environmental Laboratory Advisory Board (ELAB) 

Comment 124.1 Thomas Tourje, Augusta County Service Authority 

Comment 132.1 Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 169.1 Judith R. Morgan, American Council of Independent Laboratories 

Comment 171.1 Lola Guerra, Henrico County DPU 

Other comments: 

Comment 100 

Carol Bell 

City of Winston-Salem, North Carolina 

Table 1I, Footnote 4, Page 58067 states that as an example, samples analyzed for fecal coliforms may be 

held up to 6 hours prior to commencing analysis - this probably should read 8 hours now due to the new 

allowance of up to 8 hours holding time. However if 6 hours is correct here, then more explanation is 

needed for the 8 hour time to incubation??? 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

Table II, footnote 4, gives an example of the hold time for fecal coliforms as 6 hours. This does not agree 

with the proposed hold time of 8 hours found in footnote 22 of Table II. 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

Section II.F.2. EPA is proposing to revise the footnote to read ‘‘Sample analysis should begin as soon as 

possible after receipt; sample incubation must be started no later than 8 hours from time of collection.” 

We believe this is too restrictive. We find that this places undue constraints on a facility as there may not 

be a laboratory close enough to meet these requirements. 
2010 Methods Update Rule Response to Comments 92 March 2012 

None of the standard shippers (UPS, USPS, etc.) can meet these delivery requirements— particularly in 

remote areas of a number of states. Is this data worth the additional cost in terms of travel and personnel 

time required to transport the samples? Frequently, labs are 200 miles or more from the facility in 

question. Any type of weather or travel delay can cause an exceedance, not to mention the cost of a round 

trip. If samples are properly cooled, microbial activity should be sufficiently reduced, suggesting that 

there is not a significant difference between samples received within 8 hours and those received via 

overnight shipping. 

How are regulatory agencies expected to enforce this? Do individual states have the authority to accept 

the data from samples not meeting the hold time requirement with qualification or must samples be 

rejected? Arguably, samples collected for beach monitoring activities are equally—if not more—critical 

to human health, yet there is no equivalent holding time regulation imposed on these samples. These 

samples are routinely shipped to labs via overnight carrier. We feel that the risk is low if the permitted 

facilities are properly monitoring their disinfection processes. Many state regulatory programs, including 

Wisconsin, do not require or even offer accreditation for bacterial testing of effluents, and therefore 

details such as sample holding time are not being evaluated. Finally, if this proposed rule becomes final, 

there are provisions within the rule that would allow parties to create/approve alternate holding times with 

very little documentation, since the criteria and extent of documentation for a change are left up to the 

regulatory authority. 

II.F.3 Revising cyanide sample handling instructions in Footnote 5 to Table II 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 112.1 - Colin Elliott, King County Environmental Lab 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 153.1 - Debbie Webster, Central Valley Clean Water Association 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 169.1- Judith R. Morgan, American Council of Independent Laboratories 

Comment 177.1 - Novelle C. Stokes, South Central Wastewater Authority 

Summary of Comments: EPA proposed to revise the cyanide sample handling instructions in Footnote 

5 of Table II to recommend the treatment options for samples containing oxidants described in ASTM’s 

sample handling practice for cyanide samples, D7365–09a. Many commenters supported the change to 

the cyanide preservation requirements and instructions. Other commenters were supportive, but noted 

potential inconsistencies that they recommended EPA address. Still other commenters expressed some 

confusion regarding whether D7365-09a was a requirement or listed as another source of information 

rather than a requirement. Those commenters were concerned that making D7365-09a a requirement 

meant that they will be required to purchase a copy of this standard from ASTM, and thus incur costs. 

Response: EPA thanks the commenters for their support and recognizes that a potential inconsistency 

existed between the proposed language for Table II and ASTM D7365–09a. Therefore, EPA is revising 

the language in Table II to be consistent with the ASTM standard practice by adding the following 

language to footnote 5: " ASTM D7365–09a specifies treatment options for samples containing oxidants 

(e.g., chlorine)...." 

The citation of ASTM D7365-09a was intended to be a replacement for the version of Footnote 5 in the 

currently promulgated Table II. Therefore, the information in the ASTM standard is considered to be a 

requirement of Table II, as well as providing additional information that may not be specified in the 
2010 Methods Update Rule Response to Comments 93 March 2012 

analytical test methods. EPA recognizes that some laboratories may have to purchase a copy of the 

ASTM standard at some nominal cost, but given historical concerns about preservation of samples for 

cyanide analysis, EPA finds the purchase of this standard to be the most appropriate approach to resolving 

those concerns.

Original Comment Text: 

The following commenters supported the revised cyanide sample handling revisions to footnote 5. 

Comment 79.1 Richard Burrows, TestAmerica Inc. 

Comment 169.1 Judith R. Morgan, American Council of Independent Laboratories 

The following commenters had the same (following) comment regarding the inconsistency between 

footnote 5 in Table II and the ASTM method for cyanide sample preservation 

Comment 132.1 Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 169.1 Judith R. Morgan, American Council of Independent Laboratories 

Comment 177.1 Novelle C. Stokes, South Central Wastewater Authority 

Comment: The change to the ASTM method is supported, however, the preservation instructions in the 

Table II are different from the instructions in ASTM method D7365-09a. The introductory text to Table II 

at 136.3 (e) specifies that the instructions in Table II take precedence over other sources of information. 

Table II also contains footnote 6 which refers to ASTM D7365-09a. Thus, the requirement for 

preservation is unclear. It is unclear if ASTM D 7365-09a is considered another source of information or 

if it is a requirement of Table II as indicated by footnote 6. If it is considered another source, then cyanide 

samples must be preserved to pH > 12. On the other hand, according to ASTM D 7365-09a, adjusting pH 

to >12 may introduce potential problems as follows: 

• Adding sodium hydroxide to pH 12 in samples containing formaldehyde, an ozone disinfection 

byproduct, can result in cyanide formation during sample storage. 

• If the sample contains carbonate, low cyanide recovery will result due to the release of cyanide with 

carbon dioxide upon acidification prior to distillation. By adjusting pH to 10 per ASTM, there is a 

provision to add calcium hydroxide to pH 12 -12.5 to remove carbonate and address this issue. 

Recommendation: Resolve the inconsistency in Table II for cyanide sample preservation by requiring the 

ASTM procedure for sample preservation. 

Other comments: 

Comment 91.1 

Andrea Rex 

Massachusetts Water Resources Authority 

We endorse the two changes proposed for cyanide sample preservation, basing the requirements on 

ASTM D7365-09a. It gives permittees and laboratories the opportunity to attempt to preserve and test 

cyanide samples in a customized way to yield accurate results. Cyanide preservation and treatment for 

interferences is exceedingly problematic. We demonstrated that even in treated drinking water samples, 

cyanide could be formed in the sample container due to the preservation (Michael F. Delaney, Charles 

Blodget, Corinna E. Hoey, Nancy E. McSweeney, Polina A. Epelman, and Steven F. Rhode, “False 

Cyanide Formation During Drinking Water Sample Preservation and Storage”, Environmental Science 

and Technology, 2007, 41(24), 8383–8387). The proposed revision shifts the authority to properly collect 

and preserve the samples onto the sampler/analyst, who may have difficulty sorting through the 

bewildering array of options and have no way to demonstrate that their choices were correct. Ultimately 
2010 Methods Update Rule Response to Comments 94 March 2012 

EPA may need to require the use of field spikes so that proper preservation can be demonstrated—this 

would be very complicated. 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 

Comment: We welcome the additional recommendations for cyanide preservation and handling, which 

are in line with the current state of the art for this important and difficult analyte. 

Comment 112.1 

Colin Elliott 

King County Environmental Lab 

Comment: We agree that the procedures defined in ASTM method D7365-09a are acceptable 

requirements for sample handling. However, having requirements that are available only from a single 

source that charges a fee for access does not seem appropriate. We believe the public should have direct 

access to the requirements without paying an access fee or setting up a subscription. 

Comment 153.1 

Debbie Webster 

Central Valley Clean Water Association 

On behalf of the member agencies of the Central Valley Clean Water Association (CVCWA), we would 

like to share our support for proposed amendments related to cyanide test procedures. As explained in 

greater detail below, we specifically endorse proposed amendments to include: the addition of ASTM 

Standard Practice D7365-09a as a footnote in Table II 

In California, the Policy for Implementation of Toxics Standards for Inland Surface Waters, Enclosed 

Bays, and Estuaries of California (SIP) establishes procedures for the development of effluent limitations 

for pollutants such as cyanide. In the arid Central Valley of California, many POTWs discharge effluent 

to seasonal streams that often provide little to no dilution for prolonged periods of time. Through the SIP 

procedure, these POTWs discharging to effluent dominated water bodies often receive average monthly 

effluent limits for cyanide as low as 4.1 μg/L. Consistent compliance with this limitation is problematic, 

and numerous Central Valley POTWs employing secondary and tertiary treatment systems with chlorine 

or UV disinfection technologies have been affected. These POTWs almost universally utilize acid 

distillation procedures with amperometric or spectrophotometric detection to measure total cyanide (i.e., 

EPA methods 335.2, 335.4, and 9010B, Standard Method 4500-CN) as a NPDES permit required means 

of measuring compliance. As U.S. EPA is aware, total cyanide measurements derived from such acid 

distillation based methods are prone to interference and bias, particularly in complex matrices such as 

POTW effluent. 

The attached document Problems Associated with Using Current EPA Approved Total Cyanide 

Analytical Methods for Determining Municipal Wastewater Treatment Plant NPDES Permit Compliance, 

prepared on behalf of CVCWA member agencies by local experts familiar with POTW cyanide 

compliance issues, was presented to the Central Valley Regional Water Quality Control Board on May 

26, 2010. In this document, evidence independently generated by several POTWs strongly suggests that 

the use of sodium hydroxide as a preservative can lead to positive bias in total cyanide measurements. 

For POTWs that have not been granted dilution credit, small errors in cyanide measurement can lead to 

effluent limit violations and water quality objective exceedances. Sodium hydroxide-related bias is 

recognized by experts in cyanide analytical chemistry, and as U.S. EPA is aware through its proposed 

inclusion of ASTM D7365-09a, it is recommended as an appropriate mitigation of this interference to 
2010 Methods Update Rule Response to Comments 95 March 2012 

omit preservation with sodium hydroxide, provided cyanide’s stability can be demonstrated through a 

properly conducted hold-time study. 

Allowing for the omission of sodium hydroxide in cyanide stable matrices currently is not codified in the 

40 CFR 136. Formal reference to ASTM D7365-09a in the footnotes to Table II would significantly 

improve upon the preservation and stabilization of cyanide samples. But inclusion of the ASTM standard 

practice may not be the ultimate solution necessary to fully address the cyanide compliance and cyanide 

interference issues facing our many member agencies. 

For this reason we fully support the proposal to include “free” cyanide analytical methods in the battery 

of approved methods for NPDES compliance monitoring as well the language modifications to the Table 

II introduction that gives the local permitting authority the discretion to approve the use of alternative 

cyanide sample handling and preservation procedures. As presently stated in the footnotes to Table II, 

“There may be interferences that are not mitigated by approved procedures,” including the latest 

procedures detailed in ASTM D7365-09a. For this reason, we strongly support the regulatory flexibility 

afforded by dealing with the local permitting authority in developing analytical fixes where interference 

and bias is involved. Furthermore, the possibility of utilizing an analytical method that measures the 

portion of cyanide that is truly bioavailable is needed and, therefore, we support inclusion of the proposed 

“free” cyanide procedures. 

Although our CVCWA membership is limited to the Central Valley of California, we are aware that our 

issues with total cyanide analysis and cyanide compliance are not unique. Studies documenting the 

problems associated with total cyanide analysis on a national scale are published in the scientific 

literature, as well in professional and trade publications. We applaud U.S. EPA’s efforts to address these 

cyanide issues, and support the cyanide-related changes in the proposed rule. 

(EPA did not include attachment 153.2) 

II.F.4 Revising Cyanide Sample Handling Instructions in Footnote 6 to Table II 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Laboratory Certification 

Comment 116.1 - Wendy Harding and Mala Burton, Joint Virginia Water Environment Association and 

Virginia American Water Works Association 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 166.1 - Paul Wiegand, National Council for Air and Stream Improvement, Inc. 

Comment 169. 1- Judith R. Morgan, American Council of Independent Laboratories 

Summary of Comments: EPA proposed to revise the cyanide sample handling instructions in Footnote 

6 of Table II to recommend the treatment options for samples containing oxidants described in ASTM’s 

sample handling practice for cyanide samples, D7365–09a. Many commenters supported the change to 

the cyanide preservation requirements and instructions. Other commenters were supportive, but noted 

potential inconsistencies that they recommend EPA address. Still other commenters expressed some 

confusion regarding whether D7365-09a was a requirement or listed as another source of information 

rather than a requirement. Those commenters were concerned that making D7365-09a a requirement 

meant that they will be required to purchase a copy of this standard from ASTM, and thus incur costs. 
2010 Methods Update Rule Response to Comments 96 March 2012 

Response: EPA thanks the commenters for their support and recognizes that a potential inconsistency 

existed between the proposed language for Table II and ASTM D7365–09a. Therefore, EPA is revising 

the language in Table II to be consistent with the ASTM standard practice by adding the following 

language to footnote 6: "Sampling, preservation and mitigating interferences in water samples for analysis 

of cyanide are described in ASTM D7365–09a. There may be interferences that are not mitigated by the 

analytical test methods or D7365–09a. Any technique for removal or suppression of interference may be 

employed, provided the laboratory demonstrates that it more accurately measures cyanide through quality 

control measures described in the analytical test method. Any removal or suppression technique not 

described in D7365–09a or the analytical test method must be documented along with supporting data." 

The citation of ASTM D7365-09a was intended to be a replacement for the very lengthy version of 

Footnote 6 in the currently promulgated Table II. Therefore, the information in the ASTM standard is 

considered to be a requirement of Table II, as well as providing additional information that may not be 

specified in the analytical test methods. EPA recognizes that some laboratories may have to purchase a 

copy of the ASTM standard at some nominal cost, but given historical concerns about preservation of 

samples for cyanide analysis, EPA finds the purchase of this standard to be the most appropriate approach 

to resolving those concerns.

Original Comment Text: 

The following commenters supported the revised cyanide sample handling revisions to footnote 6. 

Comment 79.1 Richard Burrows, TestAmerica Inc. 

Comment 91.1 Andrea Rex, Massachusetts Water Resources Authority 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

The following commenters had the same (following) comment regarding the inconsistency between 

footnote 6 in Table II and the ASTM method for cyanide sample preservation 

Comment 116.1 Wendy Harding and Mala Burton, Joint Virginia Water Environment Association 

and Virginia American Water Works Association 

Comment 132.1 Paula Hogg, Hampton Roads Sanitation District 

Comment 164.1 Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 177.1 Lola Guerra, Henrico County DPU 

Comment: The preservation instruction in Table II is different from the instruction in the method ASTM 

D 7365-09a. 

The introductory text to Table II at 136.3 (e) specifies that the instructions in Table II takes precedence 

over other sources of this information. Table II also contains footnote 6 which refers to ASTM D7365-

09a. Thus, the requirement for preservation is unclear. It is unclear if ASTM D 7365-09a is considered 

another source of information or if it is a requirement of Table II as indicated by footnote 6. If it is 

considered another source, then cyanide samples must be preserved to pH >12. On the other hand, 

according to ASTM D 7365-09a, adjusting pH to >12 may introduce potential problems as follows: 

1. Adding sodium hydroxide to pH 12 in sample containing formaldehyde, an ozone disinfection 

byproduct, can result in cyanide formation during sample storage. 

2. If the sample contains carbonate, low cyanide recovery will result due to the release of cyanide with 

carbon dioxide upon acidification prior to distillation. By adjusting pH to 10 per ASTM, there is 

provision to add calcium hydroxide to pH 12 - 12.5 to remove carbonate and address this issue. 

Recommendation: The inconsistency in Table II for preservation of cyanide samples should be addressed 

in the final rule by requiring the ASTM procedure for sample preservation. 
2010 Methods Update Rule Response to Comments 97 March 2012 

Other comments: 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Laboratory Certification 

Table II Footnotes 5 and 6 reference ASTM methodology and is the only reference for these techniques. 

ASTM methods cost money to purchase. EPA needs to establish these criteria in their own document or 

publish the criteria in the footnote or somewhere else in the Federal Register. This methodology should be 

made readily available for states and laboratories and should not have to be purchased. 

Comment 169. 1 

Judith R. Morgan 

American Council of Independent Laboratories 

Section: II. Summary of Proposed Rule, Section F.3 and F.4 (pg 58034) Topic: Cyanide sample handling 

and preservation Comment: We welcome the additional recommendations for cyanide preservation and 

handling, which are in line with the current state of the art for this important and difficult analyte. 

II.F.5 Revise Footnote for Handling WET samples 

List of Comments: 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 107.1 - Patsy Root, IDEXX Laboratories 

Comment 109.1 - Andre Brousseau, Main Wastewater Control Association 

Comment 112.1 - Colin Elliott, King County Environmental Lab 

Summary of Comments: Commenters supported the changes to the sampling handling requirements for 

WET samples. 

Response: EPA thanks the commenters for their support. 

Original Comment Text: 

The following commenters supported the footnote for handling WET samples. 

Comment 91.1 Andrea Rex, Massachusetts Water Resources Authority 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 107.1 Patsy Root, IDEXX Laboratories 

Comment 109.1 Andre Brousseau, Main Wastewater Control Association 

Comment 112.1 Colin Elliott, King County Environmental Lab 

II.F.6 Clarify the Holding Time for WET samples 

List of Comments: 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 112.1 - Colin Elliott, King County Environmental Lab 

Summary of Comments: Commenters supported the clarification of the holding time requirements for 

WET samples. 

Response: EPA thanks the commenters for their support. 
2010 Methods Update Rule Response to Comments 98 March 2012 

Original Comment Text: 

The following commenters supported the clarification of holding time for WET samples. 

Comment 91.1 Andrea Rex, Massachusetts Water Resources Authority 

Comment 112.1 Colin Elliott, King County Environmental Lab 

Section II.G Proposed Revisions to 40 CFR 136.4 and 136.5 

List of Comments: 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 108.1 - George Noguchi, U.S. Department of the Interior, U.S. Fish and Wildlife Service 

Comment 112.1 - Colin Elliott, King County Environmental Lab 

Comment 122.1 - Jason Fagel, New York State Department of Environmental Conservation, Division of 

Water 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 160.1 - Robert Steidel, Virginia Association of Municipal Wastewater Agencies, Inc. 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Summary of Comments: The majority of the commenters supported EPA’s proposal to modify the ATP 

procedures applicable to nationwide applications, as well as to clarify the intent of limited use ATPs. 

However, one commenter expressed concern that the process for limited-use ATPs does not require that 

the ATP be supported by comparative data, and the commenter suggests language that could be used to 

obtain comparative data even for limited use ATPs. Several other commenters expressed concerns that 

some state programs may be taking an abbreviated approach to review of ATPs by simply specifying a 

non-approved method in a discharge permit. These commenters expressed concerns about the quality of 

any discharge data subsequently collected in such situations. 

Response: EPA appreciates comments submitted in support of the proposed changes. The Agency 

agrees that an essential component of requiring comparability data was inadvertently omitted from the 

proposed language for limited use ATP applications at part 136.5 and has corrected this by adding the text 

suggested by the commenter from NYSDEC as follows "(5) Provide comparability data for the 

performance of the proposed alternative test procedure compared to the performance of the reference 

method." Data demonstrating method comparability needs to be submitted as part of applications for 

limited-use approval of alternate test procedures. Guidance on data requirements is provided in the ATP 

and New Method Protocols, which are designed to allow for a three-tiered system of validation. Those 

requirements vary based on the intended use of a method: in a single laboratory on one or more matrix 

types; in all laboratories on one matrix type; or in all laboratories on all matrix types. 

EPA does not entirely understand the focus of the nearly identical comments from three commenters in 

Virginia regarding part 136.5 and limited use ATPs. EPA agrees that NPDES compliance monitoring 

data should be generated by methods approved at part 136 or by ATPs that have been approved for either 

nationwide use or limited use (e.g., a particular industry or facility). EPA acknowledges that states and 

other permitting authorities sometimes specify the use of a particular method in an individual permit. 

However, in instances where no method is approved for an analyte at part 136, the permitting authority 

has the authority to require both monitoring for that parameter and to require the use of a method it deems 

appropriate. 

EPA notes that the permitting process is not strictly unilateral, flowing down from the permitting 

authority to the permittee in a final form. Rather, in practice, there are often procedures in place for 

submitting data and comments regarding the specific permit requirements, particularly in instances where 

monitoring of a parameter without a part 136 method is involved. The commenters’ concerns about how 

and why the permitting authority selected and specified a method not in part 136 can be addressed during 

the permitting process. While EPA agrees that a process like that used to approve ATPs could be used by 
2010 Methods Update Rule Response to Comments 99 March 2012 

permitting authorities, EPA does not require that such a process be employed in instances where a new 

parameter without a part 136 method is specified in a given permit. 

Original Comment Text: 

The followed commenter supported the limited use ATP procedure reviews. 

Comment 91.1 Andrea Rex, Massachusetts Water Resources Authority 

The following commenters had the same (following) comment regarding the ATP approval process via 

part 136.5. 

Comment 132.1 Paula Hogg, Hampton Roads Sanitation District 

Comment 160.1 Robert Steidel, Virginia Association of Municipal Wastewater Agencies, Inc. 

Comment 164.1 Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Section 136.5 addresses the approval of alternate test procedures, those not identified and approved in 

Part 136, for limited use. In our view the intent of section 136.5 (both the current wording and the 

wording as EPA proposes to modify it) is that all data required pursuant to NPDES permits and otherwise 

under the NPDES program, if not developed pursuant to approved methods, must be by analytical 

methods that have been approved for specific or limited uses through the relatively informal alternate test 

procedures approval mechanisms that EPA has established. 

However, there are instances where state NPDES agencies have attempted to apply a less rigorous 

standard, and have taken the position that the simple incorporation of a specific method requirement in an 

issued NPDES permit is adequate to authorize the use of a non-Part 136 method. The quality of the data 

that go into the development of NPDES permits, and the quality of the data generated through permit 

requirements, is of course at the heart of the NPDES program. Therefore, any procedure that avoids the 

substantial review of applicability of any proposes alternate test methods and of the quality of the data 

generated is in our view contrary to the requirements of the regulation and contrary to the best interests of 

the program. 

We recommend that EPA enforce the clear intent of the regulation, and in its preamble and any other 

documents that accompany the final Guidelines amendment, emphasize that alternate test procedures are 

only approved through the procedures established pursuant to section 136.5 and NPDES permit issuance 

cannot substitute for such approval. 

Other comments: 

Comment 108.1 

George Noguchi 

U.S. Department of the Interior, U.S. Fish and Wildlife Service 

The Service agrees with the change to establish the procedures for obtaining approval for nationwide use 

of an alternative test procedure in a state within a particular EPA region whereas it is inclusive only of 

those methods for which EPA has published and alternate test procedure protocol. Not exactly sure what 

this is referring to. I am guessing that it may be referring to either method defined analytes or perhaps to 

test for Whole Effluent Toxicity (WET)? However, EPA is pleased that the Service agrees with the 

change. 

Comment 112.1 

Colin Elliott 

King County Environmental Lab 

The updated procedure in 40 CFR 136.5 includes only general requirements for the application rather than 

following a specific protocol. Using the documentation protocol defined for nation-wide Alternate Test 
2010 Methods Update Rule Response to Comments 100 March 2012 

Procedures was too restrictive for small changes that are limited to a single laboratory. The ATP and 

New Method protocols are applicable to major modifications that require validation through laboratory 

studies. The protocols are designed to allow for a three tiered system of validation requirements based on 

the intended use of a method (in a single laboratory on one or more matrix types, in all laboratories on 

one matrix type or in all laboratories on all matrix types). Minor or “small” changes generally fall within 

the flexibility provided at part 136.6. 

Comment 122.1 

Jason Fagel 

New York State Department of Environmental Conservation, Division of Water 

Additions - NYSDEC is in agreement with the majority of the changes proposed for § 136.5 

“Approval of alternate test procedures for limited use.” However, there is one item noticeably absent and 

if included would improve the protocol for limited use alternate test procedures (ATP) and maintain 

consistency with § 136.4 “Application for and approval of alternate test procedures for nationwide use.” 

The proposed language currently does not require comparability data be submitted when seeking a 

Regional limited use ATP approval. If the requestor has not made an application for nationwide use then 

there is no requirement to provide comparability data. NYSDEC believes this is an essential component 

in determining ATP approval. Regardless of whether it is for nationwide or limited regional use. 

Therefore, NYSDEC requests that the following language be included under § 136.5 “Approval of 

alternate test procedures for limited use.” 

“(5) Provide comparability data for the performance of the proposed alternative test procedure compared 

to the performance of the reference method for limited use ATPs where nationwide approval has not been 

requested.” 

Section II.H Revisions to Method Modification Provisions at 40 CFR 136.6 

EPA proposed to make revisions to the existing provisions for method modifications that are codified at 

40 CFR 136.6. Part of that proposal was to provide examples of some allowable modifications to 

methods or performance evaluation procedures that would not require prior approval from EPA. The 

proposal generated a large number of comments across a wide range of topics. Although this section of 

the original proposal did not include any subsections or other logical structural divisions, EPA has 

divided the comments received by topics, and presents the comment responses for each topic in 

subsections H.1 to H.11, below. 

II.H.1 General Comments 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 107.1 - Patsy Root, IDEXX Laboratories 

Comment 108.1 - George Noguchi, U.S. Department of the Interior, U.S. Fish and Wildlife Service 

Comment 111.1 - Edward F. Askew PhD, Askew Scientific Consulting 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Summary of Comments: A number of commenters offered general support for the allowed flexibility 

and many thanked EPA for providing specific examples. Several commenters expressed concerns about 

if and how state or local regulatory authorities would be notified by laboratories of such modifications. 
2010 Methods Update Rule Response to Comments 101 March 2012 

One commenter asked if EPA planned to provide guidance on the method modification requirements for 

permitting authorities. Another commenter advocated updating the affected methods rather than relying 

on the approach of describing the allowed flexibility in the regulation. One commenter expressed 

concerns about the effect of the allowed flexibility on enforcement actions, citing, but not providing, a 

memorandum from “IDNR.” 

Response: EPA thanks the commenters for their support. With regard to notification procedures, EPA 

has revised section 136.6(b)(1) to clarify that the user must notify their permitting authority of the intent 

to use a modified method. EPA does not require certification or accreditation for compliance monitoring 

under the CWA. However, if the user holds a certification or accreditation, EPA recommends that the 

permitting authority be notified of such certification or accreditation. 

With regard to guidance for permitting authorities, if permitting authorities need additional assistance 

understanding these requirements, they may wish to contact their EPA Regional Coordinator. 

With regard to the recommendation to update affected methods to reflect these allowed modifications, 

EPA notes that such an approach could only be used for methods published by EPA. In fact, as currently 

promulgated, the allowance for flexibility applies to all approved methods, including methods from EPA 

and from other organizations, such as VCSBs and ATPs from vendors. However, when EPA methods are 

updated in the future, EPA will strive to describe allowable modifications where practical. 

EPA was not able to fully respond to concerns from one commenter regarding enforcement concerns 

because it is not clear if “IDNR” refers to the Department of Natural Resources in Illinois, Indiana, or 

Iowa, and the commenter did not include the referenced memorandum with the comments. However, 

EPA notes that state and local regulatory authorities already have the authority to be more stringent than 

Federal regulations. Thus, if a given state does not wish to allow method modifications for which EPA 

does not require prior approval, EPA cannot force the state to allow those modifications. In such 

instances, it is incumbent upon the state to notify the affected dischargers and laboratories of such 

restrictions. 

Original Comment Text: 

The following commenters had the same (following) comment regarding clarification of "and/or", and the 

ability of permitting authority staff to understand requirements. 

Comment 79.1 Richard Burrows, TestAmerica Inc. 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment: The additional examples of allowed and prohibited method modifications are very useful and 

will allow laboratories to more confidently apply minor allowed modifications which can improve the 

quality of the analysis. 

Section: 136.6 (b)(1), Method Modifications and Analytical Requirements 

Comment: It states that “The user must notify their permitting authority and/or their certification 

authority/accreditation body of the intent to use a modified method....” Please clarify if it is an “and” or 

an “or.” Additionally. How does the USEPA foresee permitting authority staff being able to understand 

all the requirements for method modifications? Will additional guidance on this, for NPDES permit 

writers, be made available by the USEPA? 

Comment 107.1 

Patsy Root 

IDEXX Laboratories 
2010 Methods Update Rule Response to Comments 102 March 2012 

Generally the language used in the proposed rule is clear, easily understood and speaks to the desire of the 

EPA to have a high level of understanding among a wide audience. Commend EPA on adding clarity on 

method flexibility by presenting additional examples. 

Comment 108.1 

George Noguchi 

U.S. Department of the Interior, U.S. Fish and Wildlife Service 

We are in agreement that regulatory authorities should allow analysts the flexibility to modify CWA 

methods without prior approval provided the user has documented equivalent or better performance of the 

method in that particular matrix type. 

In instrumental analyses, analysts may need to modify approved methods in order to combat matrix 

interferences and these modifications should not require extensive review. 

The Department agrees that acceptable reasons for these modifications should include lower detection 

limits, improved precision, less spectral interference, lower laboratory cost and the reduction of laboratory 

waste. These modifications should not deviate from the underlying chemical principles. 

Comment 111.1 

Edward F. Askew PhD 

Askew Scientific Consulting 

The PMUR sections 136.6 (b)(3) and (b)(4) forbid the modifications allowed in PMUR section 136.3(e). 

These incongruities will make enforcement of violations of the CWA such as the IDNR memo difficult if 

not impossible. (Note from EPA – The referenced IDNR memo was not submitted with this comment.) 

Comment 112.1 

Colin Elliott 

King County Environmental Lab 

General Comment: The added information is helpful for clarifying issues that may not directly discussed 

in the reference method. We would encourage the EPA to also update the individual reference methods 

noted in this section rather than relying on this mechanism to make them more current. 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

The updated part 136.6 (b) (I) states that the user must inform their certification, permitting, or 

accreditation authority at the time of accreditation if a modified method is being used. This language does 

not require a laboratory to inform their regulators at other times a modified method is placed into use at 

the laboratory. This effectively enables a laboratory to use a modification that this unacceptable to 

regulators with no potential oversight until the next audit, inspection, or evaluation is performed. This 

could result in substantial amounts of data being deemed unacceptable due to this loss of oversight. 136.6 

(b) (I) should be updated to state that “The user must notify their permitting authority and/or their 

certification authority/accreditation body of the intent to use a modified method before implementation 

for regulatory compliance analysis.” 

Comment 169.1 

Judith R. Morgan 
2010 Methods Update Rule Response to Comments 103 March 2012 

American Council of Independent Laboratories 

Comment: The modifications to method 625 allowed are useful for optimizing the method for different 

matrices and are in line with techniques that have been in use for several years. 

II.H.2 Use of Relative Standard Error (RSE) to Evaluate Calibrations 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 83.1 - Anonymous Public Comment 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Summary of Comments: Four commenters supported the use of Relative Standard Error (RSE) to 

evaluate calibrations, and several of those commenters suggested minor changes to the presentation of the 

equation and the terms involved. One commenter expressed reservations about the use of RSE, noting it 

has been advocated by only a few parties, it may not be sufficiently rugged and allow calibrations to 

“pass” when they would not otherwise, and it adds an additional option with which data users and 

regulators must contend in examining compliance data. 

Response: EPA thanks those commenters who supported the allowance for using the RSE. EPA has 

modified the equation for calculation of the RSE (see 136.6(b)(4)(J)) in line with the comments, so that it 

is more consistent with other references. The revised equation is shown below: 

where: 

x'i = Calculated concentration at level i. 

xi = Actual concentration of the calibration level i. 

n = Number of calibration points. 

p = Number of terms in the fitting equation (average = 1, linear == 2, 

quadratic = 3). 

EPA recognizes that allowing the RSE to be used provides an additional approach for laboratories and 

data users to evaluate calibrations. However, EPA points out that the historical mix of calibration metrics 

(e.g., average RRF, regression coefficients, and “use the entire curve”) are not interchangeable in practice, 

nor do they share common acceptance criteria (e.g., there is no relationship between the relative standard 

deviation [RSD] for the RRF approach and a given correlation coefficient [r2

]). Thus, if the commenter 

were to examine GC/MS calibration data and calculate the correlation coefficient, there is no guarantee 

that a calibration that meets the RSD limit of the method will also meet the r2

 limit from another method. 

One advantage of the RSE is that the same acceptance limit for the RRF approach can be used for the 

RSE approach. And, as noted by one commenter, the RSE approach is more sensitive to deviations at the 
2010 Methods Update Rule Response to Comments 104 March 2012 

low end of the calibration range, and its use could improve some calibrations compared to current 

practices. 

Original Comment Text: 

Comment 79.1 

Richard Burrows 

TestAmerica Inc. 

Section 136.6 5.(J), RSE 

Comment: We are very pleased to see RSE included as an alternative calibration assessment model. The 

commonly used correlation coefficient is inadequate as a calibration assessment tool, because it allows 

very large relative errors at the low end of the curve. RSE will not allow curves with these large errors to 

pass calibration criteria. We believe that use of RSE will result in a substantial improvement in the quality 

and reliability of routine data, especially at levels near the lower end of the calibration curve. Several 

major instrument vendors are working towards adding RSE to their instrument software in anticipation of 

the finalization of this rule. 

For consistency with other documents, RSE should be expressed in a slightly different way, as follows: 

௜ݕൣ෍ඩܺ 100 ൌ ܧ%ܴܵ

ᇱ െ ݕ௜൧

௜ݕ

ᇱ

ଶ

൘ሺ݊െ݌ሻ

௡

௜ୀଵ

Where: 

y’i = Predicted (or calculated) response for the ith calibration standard 

yi = Actual response for the ith calibration standard 

n = the number of calibration points 

p = the number of terms in the fitting equation (average=1, linear=2, quadratic=3) 

Comment 83.1 

Anonymous Public Comment 

Unknown 

On xx/xx/xxxx we submitted comments on method 8000D that included a revised equation for RSE. 

Since then we have been actively researching RSE in preparation for a publication. As a result of this 

research we are proposing a different form of the equation, based on the relative errors in the amounts 

rather than the responses. 

In most cases these two forms of the equation are not much different. For example, both are exactly 

equivalent to the RSD for an average type curve. However, the RSE based on responses trends very high 

in the special case where one of the predicted responses is close to zero. The form based on amounts does 

not have this problem. 

The equation recommended is 

%ܴܵܧ ൌ 100 ܺඨ∑ ቂ

௫೔

ᇲ

ି௫೔

௫೔

ቃ

ଶ

ൗሺ݊െ݌ሻ ௡

௜ୀଵ

Where: 

x'i = Predicted (or calculated) amount for the ith calibration standard 

xi = Actual amount for the ith calibration standard 
2010 Methods Update Rule Response to Comments 105 March 2012 

n = the number of calibration points 

p = the number of terms in the fitting equation (average=1, linear=2, quadratic=3) 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 

Comment: No additional controls need to be applied when utilizing the RSE calibration assessment 

alternative. Use of the RSE makes no difference to the chemistry of the analysis but simply provides a 

more consistent and reliable calibration assessment than the currently allowed correlation coefficient. 

Comment: We are very pleased to see RSE included as an alternative calibration assessment model. The 

commonly used correlation coefficient is inadequate as a calibration assessment tool, because it allows 

very large relative errors at the low end of the curve. RSE will not allow curves with these large errors to 

pass calibration criteria. We believe that use of RSE will result in a substantial improvement in the quality 

and reliability of routine data, especially at levels near the lower end of the calibration curve. Several 

major instrument vendors are working towards adding RSE to their instrument software in anticipation of 

the finalization of this rule. 

For consistency with other documents, RSE should be expressed in a slightly different way, as follows: 

(The equation could not be captured from the comments, but is similar to the ones presented in comments 

79 and 83). 

 

Where: y’i = Predicted (or calculated) response for the ith calibration standard yi=Actual response for the 

ith calibration standard n = the number of calibration points p = the number of terms in the fitting 

equation (average = 1, linear = 2, quadratic = 3) 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

We believe it is premature to include the use of relative standard error (RSE) as an approved means of 

evaluating calibrations. Our main concern, after researching the topic, is that the RSE concept is one that 

appears to have been raised at numerous conferences, but only from a single entity. The introduction of a 

new concept, particularly one heavily rooted in statistics is best presented as a separate Federal Register 

Notice in which it is the only issue being proposed, such as the determination of method detection limits. 

In limited evaluation of test data sets using the RSE procedure, we found data which rightfully did not 

meet correlation coefficient criteria, yet the proposed RSE criteria were satisfied. This suggests that the 

approach is not sufficiently rugged. In addition, there are other procedures available, most notably the 

use of the coefficient of determination as presented in SW-846 method 8000. As with other methods in 

SW-846, this approach has not even been considered. 

One of the more important considerations which has not been addressed is how to deal with multiple 

mechanisms for evaluating calibration data. Laboratory certification authorities frequently struggle with 

the reality that where multiple evaluation options exist, laboratories often “pick and choose” which 

approach “works” for a given analyte in a multi-analyte method. Consequently, for a given calibration we 

find some analytes are evaluated against RSD criteria, some against the correlation coefficient, and now a 

third option (RSE) would be available. 

This flexibility facilitates a practice in which a laboratory is focused on using the approach that allows 

them to report a set of data for a given analyte, rather than focusing on production of good quality data. 
2010 Methods Update Rule Response to Comments 106 March 2012 

The first step towards a solution requires the agency to work with all its programs and present a unified 

approach to evaluation of calibration which is weighted more towards data quality than flexibility of 

options. 

Comment 169.1 

Judith R. Morgan 

American Council of Independent Laboratories 

Comment: We are very pleased to see RSE included as an alternative calibration assessment model. The 

commonly used correlation coefficient is inadequate as a calibration assessment tool, because it allows 

very large relative errors at the low end of the curve. RSE will not allow curves with these large errors to 

pass calibration criteria. We believe that use of RSE will result in a substantial improvement in the quality 

and reliability of routine data, especially at levels near the lower end of the calibration curve. Several 

major instrument manufacturers are working towards adding RSE to their instrument software in 

anticipation of the finalization of this rule. 

II.H.3 Adding Other Analytes to Existing Methods 

List of Comments: 

Comment 88.1 - Susan D. Hill, Wisconsin State Laboratory of Hygiene 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 120.1 - David N. Speis, Environmental Laboratory Advisory Board (ELAB) 

Summary of Comments: Numerous commenters questioned the apparent exclusion of the analysis of 

some metals by ICP and ICP/MS procedures. Titanium was frequently cited as an example. Some 

commenters questioned the exclusion of mercury. Other commenters suggested allowing addition of 

analytes to approved methods in general, as long as QA/QC requirements were met.

Response: In response to comments regarding the use of EPA Method 200.7 for measurement of 

titanium, EPA has added Method 200.7 to Table IB as an approved method for measurement of titanium 

because this pollutant is on the list of analytes covered by this method. However, titanium does not 

appear on the analyte lists for EPA Method 200.5, SM 3120, or ASTM D1976, so these methods are not 

listed in Table IB as approved for measurement of titanium. 

With regard to mercury, the sample preparation procedures that are applicable to wastewater samples 

described in Methods 200.7 and 200.8, as well as SM 3120 and 3125 involve strong-acid digestions that 

are usually carried out in open containers at temperatures approaching the boiling point of water (e.g., 85 

to 95oC). Such sample preparation procedures are not appropriate for wastewater samples to be analyzed 

for mercury, due to the volatility of both dissolved elemental mercury and any organo-mercury 

compounds that may be present, which may yield low recoveries of mercury as a result. 

The methods approved for analysis of mercury in wastewater samples include digestion procedures that 

are performed in closed vessels, and digested samples that are purged with an inert gas to quantitatively 

transfer mercury to the analytical instrument. 

Historically, mercury was included as an analyte in Methods 200.7 and 200.8 because in drinking water 

samples that have very low turbidities (i.e., less than 1 nephelometric turbidity units [NTU]), mercury 

may be measured by direct analysis without digestion and without the potential losses through 

volatilization. 

However, since the vast majority of wastewater samples do not have turbidities of less than 1 NTU, 

appropriate digestion of the sample is required. Therefore, EPA has not included Methods 200.7 and 
2010 Methods Update Rule Response to Comments 107 March 2012 

200.8 in Table IB as approved methods for measurement of mercury, and SM 3120-1999 and 3125-2009 

have been removed from Table IB for the analysis of mercury as well. 

With regard to other metal analytes, none of the ICP/AES methods, EPA 200.5 or 200.7, SM 3120, or 

ASTM D1976, list gold, iridium, osmium, palladium, platinum, rhodium, or ruthenium. Therefore, these 

methods do not appear in Table IB as approved for their measurement. 

Standard Method (SM) 3113 B-2004 was not included in Table IB as an approved method for 

measurement of iridium, osmium, palladium, platinum, rhodium, ruthenium, titanium, and zinc because 

the method does not list these as analytes of the method. The method states that it is suitable for 

determination of micro quantities of aluminum, antimony, arsenic, barium, beryllium, cadmium, 

chromium, cobalt, copper, iron, lead, manganese, molybdenum, nickel, selenium, silver, and tin. In 

addition, SM 3113B-2004 states that it is also applicable to analysis of bismuth, gallium, germanium, 

gold, indium, mercury, tellurium, thallium, and vanadium, but precision and accuracy data are not yet 

available. EPA has included SM 3113 B-2004 in Table IB as an approved method for measurement of 

gold, thallium and vanadium. 

Cobalt and molybdenum are not on the analyte list for EPA Method 200.5, but they are in Method 200.7, 

SM 3120, and ASTM D1976. One of the principal differences between Methods 200.5 and 200.7 is that 

Method 200.5 includes the use of the axially viewed torch. By virtue of allowing the use of the axially 

viewed torch in Method 200.7, or the other approved ICP/AES methods, cobalt and molybdenum can be 

analyzed in the same fashion as in Method 200.5, provided that they met the acceptance criteria in the 

approved methods. In either case, e.g., using Method 200.5 or Method 200.7, employing an axially 

viewed torch, the analytical method used to generate the results must be reported as the approved method. 

With respect to the comments recommending that EPA allow the addition of analytes not included in an 

approved analytical method as long as the QA/QC requirements are met, this change is outside the scope 

of this rulemaking. 

EPA also refers readers to a November 7, 2007 memorandum from Richard Reding to Regional QA 

Managers, ATP Coordinators, and NPDES Coordinators on the addition of metals to Methods 200.7 and 

200.8. In any case when an analyte may be added to these methods, the general required QC criteria and 

sensitivity needed for the specific application must be met. 

Original Comment Text: 

Comment 88.1 

Susan D. Hill 

Wisconsin State Laboratory of Hygiene 

The examples of flexibility specified at 136.6 should allow the extension of multi-analyte methods (GC, 

GC/MS, HPLC, ICP, AA, ICP-MS) for use to generate data for similar analytes that are not listed in 

approved methods in the rule. For example, a lab should be allowed to use ICP for the analysis of 

Titanium. 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

The proposed rule summary states, 

“If the underlying chemistry and determinative technique in a modified method are essentially the same 

as an unmodified part 136 method, then the modified method is an equivalent and acceptable alternative 
2010 Methods Update Rule Response to Comments 108 March 2012 

to the approved method. [p 58035]” and, “Acceptable reasons for an analyst to modify a method include 

analytical practices that lower detection limits, improve precision, reduce interferences, lower laboratory 

costs, and promote environmental stewardship by reducing generation of laboratory wastes. Acceptable 

modifications may use existing or emerging analytical technologies that achieve these ends provided that 

they do not depart substantially from the underlying chemical principles employed in methods currently 

approved in 40 CFR part 136.” 

We believe that two critical aspects of method modification, which should be allowed, are not being 

discussed as part of the proposed rule: 

Recognized technologies - Method modification and flexibility should allow the use of generally 

recognized multi-analyte technologies (e.g., GC, GC/MS, HPLC, ICP, AA) to generate data for analytes 

where parallel technologies are approved. (Example: The use of ICP is not allowed in Table IB for 

Titanium, while both graphite furnace AA and ICP/MS methods are approved. Labs routinely and 

successfully use ICP for the analysis of Titanium, and the analyte is listed as a target analyte in EPA 

method 200.7.) 

Extending method target analyte lists - Method modification and flexibility should allow the extension of 

generally approved multi-analyte methods (e.g., GC, GC/MS, HPLC, ICP, AA) to generate data for 

similar analytes that are not listed in approved methods. (Example: SM 3125 is an ICP/MS method 

approved for the analysis of mercury, yet widely used EPA method 200.8 is not.) 

One classic example is Titanium (parameter number 72 in Table IB). The use of ICP technology is not 

allowed for titanium. It is a generally accepted practice to use ICP for the analysis of Titanium, as well as 

for other trace elements for which ICP is not allowed in rule. The technology is approved (for other 

elements), and recognized emission lines have been established. Further, section 1.2 of SW-846 ICP 

method 6010C states, “Other elements and matrices may be analyzed by this method if appropriate 

performance at the concentrations of interest (see Sec. 9.0) is demonstrated “. SW-846 method 6010C was 

most recently revised in 2007, which is significantly more current than revision 4.4 to EPA method 200.7, 

last revised in 1994, which is promulgated in rule. 

 In accordance with the intended flexibility of the proposed rule, a lab should be allowed to use ICP for 

the analysis of Titanium provided that it has determined the potential for inter-element interferences, can 

achieve an MDL that affords adequate sensitivity, and has generated acceptable demonstration of 

capability data. The fact that the EPA or a third party has not published validation data to extend the 

analyte lists to include all of those analytes typically analyzed by a multi-analyte technology should not 

serve as rationale to exclude them. Greater consideration needs to be given to both scientific rationale 

and generally accepted analytical practices used by environmental testing laboratories. 

With respect to our general comment, we ask the following: 

Why does Table IB not allow the use of ICP for the analysis of Ti? Method 200.7 specifically includes Ti 

as an element for which the method has been validated? 

Why is Standard Methods 3113B-1999 approved for Cd, Cr, Fe, Pb, and Ag, while 3113B-2004 is 

approved for Al, Sb, As, Ba, Be, Co, Cu, Au, Mn, Mo, Ni, Se? 

Why is ICP/MS technology but not ICP technology approved for the elements: Au, Ir, Os, Pd, Pt, Rh, Ru, 

Sn, and Ti? 

Why is ICP/MS method SM3125 allowed for the analysis of mercury yet EPA 200.8 (which is routinely 

used for mercury analysis) is not? 
2010 Methods Update Rule Response to Comments 109 March 2012 

Why is EPA method 200.5 not approved for the analysis of Co or Mo? 

Why are 1978 versions of EPA “200” series graphite furnace AA methods approved for a number of 

elements (Au, Ir, Os, Pd, Pt, Rh, Ru, Ti, Zn) when similar, more recently updated Standard Methods 

procedures (SM 3113B-2004) are not? 

Comment 120.1 

David N. Speis 

Environmental Laboratory Advisory Board (ELAB) 

Comment: There is a need for flexibility in adding analytes to EPA-approved methods as long as the 

supporting quality assurance (QA) and QC based on data quality objectives (DQOs) demonstrates 

acceptable data quality. As water quality criteria are adopted for new analytes, this type of method 

flexibility would facilitate more defensible and reliable monitoring of these analytes. Where feasible for a 

given technology, EPA should allow current EPA-approved methods to be used to analyze compounds/ 

analytes in addition to those listed in the methods as long as QA/QC demonstrates acceptable data quality. 

The development of DQOs for individual programs would facilitate this flexibility and reduce the need 

for new methods. ELAB recommends that EPA consider providing this flexibility in the final rule. 

II.H.4 Changes to Method-defined Parameters 

List of Comments: 

Comment 91.1 - Andrea Rex, Massachusetts Water Resource Authority 

Summary of Comments: One commenter recommended that EPA allow modifications to methoddefined parameters as long as the modifications don’t alter the method’s performance in quantifying the 

method-defined analyte. 

Response: Because of the nature of method-defined parameters, modifications to methods approved for 

measurement of such parameters do not fall within the flexibility specified at 40 CFR Part 136.6, and 

therefore must be evaluated by EPA as alternate test procedures under the ATP program, the specifics for 

which can be found at http://water.epa.gov/scitech/methods/cwa/atp/atp_index.cfm. EPA requires 

evaluation of most modifications for method-defined analytes (with some exceptions, such as a smaller 

sample size to minimize interferences, a change in the type of vessels used such as graduated cylinders 

and pipettes that transfer sample) because the results obtained with the method may not be directly 

compared to the results obtained with a modified method. For example, a change in extraction solvent 

may extract different compounds and compound quantities for oil and grease. 

Original Comment Text: 

Comment 91.1 

Andrea Rex 

Massachusetts Water Resource Authority 

Revisions to Method Modification Provisions at 136.6. We endorse the direction EPA is taking on 

method modifications and ask EPA to urge permitting authorities to be receptive to such modifications. 

The restriction from modifying method-defined analytes is too strict. Modifications that don’t alter the 

method’s performance in quantifying the method-defined analyte should be allowed. 

II.H.5 Metals Digestion Changes 

List of Comments: 
2010 Methods Update Rule Response to Comments 110 March 2012 

Comment 92 - Lee Wolf, Columbia Analytical Services, Inc. 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Summary of Comments: Two commenters requested clarifications regarding digestion procedures for 

metals. One questioned whether the digestion could be modified at all. The other asked that the closedvessel sample preparation steps from EPA Method 1638 be cited as an allowed modification for other 

digestions. 

Response: EPA notes that digestion procedures are similar to methods that measure method-defined 

parameters in that the digestion procedures specified in the approved methods will define the forms and 

species of the analyte that are measured as part of the “total” measurement. The specific acids used and 

the overall acid strength will affect how much metal may be released from the sample matrix, and this 

effect may vary across different metals. An extreme example is the use of hydrofluoric acid (HF) to 

completely dissolve any minerals in a sample, versus the currently approved digestion procedures that 

will not. 

Therefore, modifications to digestion procedures in methods that measure “total” analytes (e.g., total 

metals, total cyanide, total Kjeldahl nitrogen, and total phosphorus) do not fall within the flexibility to 

modify methods allowed at part 136.6. EPA has included the following text in part 136.6(b)(4)(T) to 

clarify this point: "The use of gas diffusion (using pH change to convert the analyte to gaseous form 

and/or heat to separate an analyte contained in steam from the sample matrix) across a hydrophobic semipermeable membrane to separate the analyte of interest from the sample matrix may be used in place of 

manual or automated distillation in methods for analysis such as ammonia, total cyanide, total Kjeldahl 

nitrogen, and total phenols. These procedures do not replace the digestion procedures specified in the 

approved methods and must be used in conjunction with those procedures." 

As reasoned by the state agencies cited by one commenter, these measurements have been used to create 

regulatory limits specified in many permits. Thus, the “equivalent or better” performance (emphasis 

added) cited by the commenter is the concern. Modifications to these procedures have the potential to 

change the results obtained in a given discharge and only are allowed under the ATP program, which 

requires data demonstrating comparability to the approved methods using a study design that has been 

agreed upon by the Regional Coordinator or permitting authority. These types of modifications require 

approval according to the procedures specified at 40 CFR parts 136.4 and 136.5. 

In contrast, the closed-vessel digestion procedure in EPA Method 1638 uses the same acids as specified in 

the 200-Series EPA and VCSB methods, at similar concentrations. It differs from those procedures in the 

means of heating the sample, placing the sample in a capped bottle and heating the bottle in an oven at 85 

oC, rather than in an open beaker on a hot plate held at the same temperature. The closed-vessel digestion 

produces comparable results as the digestions in other approved methods. EPA agrees with this comment 

and has included the following text in part 136.6(b)(4)(E): "The use of EPA Method 200.2 or the sample 

preparation steps from EPA Method 1638, including the use of closed-vessel digestion, is allowed for 

EPA Method 200.8, provided the method performance specifications relevant to the ICP-MS are met." 

 

Original Comment Text: 

Comment 92 

Lee Wolf 

Columbia Analytical Services, Inc. 

Using a more vigorous metals digestion (more concentrated acid and/or longer reaction time - as found in 

SW-846 or CLP digestions) than that found in the 200 series methods should be interpreted as falling 

under the conditions of “allowable changes.” Some state agencies have specifically disallowed modifying 

the 200 digestion, although a more vigorous digestion produces “equivalent or better performance” and 
2010 Methods Update Rule Response to Comments 111 March 2012 

falls under the “acceptable reasons for an analyst to modify a method including analytical practices that... 

lower laboratory costs (by batching) and do not depart substantially from the underlying chemical 

principles employed in methods currently approved in 40 CFR part 136.” The state agencies have used 

the reasoning that metals undergoing a more rigorous digestion may produce higher than historical results 

for the method. Since metals are not defined as “method-defined analytes”, a digestion which meets the 

QC of the analytical method should be acceptable. We would like to see this specific example addressed. 

Comment 132.1 

Paula Hogg 

Hampton Roads Sanitation District 

Comment/Recommendation HRSD supports the clarification of the closed-vessel sample preparation 

steps from EPA Method 1638 as an allowable method modification. 

II.H.6 Use of Selected Ion Monitoring (SIM) 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 166.1 - Paul Wiegand, National Council for Air and Stream Improvement, Inc. 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Summary of Comments: Several commenters welcomed inclusion of selected ion monitoring (SIM) as 

an allowed modification for GC/MS methods and thought the suggested approach provides a sound 

balance. One commenter questioned the citation to the specific criteria and recommended that they be 

made consistent with those from the RCRA program (e.g., SW-846). Another commenter objected to the 

allowance for SIM, claiming it represents a change to the determinative technique and thus requires 

thorough validation before it could be approved. 

Response: EPA appreciates the commenters in support of this additional approach allowing the use of 

the SIM mode for analytes that cannot be effectively analyzed in full-scan mode. With respect to the 

specific criteria, EPA developed these criteria to ensure that appropriate limits are in place when 

generating data using the SIM mode in methods that employ GC/MS as the determinative technique. 

These criteria have been developed for use when performing compliance monitoring under the Clean 

Water Act and may differ from requirements developed for use in other programs. More specifically, 

EPA notes that methods in the SW-846 manual are issued by the Office of Resource Conservation and 

Recovery (ORCR) as guidance, and are generally not required for use in complying with RCRA 

regulations. Neither program requires that SIM be used, but in allowing its use as a modification to an 

approved monitoring method for CWA compliance using the criteria specified in part 136.6, EPA sought 

to strike a balance aimed at minimizing the likelihood of false positives, which are more of a concern 

when using SIM than full scan analysis. 

EPA does not agree that the use of SIM represents a change in the determinative technique of the method 

because it uses the same technique (mass spectrometry) as the full scan mode. The main difference is that 

the SIM mode gathers data for selected masses of interest rather than scanning for all masses over a wide 

range of mass to charge ratios. EPA also disagrees that the technique will most often be used to improve 

sensitivity. Although it is true that sensitivity generally increases, the primary reason to use SIM is that it 

is an excellent tool to reduce interferences with the target analytes. Therefore, EPA will allow the use of 

SIM under part 136.6. 
2010 Methods Update Rule Response to Comments 112 March 2012 

Original Comment Text: 

The following commenters supported the additional guidance for adopting SIM analysis. 

Comment 79.1 Richard Burrows, TestAmerica Inc. 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 169.1 Judith R. Morgan, American Council of Independent Laboratories 

Other comments: 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

Section 136.6 (b) (S) includes previously accepted modifications. Section xv discusses criteria specified 

in the proposed rule for SIM analyses. We were unable to locate where these criteria were previously 

specified. The section goes into specifics on retention times, number of scans, ratio acceptance criteria, 

etc. Some of these criteria are more specific than what is required in SW-846. If the criteria are going to 

be specified for acceptable data using SIM, it needs to correspond with RCRA methodology and 

acceptable procedures to provide consistency across programs and similar methods and technologies. 

Comment 166.1 

Paul Wiegand 

National Council for Air and Stream Improvement, Inc. 

EPA should not allow use of Selected Ion Monitoring as a method modification because it (a) represents a 

change in the final determinative step; (b) would be applied at levels below those for which a method has 

been validated; and (c) includes no requirement to verify selectivity. EPA should withdraw this proposed 

allowed modification until sufficient supporting data are made available. 

EPA has proposed that modifying a method from full scan GC/MS to Selected Ion Monitoring (SIM) is 

an allowed modification provided certain criteria it sets forth are met. We believe this is an inappropriate 

interpretation of its own restriction against modifying the final determinative step. EPA claims that this 

has been done successfully in the past, but does not provide any data substantiating that claim. While we 

recognize that under certain circumstances this may be a reasonable modification, for the vast majority of 

other situations it should only be allowed after very careful evaluation and validation. 

The most probable reason for utilizing SIM is to improve sensitivity. Thus, this change would be applied 

in concentration ranges where the promulgated method has never been validated. Furthermore, reducing 

the amount of spectral information available to analysts increases the potential for false positives or bias. 

These considerations justify the need for very careful and targeted validation before the acceptability of 

the SIM approach can be determined. 

The criteria that EPA has set forth to document method performance when an analyst modifies the 

method do not include any meaningful demonstration of selectivity. About all they demonstrate is that 

other analytes do not interfere or are not misidentified. Thus, EPA’s proposal fails to provide any 

meaningful verification of selectivity in any type of sample. This is of particular concern considering that 

the measurements would be made in an unexplored concentration range where selectivity would most 

likely be challenged. 

The number of ions and ion ratio criteria proposed by EPA are inadequate to assure confident substance 

identification for all potentially regulated substances. The limitations of EPA’s proposed criteria are 

apparent when one looks at the detailed requirements that were thoughtfully developed and adopted in the 

European Union (see Commission Decision of 12 August, 2002, implementing Council Directive 
2010 Methods Update Rule Response to Comments 113 March 2012 

96/23/EC concerning the performance of analytical methods and the interpretation of results). Clearly 

what EPA has proposed does not meet widely accepted scientific criteria. 

We recommend that EPA withdraw its proposal with respect to Selected Ion Monitoring until such time 

as EPA develops meaningful and thorough sensitivity testing and validation protocols, develops more 

robust ion and ion ratio criteria, tests these procedures on representative methods, and submits the overall 

approach to peer review. 

II.H.7 Holding Times and Preservation Changes 

List of Comments: 

Comment 91.1 - Andrea Rex, Massachusetts Water Resource Authority 

Summary of Comments: One commenter requested that changes to holding times and sample 

preservation be explicitly prohibited and suggested changes to 136.6 (b)(3) to that effect. 

Response: EPA notes that holding times, while often listed in EPA methods, are governed by Table II at 

40 CFR 136, and Table II requirements take precedence over holding times specified in the methods as 

noted in a previous rulemaking. Thus, the suggested sentence is in part incorrect. However, to help 

clarify, EPA has modified 136.6(b)(3) as follows: “An analyst may not modify any sample collection, 

preservation or holding time requirements of an approved method. Such modifications to sample 

collection, preservation and holding time requirements do not fall within the scope of the flexibility 

allowed at Part 136.6.” 

Original Comment Text: 

Comment 91.1 

Andrea Rex 

Massachusetts Water Resource Authority 

The following sentence should be modified to comport with section II.F of this proposed rule that 

describes how sample preservation and holding time requirements can be modified: “An analyst may not 

modify any sample preservation and/or holding time requirements of an approved method.” 

II.H.8 Calibration Models 

List of Comments: 

Comment 112.1 - Colin Elliott, King County Environmental Lab 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 157.1 - Marlene Moore, Advanced Systems, Inc 

Summary of Comments: One commenter objected to statements that results should not be extrapolated 

beyond the demonstrated calibration range when using a quadratic calibration model. Another 

commenter stated that additional requirements must be placed on the use of quadratic models, including 

the use of multiple concentrations for verifying the curve, and restrictions on when a quadratic model can 

be applied that are in keeping with those in the SW-846 methods manual. A third commenter 

recommended more radical changes to EPA’s approach to calibration curves and acceptance criteria. 

Response: EPA disagrees that it is appropriate to extrapolate results when using a quadratic calibration. 

Many approved methods specifically require that when sample results fall outside of the calibration range, 

the sample must be diluted and re-analyzed so that the result falls within the lowest and the highest 

standards used for calibration. Those methods that allow extrapolation of results often require that a 
2010 Methods Update Rule Response to Comments 114 March 2012 

“linear range” standard above the highest calibrator be analyzed periodically as a check on such 

extrapolations. Therefore, EPA is maintaining its position that all reported sample results must be within 

the range determined during initial calibration of the method. Any samples with results above this range 

must be diluted and reanalyzed for reporting purposes. 

EPA disagrees that additional requirements on quadratic calibration beyond those in the proposal (such as 

those in SW-846) are needed because calibration verification standards are part of the ongoing quality 

controls that are specified in the approved methods and the additional clarifying language suggested is 

unnecessary. Therefore, EPA is finalizing the language as proposed. 

Although the approach to calibration curves and acceptance criteria suggested by the third commenter 

may have merit, it represents a massive change to all approved methods, and goes beyond the scope of 

both the discussion of allowed flexibility, and the scope of today’s rulemaking. EPA may consider 

whether additional requirements are needed for calibration in the future. 

Original Comment Text: 

Comment 112.1 

Colin Elliott 

King County Environmental Lab 

Comment: Not allowing concentrations to be extrapolated above the most concentrated calibrator when 

using a quadratic curve is too restrictive. We believe that instrument responses above the highest 

calibration standard may still be within the expected accuracy of the method. We propose that 

concentrations may be extrapolated above the highest calibration standard as long as all responses above 

the curve are confirmed to be accurate. This can be done by running a continuing calibration verification 

or other check standard that is at a concentration at or above the extrapolated data point. This standard 

must pass the same method criteria for all other continuing calibration standards. 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

New language has been added to Part 136.6 (b) (S) (x) to address the use of non-linear or quadratic 

calibration models. Some calibration models for certain methods exhibit quadratic character and in these 

instances, a quadratic fit would be a more adequate fit than a linear fit model. However, the only 

stipulations written into the new MUR for using quadratic fits are the following: 1) use a minimum of six 

standards and 2) no extrapolations of instrument responses that exceed the most concentrated calibrator. 

While these stipulations are necessary, additional requirements must be added for using non-linear or 

quadratic calibration models. Since the nature of quadratic fit models usually involves at least one or two 

points of inflection, the importance of verifying accuracy through the entire analytical range cannot be 

understated. This is especially important for the lowest and highest concentrated calibration standards. 

Therefore, if a quadratic calibration model is established, check standards must be analyzed after 

calibration that verify the accuracy of the lowest, mid-range, and highest calibration standards with 

acceptable percent difference criteria specified. Also, additional language must be added to provide 

clarification concerning the conditions under which a non-linear calibration model may be used. Nonlinear calibrations must not be used to compensate for detector saturation at higher concentrations or to 

avoid proper instrument maintenance. Non-linear calibrations must also not be used for methods or 

instruments previously shown to exhibit linear calibration for the analytes of interest. This language can 

be found in section 7.5.3 of EPA 8000B of the SW-846 methods. This same philosophy regarding the use 

of non-linear calibrations must be added to the new MUR. 
2010 Methods Update Rule Response to Comments 115 March 2012 

Comment 157.1 

Marlene Moore 

Advanced Systems, Inc. 

The use of the RSE and correlation coefficients must be changed as the evaluation criteria for calibration 

curves. Adding the use of the RSE provides only a partial evaluation of the calibration. The industry has 

allowed criteria for acceptable calibration that is not sufficient to ensure quality data. In addition the 

acceptable performance of the ICV and CCV (QC checks) are just checks, and must not be used as the 

criteria for calibration acceptance. Please refer to the following document for a detailed review of how to 

evaluate calibration data that must be part of any quality control program. As we venture toward a 

performance approach to generating data, we must ensure the difference between checks and method 

performance are more clearly defined. 

“Preparation of Calibration Curves, A Guide to Best Practices”, September 2003, LGC/VAM/2003/032. 

“The aim of this guide is to highlight good practice in setting up calibration experiments, and to explain 

how the results should be evaluated. The guide focuses on calibration experiments where the relationship 

between response and concentration is expected to be linear, although many of the principles of good 

practice described can be applied to non-linear systems.” 

http://www.nmschembio.org.uk/PublicationArticle.aspx?m=115&amid=472 

The evaluation of the calibration is a critical element that must be added as part of the calibration review 

(40 CFR 136.7 a. item 7). Laboratories not performing this type of evaluation are subjecting data users to 

poor quality data as was demonstrated in the inter-laboratory study that resulted in this reference paper 

being generated and has been the case in many proficiency testing studies for the WS and WP programs. 

(This may be one of the reasons many laboratories are allowed to say ‘the QC passed but the PT failed 

and we can’t find a reason.’ So as an assessor I have no recourse but to attempt to convince the laboratory 

that other QA items influence this result including poor calibration.) 

Please require more than a correlation coefficient or RSE for evaluation calibration curve and more than 

just an ICV and CCV check. Please require the evaluation of calibration curves using consensus 

documents such as the LGC/VAM/2003/032. 

II.H.9 Gas Diffusion 

List of Comments: 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Summary of Comments: One commenter requested clarification regarding the use of gas diffusion. 

Response: In response to this comment, EPA has clarified the language at part 136.6 (b)(4)(T) to read as 

follows: “The use of gas diffusion (using pH change to convert the analyte to gaseous form and/or heat to 

separate an analyte contained in steam from the sample matrix) across a hydrophobic semi-permeable 

membrane to separate the analyte of interest from the sample matrix may be used in place of manual or 

automated distillation in methods for analysis such as ammonia, total cyanide, total Kjeldahl nitrogen, and 

total phenols. These procedures do not replace the digestion procedures specified in the approved 

methods and must be used in conjunction with those procedures.” 

Original Comment Text: 
2010 Methods Update Rule Response to Comments 116 March 2012 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

Part 136.6 (b) (4) (A) references the use of gas diffusion. Please provide clarification for which 

parameters and method numbers would be allowed the modification with gas diffusion. It is unclear what 

specifically constitutes gas diffusion when used in lieu of distillation. If this is referring only to flow 

injection analysis, then it should be specifically stated as such. 

II.H.10 Collision Cell for ICP/MS 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 120.1 - David N. Speis, Environmental Laboratory Advisory Board (ELAB) 

Comment 125.1 - John H. Phillips, Ford Motor Company 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Comment 176.1 - James N. Christman, Utility Water Act Group (UWAG) 

Summary of Comments: Six commenters were strongly in favor of allowing the use of a collision cell 

device in ICP/MS analyses, with many citing improved performance for chromium, arsenic, selenium and 

vanadium. One commenter was supportive, but requested that additional details be provided, citing an 

approach that EPA is currently studying for use in a specific complex matrix (flue gas desulfurization 

effluents) from the steam electric power generating industry. 

Response: EPA thanks the commenters for their support of the use of collision cell techniques. EPA 

reviewed the comments on the industry-specific approach under study and agrees that such additional 

controls may be useful for those complex matrices. The current approval of the collision cell technology 

is allowed for more general uses in analyses of many wastewater matrices. However, analysts may add 

additional controls for specific complex matrices to address matrix interferences. 

Original Comment Text: 

The following commenters supported the use of collision cells. 

Comment 79.1 Richard Burrows, TestAmerica Inc. 

Comment 94.1 Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 120.1 David N. Speis, Environmental Laboratory Advisory Board (ELAB) 

Comment 125.1 John H. Phillips, Ford Motor Company 

Comment 132.1 Paula Hogg, Hampton Roads Sanitation District 

Comment 169.1 Judith R. Morgan, American Council of Independent Laboratories 

Other comments: 

Comment 176.1 

James N. Christman 

Utility Water Act Group (UWAG)` 

Allowing collision or reaction cells for ICP-MS is desirable, but EPA has not provided enough details 

At 75 Fed. Reg. 58,069 col. 3 EPA proposes to allow the use of collision or reaction cells for ICP-MS: § 

136.6(b)(5)(iv) 
2010 Methods Update Rule Response to Comments 117 March 2012 

In general, ICP-MS is a sensitive and selective detector for metal analysis; however isobaric interference 

can cause problems for quantitative determination as well as identification based on the isotope pattern. 

Interference reduction technologies, such as collision or reaction cells, are designed to reduce the effect of 

spectroscopic interferences that may bias results for the element of interest. The use of interference 

reduction technologies is allowed provided the method performance specifications relevant to ICP-MS 

measurements are met. UWAG supports this change. 

Standard mode inductively coupled plasma-mass spectrometry (ICP-MS) is typically performed 

according to EPA method 200.8 (unmodified) on a standard ICP-MS instrument that lacks any type of 

collision cell or dynamic reaction cell (DRC) based molecular ion (polyatomic) interference control 

technology. In sample matrices with elevated calcium and chloride concentrations (such as elevated TDS 

FGD wastewaters), standard mode ICP-MS cannot control the molecular ion interferences associated with 

these interferants, and, as a result, routinely overstates the true concentrations of several elements such as 

arsenic, selenium, chromium, and nickel. The problem occurs not only with FGD wastewaters; UWAG 

members have found the same overstatement of selenium and arsenic using the unmodified method on 

discharges from ash treatment ponds. 

In an effort to minimize such matrix specific interferences, interference control cell technologies have 

been developed which attempt to break up or remove the molecular ion interferences (e.g., argon or 

calcium chloride, which mimics arsenic-75) and allow accurate elemental measurements even in complex 

sample matrices. 

UWAG provided detailed recommendations on using inductively coupled plasma mass spectrometry for 

flue gas desulfurization wastewater in letters of March 19 and April 6, 2010, which are attached to these 

comments and expressly incorporated herein. See Letter, UWAG to Ronald P. Jordan and Richard W. 

Reding, March 19, 2010; Letter, UWAG to Ronald P. Jordan and Richard W. Reding, April 6, 2010. In 

particular, UWAG recommended, and still recommends, conducting the analysis of flue gas 

desulfurization wastewater with multiple mass numbers and using additional quality control measures, 

such as a National Institute of Standards and Technology standard or equivalent, to verify results. 

II.H.11 Other Comments 

List of Comments: 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 123 - Vincent Sapienza, Bureau of Wastewater Treatment, New York City Department of 

Environmental Protection 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Comment 183.1 - Sanwat Chaudhuri, Utah Public Health Department 

Comment 187 - Peter Halpin, Caltest Analytical Laboratory 

Comment 190 - Lynn Egan, Lachat Instruments 

Summary of Comments: EPA received comments on a variety of other topics that were difficult to 

categorize. One commenter supported the allowed modifications to Method 625, but noted that the bulk 

of the 600-Series methods date to 1984 and wondered when these methods would be revised. Another 

commenter supported changes to purge-and-trap methods, but requested that EPA makes the allowed 

modifications or restrictions consistent across the wastewater and drinking water programs. A third 

commenter requested that pH meters be permitted for monitoring sample pH to affect better control of 

extraction pH to a optimal range for the analytes of interest. One commenter requested that the Agency 

establish data quality objectives to facilitate method flexibility. Another commenter specifically 

requested adding changes to desorb time for purge-and-trap methods as an allowed modification. 
2010 Methods Update Rule Response to Comments 118 March 2012 

Another commenter recommended explicitly allowing solid-phase extraction, solid-phase microextraction, and changes in the detector system. One commenter requested changes to a section of the 

preamble regarding allowed modifications to state that the Agency strongly encourages regulatory 

authorities to allow such modifications. 

Response: With respect to the 600-series methods, EPA recognizes that many of these methods are 

older. However, revision of these methods is beyond the scope of this rule. The existing allowances for 

modifications described in today’s rule are included in part 136.6 to address some of the issues of concern 

with 600-series methods regarding allowable modifications. 

With regard to changes in purge times and inconsistencies across EPA programs, EPA notes that the 

methods approved for the drinking water and wastewater programs are intended for different uses and 

therefore may have different requirements. Unfortunately, it is not possible to always have a consistent 

response because of the differences between the two programs and matrix types. The purge times for 

methods used for compliance monitoring in drinking water fall outside of the scope of the changes that 

were proposed and thus are not included in today’s rule. 

Regarding the use of a pH meter to monitor extraction pH, as the commenter notes, the prohibition stems 

from concerns with contamination of the sample by the pH electrode that can be avoided by not inserting 

anything directly into the sample to be analyzed. The extraction pH ranges specified in some methods are 

relatively wide, and were designed to accommodate many types of samples without the need to adjust pH. 

EPA recognizes that some analytes may have narrower optimal ranges for extraction that the method does 

not disallow narrowing the pH range by using “narrow range pH paper” or some other non-intrusive 

means. Alternatively, a laboratory could submit a procedure using a pH meter as an ATP, provided 

sufficient study and documentation was produced. 

The development of data quality objectives (DQOs) for compliance monitoring falls outside of the scope 

of this rule. As a general rule, a single set of DQOs is not practical for all regulatory situations. For 

example, DQOs used for monitoring compliance with water quality standards could involve very different 

considerations than those used for technology-based effluent guidelines or other approved uses of CWA 

methods. 

Regarding desorb times, Part 136.6 (b)(4)(P)(5) allows changes in purge-and-trap sample volumes or 

operating conditions such as: “Changes to the desorb time. Shortening the desorb time (e.g., from 4 

minutes to 1 minute) may not affect compound recoveries, and can shorten overall cycle time and 

significantly reduce the amount of water introduced to the analytical system, thus improving the precision 

of analysis, especially for water soluble analytes. A desorb time of four minutes is recommended, 

however a desorb time may be used, provided that all QC specifications in the method are met.” Thus, no 

additional changes are needed in this rule. 

EPA agrees that there are merits to the use of solid-phase extraction, and where practical, EPA has 

allowed its use in wastewater methods, either directly in those methods, or through ATPs. However, 

there are limits to the ability of such techniques to handle the dissolved and suspended solids in many 

wastewater samples. For this reason, EPA only allows the use of these techniques for specific applications 

and has concluded that it is not appropriate to provide a blanket approval. Many methods that employ 

solid-phase extraction stipulate performance requirements on the solid-phase materials, i.e., disks, 

cartridges, or other forms. For example, the laboratory may be required to test representative materials 

from each “lot” of cartridges purchased from a supplier to determine their capacity to adsorb potential 

interferences and release target analytes. Those methods provide performance metrics and acceptance 

criteria that have no counterparts in methods that do not describe the use of solid-phase extraction. 

Absent such performance criteria, there is no way that a laboratory, or a data user, can ensure that a 
2010 Methods Update Rule Response to Comments 119 March 2012 

modification that employs solid-phase extraction is performing adequately for monitoring under CWA 

programs. 

The use of solid-phase micro-extraction presents even greater challenges than other sorptive extraction 

techniques. The key issue remains how to demonstrate that “these approaches meet the monitoring 

objective.” 

Changes in the detection system (e.g., the use of a mass spectrometer that is not specified in a method 

instead of gas chromatography) are not allowed because such changes are a fundamental change of the 

measurement technique and require a demonstration of performance under the alternate test procedures 

(ATP) program. 

 

Thus, EPA does not allow blanket the use of solid-phase extraction or the use of alternate detector such as 

a mass spectrometer that is not specifically allowed in a given method. These changes do not fall within 

the flexibility to modify methods allowed at part 136.6 and require approval under the ATP program as 

described in parts 136.4 and 136.5. 

Finally, with regard to the recommended changes for the language on Page 58035 of the proposal 

recommending that EPA strongly encourage permitting authorities to allow method modifications, that 

text was part of the preamble to the proposed rule and not part of the regulatory text. Therefore, no 

change to the regulatory text is needed. 

Original Comment Text: 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 

Comments on additional controls: (1) for pH change must: gain better detection limit(s), produce less 

matrix interference, and achieve higher accuracy and precision; (2) for purge times change must: remain 

linear in calibration curve for all compounds, maintain minimum required total purge flow, improve 

reporting limits, and result in less instrument downtime or surrogate failure due to less water purged into 

the system. 

Even though the proposed rule allows some limited modifications for some methods, the full text of EPA 

Methods 601 - 610, 624, and 625, given in Appendix A, have not been revised since 1984. These 600 

series methods still reference packed columns, old types of glassware for sample preparation, and threepoint calibration. Also, the precision and accuracy studies were outdated since they were completed by 

old technology more than 25 years ago. When are these methods going to be revised? 

Comment: The modifications to method 625 allowed are useful for optimizing the method for different 

matrices and are in line with techniques that have been in use for several years. 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

While we support the allowance of alternate purge times, we respectfully request that the agency work 

towards a unified position with respect to this issue. 

The drinking water program, in particular, specifically does not allow any modification of purge times 

from those published in method s 524.2 or 502.2. The language in the EPA document, “Technical Notes 

on Drinking Water Methods (EPA-600/R-94-173) states, 
2010 Methods Update Rule Response to Comments 120 March 2012 

“The use of alternative sorbents is acceptable provided the data acquired meets all quality control criteria 

described in Section 9, and provided the purge and desorption procedures specified in Section 11 of the 

method are not changed.” and, “...the purge and desorption procedures specified in the methods are 

optimized for the trap media specified in the methods. These procedures may not be changed. 

Specifically, the purge time, purge gas flow rate, and the desorption time specified in the method may not 

be changed, because EPA has no data to show that reliable or reproducible results can be obtained if 

purging or desorption times or flows differ from the specified limits.” 

It would appear that this language represents an agency-wide opinion in conflict with proposed changes to 

40 CFR Part 136. If alternate purge times are allowed for samples analyzed under the Clean Water Act, 

which arguably pose more significant matrix-based challenges, then alternate purge times should be 

allowed for drinking water analysis. 

Comment 123 

Vincent Sapienza 

Bureau of Wastewater Treatment, New York City Department of Environmental Protection 

EPA should allow use of a pH meter and electrode for the measurement of pH during the sample 

preparation steps if an analyst determines that tight control of pH is necessary for the more reliable 

analysis of the parameters and if the analyst can demonstrate that the procedure utilizing the pH meter and 

electrode will not compromise the integrity of the sample. For example, in EPA method 608, the pH 5 to 

9 is mentioned as acceptable pH for sample extraction. Based on our lab experience, this range is very 

wide. If the sample extracted is at the extreme edge of either side of the range of pH, it certainly affects 

the percent recovery of a group of compounds. The best range of pH for the extraction of pesticides is 7.3 

± 0.2, which cannot be controlled practically by the use of pH paper, especially in the wastewater 

samples. In the organic analyses, the use of a pH electrode is generally not an accepted practice because 

of a concern that there will be contamination or loss of chemicals of interest because they might stick to 

the electrode. We believe that the improved recovery of chemicals effectuated by the use of electrodes 

will outweigh those two concerns and benefit science and analysis. 

Comment 132.1 

Paula Hogg 

Hampton Roads Sanitation District 

Comment/Recommendation HRSD supports the concept of method flexibility. However, established EPA 

Program Data Quality objectives must drive and facilitate method flexibility. 

There is a need for flexibility in adding analytes to EPA approved methods as long as supporting QA/QC 

based on data quality objectives demonstrates acceptable method performance. As Water Quality 

Standards are added, this type of method flexibility would facilitate more consistent monitoring of these 

constituents. 

Comment/Recommendation: Where feasible for a given technology, allow for addition of 

compounds/analytes for current EPA approved methods as long as QA/QC demonstrates acceptable 

method performance. Develop data quality objectives for programs that would facilitate this flexibility 

and address the need for new methods. 

Comment 169.1 

Judith R. Morgan 

American Council of Independent Laboratories 
2010 Methods Update Rule Response to Comments 121 March 2012 

Comment: The modifications to method 625 allowed are useful for optimizing the method for different 

matrices and are in line with techniques that have been in use for several years. 

Comment 183.1 

Sanwat Chaudhuri 

Utah Public Health Department 

We support modification of 40CFR 136.6 to allow flexibility without departing "substantially from the 

underlying chemical principles employed in methods currently approved in 40 CFR 136". We recommend 

adding desorb time to the example of flexibility. 

The GC/MS method for EPA 524.2 requires 4 minutes of desorb time, whereas the newer GC/MS need 

only 1 minute desorb time to obtain the same method precision and accuracy of EPA method 524.2. 

When the desorb time is increased to 4 minutes with these newer GC/MS, the instrument response time 

goes down resulting in unacceptable data quality. By changing the desorb time to 1 minute the laboratory 

saves time while maintaining the same QC requirements of the method. 

Therefore we recommend that desorb time be added to the examples of flexibility specified at 136.6. 

Comment 187 

Peter Halpin 

Caltest Analytical Laboratory 

In the spirit of the March 2007 Method Update Rule that applied to Clean Water Act analyses and 

sampling procedures we are requesting that you include flexibility to reduce costs where feasible and 

where the changes do not result in a reduction of data quality. Specifically in allowing alternate extraction 

procedures, addition of an analyte, and the use of mass spectrometer detectors for all semivolatile analytes 

where the mass spectrometer is capable of providing sufficiently sensitive detection limits for the purpose 

of the analysis. 

For example, where extractable organics can be demonstrated to be adequately extracted from the target 

water by solid phase extraction, we advocate allowing the solid phase extraction. This would result in 

much less use of the toxic methylene chloride solvent, and generate less waste. Some methods explicitly 

allow solid phase extraction, some are too old to make reference to the technique. In addition to solid 

phase extraction, other green chemistry approaches that minimize solvent waste, hazard, and analyst time 

include stir bar sorptive extraction, and solid phase microextraction. When these approaches can be 

shown to meet the monitoring objective it would be helpful to be able to use them for compliance 

purposes, and not just for informational studies (variations of the stir bar sorptive extraction can be used 

to extract the solids in a wastewater to allow for “whole water” extraction as opposed to the otherwise 

assumed extraction of only ‘dissolved’ analytes). 

We understand the difficult nature of meeting legal issues with respect to the Clean Water Act, and 

advancing and improving the analytical methods of compliance. We applaud the 2007 Method Update 

rule with respect to allowing minor changes that do not hinder the generation of sound data, suitable for 

the use for which it was collected. We encourage you to add as much flexibility as possible to this round 

of updates, all the while maintaining the generation of sound data, not only suitable for the use for which 

it was collected, but also more and more cost effective. We also encourage the taking advantage of the 

improvement of the tools of analyses as they come available, some of which we listed in our comments. If 

we can be of any help feel free to contact us. 

Comment 190 

Lynn Egan 
2010 Methods Update Rule Response to Comments 122 March 2012 

Lachat Instruments 

The additional information in the proposed rule (section 136.6) will help to further clarify acceptable 

modifications, as well as the requirements for the validation and use of a modified method. But in those 

places where methods that fall under the MUR have not been allowed to date, it seems unlikely that 

additional explanation will have a large impact --NOT to allow the use of modified methods is already the 

rule. 

Within the text of these first few paragraphs, the addition of (or at least reference to) information in 

section 136.6 and allowed flexibility/use of modified methods should be added. Without this text, it 

seems possible (if not likely) that Table IB will be taken literally and those modifications that are allowed 

at the Federal level are even less likely to be allowed by States. 

P58035 (H): "EPA encourages regulatory authorities to allow analysts the flexibility to modify CWA 

methods without prior approval provided the user has documented equivalent or better performance...." 

Restate as "EPA strongly encourages regulatory authorities to allow analysts the flexibility to modify 

CWA methods without prior approval, provided the user has documented equivalent or better 

performance...." 

Section II.I Proposed New QA/QC Language at 40 CFR 136.7 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 81 - Jack Hauskins, City of Lafayette, TN 

Comment 82 - LeeAnna Hutchings, Great Salt Bay Sanitary District Damariscotta, ME 

Comment 88.1 - Susan D. Hill, Wisconsin State Laboratory of Hygiene 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 92 - Lee Wolf, Columbia Analytical Services, Inc. 

Comment 93 - David Howell, City of Tampa 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 

Comment 96.1 - Denise Paige, Tennessee Municipal League (TML) 

Comment 97 - Dewayne Culpepper, Tennessee Association of Utility Districts (TAUD) 

Comment 101.1 - New York State Department of Environmental Conservation 

Comment 105 - Sandra Dudley, Water Authority of Dickson County 

Comment 106.1 - Charles Boepple, Upper Occoquan Service Authority 

Comment 107.1 - Patsy Root, IDEXX Laboratories 

Comment 109.1 - Andre Brousseau, Maine Wastewater Control Association 

Comment 110.1 - Laurie Curra, Texas Commission on Environmental Quality 

Comment 112.1 - Colin Elliott, King County Environmental Lab 

Comment 113.1 - Susan E. Butts, South Carolina Department of Health and Environmental Control 

Office of Environmental Laboratory Certification 

Comment 116.1 - Wendy Harding and Mala Burton, Joint Virginia Water Environment Association and 

Virginia American Water Works Association 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 120.1 - David N. Speis, Environmental Laboratory Advisory Board (ELAB) 

Comment 124.1 - Thomas Tourje, Augusta County Service Authority 

Comment 125.1 - John H. Phillips, Ford Motor Company 

Comment 126.1 - Sterling Pierce, Maine Department of Environmental Protection 

Comment 130.1 - Heather L. Beard, Richland County Utilities 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 133.1 - Terri Grimes, Pinellas County Utility Laboratories 

Comment 151. 1- Aaren S. Alger, Pennsylvania Department of Environmental Protection 
2010 Methods Update Rule Response to Comments 123 March 2012 

Comment 152.1- James Matthew, On Line Environmental Inc (OLE) 

Comment 154.1 - Sharon Mertens, Milwaukee Metropolitan Sewerage District 

Comment 157.1 - Marlene Moore, Advanced Systems, Inc 

Comment 158. 1- Jerry Parr, The NELAC Institute 

Comment 161.1 - Carol Batterton, Water Environmental Association of Texas 

Comment 162.1 - Ed Saxon, South Carolina Water Quality Association 

Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility 

Comment 166.1 - Paul Wiegand, National Council for Air and Stream Improvement 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Comment 171.1 - Lola Guerra, Henrico County DPU 

Comment 177.1 - Novelle C. Stokes, South Central Wastewater Authority 

Comment 189.1 - William Ray, California State Water Resources Control Board 

Comment 190 - Lynn Egan, Lachat Instruments 

Summary of Comments: Although some commenters expressed support for EPA’s intent with the new 

QC language, many commenters noted problems with the specific language, including the fact that many 

of the QC checks do not apply to common parameters (e.g., MDLs cannot be calculated for pH or BOD, 

and surrogates and internal standards have no counterparts in microbiological methods). Other 

commenters expressed concern that the new language was either duplicative or contradicted language in 

existing approved methods, or presented conflicts with various state or national accreditation programs. 

Still other commenters objected to the perceived costs of meeting the letter of this new language and 

suggested that the QC checks simply will not occur, regardless of the language. A few commenters 

suggested improved language should EPA decide to proceed with this new section. One commenter 

stated that the section was not needed, since EPA should not be approving methods at 40 CFR 136 that do 

not already contain appropriate QC checks. One commenter asked about the application of these 

requirements when there are difficult matrices that interfere with results. Several commenters requested 

definitions of terms. One commenter suggested that training was needed. One commenter wanted to 

know what the minimum acceptance criteria were for these new requirements and one commenter asked 

for references for each requirement. Two commenters informed that the TNI standards would be replaced 

in July 2011. 

Response: With respect to the issue of applicability of the QC elements, EPA agrees with commenters 

who stated that some quality control (QC) elements listed in Part 136.7 may not apply to common 

parameters (e.g., matrix spike and matrix spike duplicate does not apply to pH measurements). For any of 

the Part 136 methods that include (or reference) appropriate QC elements for these parameters, these new 

QA/QC requirements are not applicable. As a result, in today’s final rule, EPA has added introductory 

language in Part 136.7 to clarify how laboratories should comply with this new requirement when one or 

more of the twelve essential quality control elements is not applicable to a method. See Section IV.C of 

the preamble and Section 136.7 of the final rule for details. 

In response to the comment that the language is either duplicative or contradicted in existing approved 

methods or accreditation programs, EPA has added a new section at Part 136.7 to address concerns that 

certain approved methods do not contain QA/QC procedures. If an approved method incorporates these 

QA/QC procedures (as applicable to that method), the laboratory should simply follow the method as 

written. This new requirement does not apply in those instances. Standard Methods incorporated new QC 

requirements starting with the 20th edition of Standard Methods similar to the QC requirements included 

in EPA methods for the last two decades. Thus, most Standard Methods that are also approved methods in 

Part 136 already contain QA/QC requirements, as applicable. Similarly, EPA does not anticipate conflicts 

with laboratory accreditation programs because these programs generally follow the QC requirements in 

the method or otherwise specified in regulatory programs. The purpose of this new section is to ensure 

that analyses conducted for compliance monitoring with CWA regulatory programs contain appropriate 
2010 Methods Update Rule Response to Comments 124 March 2012 

QA/QC and the Agency’s view is that this is already occurring in most laboratories (with very few 

exceptions). This new requirement is added to clarify that laboratories must implement proper QA/QC, as 

needed, for all CWA compliance related analyses to provide quality data that will withstand regulatory 

and legal challenges. EPA has added regulatory language to 136.7 that provides several options to comply 

with the QA/QC requirements if these requirements are lacking in the approved method. 

In response to the comment that this new requirement will be costly, proper QA/QC is essential for 

obtaining results of known and acceptable quality. In the long run, it could be much more costly to use 

data which lacks proper QC in demonstrating or enforcing discharge requirements. In the short run, 

laboratories would only incur costs associated with this new requirement when the method lacks QA/QC 

and when they have not included QA/QC as part of their SOPs. EPA estimates that this would not have a 

significant impact on laboratories because the vast majority of Part 136 methods already include or 

reference QA/QC requirements. Further, most laboratories already implement the QC checks prescribed 

by the newer methods and are already documenting these QC checks in the laboratory SOPs. Some of the 

QC checks are a one time or infrequent expense (e.g., demonstration of capability and determination of a 

method detection limit), while other checks are routine (e.g., running a method blank). Typically, 

laboratories include QC as part of the overall analyses costs, and these costs generally add 10-20% to the 

analyses cost initially for an analyst demonstration of capability, and less (5-10%) after the initial cost for 

routine QC (e.g., running a blank with every batch of samples). For a typical analysis of a metal using 

furnace atomic absorption, at a cost of $35-50 per sample, the QC costs would be typically 5-10% of the 

total costs, and are generally included in the laboratory pricing schedule. Thus, EPA expects that any 

costs associated with this aspect of today’s rule will be minimal and limited to a few older methods that 

some laboratories may still elect to use rather than the many other methods that contain QA/QC 

requirements. EPA considers these QC checks to be an essential part of an overall approach to producing 

data of known quality and defensibility where applicable to the methods used to measure pollutants for 

compliance monitoring purposes and ignoring these QC checks, as a comment suggested, is in violation 

of Part 136 and Part 122. Subpart C, Part 122.41 (Permit Conditions) in 122.41(e) states that the permittee 

“shall at all times properly operate and maintain all facilities and systems of treatment and 

control...Proper operation and maintenance also includes adequate laboratory controls and appropriate 

quality assurance procedures...” In most cases, these procedures are already a part of the quality control 

practices of most laboratories and will not create an additional burden. However, in codifying QC 

requirements, EPA provides clarification that these procedures are mandatory, as applicable and not 

merely optional. 

Regarding the comment on the application of these requirements when there are difficult matrices that 

interfere with results, the laboratory must make every effort to address potential interferences but it does 

not relieve the laboratory of conducting proper QA/QC procedures. 

With regard to the request for definitions of terms, EPA refers laboratories to appropriate QA/QC sections 

of EPA methods that contain such procedures, voluntary consensus standards organizations such as 

Standard Methods and ASTM, and other relevant sources such as the 2009 TNI Standard, Volume 1: 

Management and Technical Requirements for Laboratories Performing Environmental Analysis. 

Regarding the comment suggested that training was needed, EPA agrees that laboratories must provide 

adequate training to analysts on the analytical procedures as well as the relevant QA/QC procedures. This 

type of training should occur on an on-going and as-needed basis irrespective of this new requirement. 

The minimum acceptance criteria for these new requirements are described in the appropriate EPA 

method for that parameter or in any other Part 136-approved method. 

With regard to the references for each requirement, EPA refers laboratories to the same sources described 

above for definition of terms. 
2010 Methods Update Rule Response to Comments 125 March 2012 

Lastly, regarding the comment that the TNI standards would be replaced in July 2011, EPA is aware that 

the new TNI standards are now available, as referenced above. 

Original Comment Text: 

The following commenters had the same (following) comment regarding each of the 12 proposed 

mandated requirements. 

Comment 120.1 David N. Speis, Environmental Laboratory Advisory Board (ELAB) 

Comment 125.1 John H. Phillips, Ford Motor Company 

Comment 158. 1 Jerry Parr, The NELAC Institute 

Comment: Section I, Quality Assurance Language at Part 136.7. ELAB commends the Agency on 

proposing minimum QC analyses. ELAB has long supported such minimum requirements as essential for 

improving data quality. ELAB believes, however, that the proposed language at Part 136.7 lacks 

sufficient detail and as written will present many problems, both for laboratories and laboratory auditors. 

The NELAC Institute (TNI) has a consensus standard, Management and Technical Requirements for 

Laboratories Performing Environmental Analyses, that represents the best professional practice in the 

industry, contains sufficient detail for laboratories and laboratory auditors to clearly understand what is 

required, and defers to QC requirements in mandated methods where such QC requirements exists. Thus, 

the QC requirements published in methods developed by EPA, ASTM International, or Standard Methods 

would apply where such QC requirements exist. Where such requirements do not exist, the TNI standard 

would specify the minimum requirements. The TNI standard is a consensus standard focused on 

environmental analyses that “contains the essential elements required to establish a quality system that 

produces data of known and documented quality.” No other such consensus standard exists; therefore, 

under the National Technology Transfer and Advancement Act, ELAB believes that the Agency should 

defer to the TNI standard as TNI’s standard is not “inconsistent with applicable law or otherwise 

impracticable.” 

The paragraphs below address each of the 12 proposed mandated requirements. 

(1) Demonstration of Capability (DOC) 

ELAB supports the concept of a DOC. As written, however, the language is vague. Is this something the 

laboratory performs one time or annually? Does it apply to the method or to the analyst? What specific 

procedures are required for a DOC? TNI’s standard contains extensive language concerning DOC, 

including what the laboratory must do to demonstrate competence as well as requirements for each 

analyst. TNI’s requirements contain both an initial DOC and an ongoing annual demonstration to 

demonstrate continued proficiency. The TNI standard has detailed instructions for what activities should 

be performed and has appropriate activities for chemistry, microbiology, and radiochemistry laboratories. 

(2) Method Detection Limit (MDL) 

The proposed language at Part 136.7 implies that laboratories would have to perform MDL studies for all 

methods, including methods for parameters such as temperature, pH, BOD, and presence/absence tests for 

microbiological parameters. MDL studies are not appropriate for such parameters. Further, if NPDES 

permit laboratories are not required to report to the MDL (and many are not) why would the laboratory 

need to demonstrate this capability? The TNI standard uses the internationally accepted definitions of 

Limit of Detection (LOD) and Limit of Quantitation (LOQ). Under the TNI standard, if laboratories 

report data to the LOD, they must perform an LOD study and, more importantly, must verify that the 

LOD is appropriate. All laboratories must establish an LOQ and verify acceptable precision and accuracy 

at that concentration. The TNI standard has an exclusion provision for methods and parameters such as 

pH or temperature in cases in which LOD/LOQ studies are inappropriate. The TNI standard also 

addresses the unique situations for other scientific disciplines, such as radiochemistry and whole effluent 

toxicity. 
2010 Methods Update Rule Response to Comments 126 March 2012 

(3) Laboratory Reagent Blank (LRB or method blank) 

ELAB supports requirements for method blanks to be a minimum QC requirement. The proposed 

language, however, does not describe the frequency of such analyses, what constitutes an acceptable 

blank result, and what corrective actions should be performed by the laboratory if unacceptable results are 

observed. The TNI standard contains extensive detailed language describing these activities. 

 

(4) Laboratory Fortified Blank (LFB, spiked blank, or laboratory control sample [LCS]) 

ELAB supports requirements for LCS analyses to be a minimum QC requirement. The proposed 

language, however, does not describe the frequency of such analyses, what constitutes an acceptable 

result, and what corrective actions should be performed by the laboratory if unacceptable results are 

observed. The TNI standard contains extensive detailed language describing these activities. 

(5) Matrix Spike, Matrix Spike Duplicate, or Laboratory Fortified Blank Duplicate for Suspected Difficult 

Matrices 

ELAB supports requirements for such activities as matrix spike and matrix spike duplicates to be a 

minimum QC requirement. The proposed language, however, does not describe the frequency of such 

analyses, what constitutes an acceptable result, and what corrective actions should be performed by the 

laboratory if unacceptable results are observed. The TNI standard contains extensive detailed language 

describing these activities. 

(6) Internal Standards, Surrogate Standards (for organic analysis), or Tracers (for radiochemistry) 

ELAB supports requirements for such activities as internal standards and surrogates to be a minimum QC 

requirement. The proposed language, however, does not describe the frequency of such analyses, what 

constitutes an acceptable result, and what corrective actions should be performed by the laboratory if 

unacceptable results are observed. The TNI standard contains extensive detailed language describing 

these activities. 

(7) Calibration (initial and continuing) and Initial and Continuing Performance Solution (also referred to 

as initial calibration verification [ICV] and continuing calibration verification [CCV]) 

ELAB supports requirements for calibration a minimum QC requirement. The proposed language, 

however, does not describe the frequency of such analyses, what constitutes an acceptable result, and 

what corrective actions should be performed by the laboratory if unacceptable results are observed. The 

proposed language does not address the differences in calibration requirements for analytical instruments 

(those that generate a result) and support equipment (e.g., balances, ovens, water baths). The TNI 

standard contains extensive detailed language describing these activities. 

(8) Control Charts (or other trend analyses of QC results) 

ELAB supports requirements for evaluating QC results to determine the validity of the resulting data. 

(9) Corrective Action (root cause analyses) 

ELAB supports the requirements for corrective action. The TNI standard provides further detail and 

discusses the monitoring to the corrective action to ensure it was implemented and preventative actions. 

(10) QC Acceptance Criteria 

ELAB agrees that QC acceptance criteria are important. The proposed language contains no detail, and 

thus a laboratory could decide their acceptance criteria for LCS is 0–200%, whereas a laboratory auditor 

could require the laboratory to meet arbitrary limits of 90–100%. 

(11) Definitions of a Batch (preparation and analytical) 
2010 Methods Update Rule Response to Comments 127 March 2012 

As written, a laboratory could define a batch as all samples analyzed during a 1-year period and perform 

the required QC checks once per year. TNI has established both sample preparation and analytical batch 

requirements. 

(12) Minimum Frequency for Conducting QC Checks 

ELAB agrees that these minimum QC checks could be performed at some frequency. The proposed 

language does not define the frequency, and thus a laboratory could decide the frequency was once per 

year, or a laboratory auditor could decide to require a laboratory to perform an MDL study daily. The TNI 

standard has clearly defined frequencies for each QC check. Some are daily, some are per batch, and 

some are annually. 

Other QC Requirements 

The 12 items proposed to be added are essential but do not represent the full extent of activities that 

laboratories should be required to perform to demonstrate the technical validity of their results. The 

requirements in TNI’s standard, which are based on the internationally accepted standard ISO/IEC 17025, 

General Requirements for the Competence of Testing and Calibration Laboratories, contain many more 

elements addressing issues such as: 

 Personnel, 

 Accommodation and Environmental Conditions, 

 Method Selection and Method Validation, 

 Measurement Traceability, 

 Collection of Samples, 

 Handling Samples, and 

 Reporting the Results. 

Based on the discussion above, ELAB recommends the Agency replace the current proposed Part 136.7 

with the following: 

Regardless of the publisher, edition, or source of an analytical method approved for CWA compliance 

monitoring, analysts must use suitable QA/QC procedures whether EPA or other method publishers have 

specified these procedures in a specific Part 136 method or referenced these procedures by other means. 

Consequently, EPA expects that an analyst using consensus body methods for reporting under the CWA 

will also comply with the QA/QC requirements listed in the appropriate sections in the consensus body 

compendium. EPA’s approval of use of these voluntary consensus standard body methods indicate that 

any analysis using such methods would also meet the QA/QC requirements prescribed for the particular 

method. Thus, not following the applicable and appropriate QA/QC requirements of the respective 

method means that the analysis would not comply with the requirements in EPA’s NPDES regulations to 

monitor in accordance with the procedures of Part 136 for analysis of pollutants. 

For methods that have insufficient QA/QC requirements, analysts should refer to and follow the 

consensus standards published by The NELAC Institute (cf. Volume 1: Management and Technical 

Requirements for Laboratories Performing Environmental Analyses). 

Other comments: 

Comment 79.1 

Richard Burrows 

TestAmerica Inc. 

Comment: We welcome the requirement for basic QC parameters in general, and the reference to NELAC 

Chapter 5 in particular, but note that the 2003 NELAC standards will be superseded in July 2011. We 

suggest the following modification: 
2010 Methods Update Rule Response to Comments 128 March 2012 

Examples of these sources include the instructions in an equivalent approved EPA method; standards 

published by the National Environmental Laboratory Accreditation Conference (cf. Chapter 5 of the 

compendium published in 2003.); or The NELAC Institute (TNI) NELAP standards adopted in 2009 for 

implementation in 2011. 

Comment: With three partial exceptions we agree with the 12 essential quality assurance checks, and 

believe that requiring these will go a long way towards improving the quality of data from older EPA and 

other methods that do not include rigorous QC requirements. 

Exception 1 is the requirement for internal standards in organics analysis (QC requirement #6). We agree 

that internal standards should be required for GC/MS analysis, but they can be problematical for GC 

analysis with selective or non-selective detectors such as FID, PID and ECD. It is possible to use internal 

standards with methods such as 602, 604, and 608 for some matrices, and certainly they will work well 

with the calibration standards, but there is a substantial risk of interference with the internal standard 

when analyzing complex and dirty matrices. Because of this potential problem, we believe that internal 

standards should be allowed, but not required, for GC analysis (and HPLC analysis when using a UV 

detector). 

Exception 2 relates to the requirement for a method detection limit (MDL). A detection limit 

determination should only be required when results are reported below the quantitation limit. In addition, 

EPA should consider whether determination of a quantitation limit should be an essential Quality Control 

parameter. 

Exception 3 concerns tests for which some of the quality assurance tests are not possible or inappropriate. 

For the most part, these are tests for which spiking standards are not available, such as temperature, or 

pH. We suggest adding a section (c) after Section 137 (b) as follows: 

(c) Quality assurance tests requiring spiking solutions, such as MDL, LFB, matrix spikes, etc., are not 

required for tests where the use of spiking solutions is not possible or inappropriate, such as pH, 

conductivity, flash point, temperature, dissolved or suspended solids, color, odor, dissolved oxygen, 

turbidity, BOD, COD and others. Method blanks are also inappropriate for certain tests, such as 

conductivity, temperature, flash point and pH. 

Comment 81 

Jack Hauskins 

City of Lafayette, TN 

I understand why the EPA wishes us to add these new changes to our labs. This seems, on the surface, to 

be a good thing. Who can argue with needing more quality control? However, someone has failed, as so 

often happens, on the level things like this are decided, to look at reality. There is just so much time you 

can spend confirming the accuracy of every aspect of every test that’s run. Some of the larger 

Wastewater Treatment Plants where they have larger staffs, where one person is assigned to a single test 

procedure, would hardly notice an extra hour of work added to his week. However, at Plants like mine, 

which are more plentiful by far, there are only two of us doing all the work? We do all the Lab for a 

Grade 4 plant which has to run analysis 5 days a week on DO, pH, NH3, CBOD, GGA, E Coli, TSS, 

Phosphorus and Settleable Solids as well as numerous Process Control tests like NO2, NO3, MLSS, 

MLTSS, Sludge SS & TSS, which are not required but have to be done to monitor and make changes in 

the treatment process to stay within permit limits. We must also perform all aspects of maintenance and 

Sludge processing and disposal which means we have to run a rotary press, and haul our own sludge to 

the land fill, which leaves only one at the plant to do it all on that day. 
2010 Methods Update Rule Response to Comments 129 March 2012 

The small municipal WWTPs do not have the budgets or the manpower to continually add extra cost and 

time restraints to an already strained budget and situation. You’re going to regulate us into a corner. You 

think you will get more accurate reporting but the plant will suffer because we won’t have time fix 

anything. Also, once you make Lab work such a complicated task requiring ever higher educated 

individuals to perform them you will loose people and no one in their right mind will apply. Look at who 

small towns hire and what they pay. Garbage men on average make more than grade 4 operators in most 

towns. What is the incentive? This kind of regulation will do one thing really well. It will cause less 

people to desire work at a Sewer Plant. What other City employee has to face the threat of being led away 

in handcuffs by federal marshals every day? Not one! The Small Cities will have to hire additional 

personal or subcontract all Lab work which won’t work in every where. Someone has to take the test 

results and adjust the plant based on the results. Who’s going to do that when it takes a week for the 

results to come back from a contract lab? Nobody! There’s also this push to make all WWTPs meet their 

budgets. How can we do that when you are going force us to increase our lab budget 400% and possibility 

have to hire another person? This is one of those,” Looks good on paper.” 

Comment 82 

LeeAnna Hutchings 

Great Salt Bay Sanitary District Damariscotta, ME 

I think that this might be an unjustified waste of resources both from a cost and a time perspective based 

on the likelihood that these additional burdens will likely change significantly the output of data to justify 

this expense. 

Comment 88.1 

Susan D. Hill 

Wisconsin State Laboratory of Hygiene 

Section 136.7, Quality assurance and quality control—Our lab is already NELAC accredited and certified 

by the state of Wisconsin under NR 149, “Laboratory Certification and Registration.” Both of these 

sources, as well as the approved methods, specify required quality control checks for analytical runs. It 

would be cumbersome, unnecessary, and redundant to have to cite 136.7 requirements. In addition, some 

of these requirements (e.g. matrix spikes, internal standards) are often not applicable to certain analyses, 

or they conflict with existing rules. Section 136.7 does not contain language that is in the summary (p. 

58036, section I) that explains how a laboratory can include in its quality system rationale to explain why 

these controls are inappropriate for a specific analytical method; we ask that this language be incorporated 

into 136.7. 

Comment 91.1 

Andrea Rex 

Massachusetts Water Resources Authority 

Having proper QA/QC procedures is important to achieving a high quality laboratory operation and EPA 

has enumerated 12 essential QC elements. This section should not include “Quality Assurance” in its title, 

because it doesn’t include QA elements. The impact of the addition of this section is unclear. For 

wastewater laboratories holding state certification this is nothing new. But for uncertified laboratories at 

wastewater facilities this could result in a major effort to adopt all of these QC procedures and write them 

into the laboratory’s documentation. This section would require that if any of the 12 essential elements 

are not included in a laboratory’s procedure then the SOP must specifically include the rationale for not 

including an element. This seems excessive. 

Comment 92 

Lee Wolf 
2010 Methods Update Rule Response to Comments 130 March 2012 

Columbia Analytical Services, Inc. 

Item 8 lists “Control charts (or other trend analyses of quality control results)” as a quality control check 

that must be clearly documented in the written method along with a performance specification or 

description. 

This line item should be removed because the section is addressing essential QC for the specific analysis 

and batch of samples. Control charts are not commonly used in environmental analysis as a control 

metric; that is, the acceptance or rejection of data is not based on trends in control charts. The use of 

control charts is a process, not a control parameter. 

Also, the section states that for each of the 12 QC elements there must be a performance specification but 

doesn’t give any indication as to what that may be for control charts. The requirement is rather 

ambiguous. Performance specifications are given within the analytical methods and the other QC 

elements. Again, I suggest that this be removed. 

Comment 93 

David Howell 

City of Tampa 

Specifically section 40 CFR 136.7 should be removed from the proposed rule. This section is redundant 

and thus unnecessary given that analytical method quality assurance and quality control (hereinafter 

"QA/QC") are already effectively specified through other regulatory accepted sources. 

QA/QC requirements already originate from the analytical methods themselves, quality assurance 

sections applicable to the analytical methods as issued by voluntary consensus standards bodies, NELAC 

standards where required by state regulators, and QA/QC regulations issued by state regulatory agencies. 

Section 136.7 will also constitute a burden on laboratories which must revise numerous SOPs to address 

QA/QC checks which are not relevant (ex. internal standards, surrogate standards or tracers)to the method 

but require a documented rationale for their absence from the method SOP under section 136.7. Other 

similar unproductive costs will also be incurred under this section. 

QA/QC requirements are already being satisfactorily handled through the aforementioned sources. 

Section 136.7 offers no benefit, creates unnecessary compliance costs, and represents a probable future 

source of conflict with the already existing QA/QC standard sources. 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 

Comment: Welcome the requirement for basic QC parameters in general, and the reference to NELAC 

Chapter 5 in particular, but note that the 2003 NELAC standards will be superseded in July 2011. We 

suggest the following modification: 

Examples of these sources include the instructions in an equivalent approved EPA method; standards 

published by the National Environmental Laboratory Accreditation Conference (cf. Chapter 5 of the 

compendium published in 2003.); or The NELAC Institute (TNI) NELAP standards adopted in 2009 for 

implementation in July 2011. 

Section: 136.7 Quality Assurance and Quality Control (a)(5) 

Comment: Matrix spike, matrix spike duplicate, or laboratory fortified blank duplicate (LFBD) for 

suspected difficult matrices: How can a lab conduct LFBD instead of MSD in a batch which contains 

difficult matrices even though this is not recommended by the specific analytical method? Also, certain 
2010 Methods Update Rule Response to Comments 131 March 2012 

matrix interferences can never be fully removed even after cleanup procedures, so does EPA expect a 

laboratory to report test results without flagging them “suspect”? Please clarify. 

Comment: With three partial exceptions we agree with the 12 essential quality assurance checks, and 

believe that requiring these will go a long way towards improving the quality of data from older EPA and 

other methods that do not include rigorous QC requirements. 

- Exception 1 is the requirement for internal standards in organics analysis (QC requirement #6). We 

agree that internal standards should be required for GC/MS analysis, but they can be problematical for 

GC analysis with selective or non‐selective detectors such as FID, PID and ECD. It is possible to use 

internal standards with methods such as 602, 604, and 608 for some matrices, and certainly they will 

work well with the calibration standards, but there is a substantial risk of interference with the internal 

standard when analyzing complex and dirty matrices. Because of this potential problem, we believe that 

internal standards should be allowed, but not required, for GC analysis (and HPLC analysis when using a 

UV detector). 

- Exception 2 relates to the requirement for a method detection limit (MDL). A detection limit 

determination should only be required when results are reported below the quantitation limit. In addition, 

EPA should consider whether determination of a quantitation limit should be an essential Quality Control 

parameter. 

- Exception 3 concerns tests for which some of the quality assurance tests are not possible or 

inappropriate. For the most part, these are tests for which spiking standards are not available, such as 

temperature, or pH. We suggest adding a section (c) after Section 137 (b) as follows: 

(c) Quality assurance tests requiring spiking solutions, such as MDL, LFB, matrix spikes, etc., are not 

required for tests where the use of spiking solutions is not possible or inappropriate, such as pH, 

conductivity, flash point, temperature, dissolved or suspended solids, color, odor, dissolved oxygen, 

turbidity, BOD, COD and others. Method blanks are also inappropriate for certain tests, such as 

conductivity, temperature, flash point and pH. 

Comment 96.1 

Denise Paige 

Tennessee Municipal League (TML) 

Though there are a few good and needed changes proposed, the TML has grave concerns about an 

increase in the regulatory burden, increase in the cost and an increase the level of confusion at the 

operational levels of municipal wastewater treatment. The twelve Quality Control checks are vague and 

need much better clarification so there will not be a federal, state, and local regulatory interpretation 

leading to inconsistent understanding, usage and enforcement. Professional estimates are that the cost of 

implementing the twelve checks will be in the range of a 25-50% increase over the current testing cost. 

There are tests required by other Federal Regulations that this proposed rule "unapproves" making full 

compliance impossible. 

Statutory and Executive Order Review (FR page 58037): TML believes that this rule is a "significant 

regulatory action" and should be reviewed according to the terms of Executive Order 12866. Under letter 

C. Regulatory Flexibility Act, it states that: "I certify that this action will not have a significant economic 

impact on a substantial number of small entities." 

In Tennessee there are only 9 of 346 cities that have the specified populations greater than 50,000. This 

results in about 170 or about 95% of the publically owned wastewater treatment plants that will fit into 
2010 Methods Update Rule Response to Comments 132 March 2012 

the "small entity" classification. Most all of these will experience a significant cost increase because of 

this proposed rule. 

Though most plants perform a degree of laboratory Quality Assurance/Quality Control, to fully comply 

with the proposed twelve Quality Control Checks (page 58071) will require an increase in laboratory time 

and cost in the range or 25-50%. Even at the low level this is a significant increase in costs to pass along 

to ratepayers especially during a time of recession. There are some small publically owned wastewater 

utilities whose user rates are close to the EPA published maximum of 2% of family income. How will 

local officials explain to citizens who have these very high rates that EPA is mandating additional work 

that will add to the cost of wastewater treatment? If the twelve QC checks are adopted, small utilities will 

respond in three ways. First they may lie about it. Second they may attempt to comply by adding the 

twelve QC checks to the workload of personnel who are already overloaded with additional federally 

mandated requirements beyond the NPDES permit such as, the existing annual DMR-QA checks, CMOM 

with its numerous subprograms, or OSHA regulations and the numerous sub programs. A third way of 

meeting the requirements will be to simply send all possible analyses to a commercial laboratory. This 

will improve the extent of the QC, but may also result in a degradation of wastewater plant effluent 

quality because plant operators, as they wait two to three weeks for those test results, will be operating 

their plants blind. Though most of the state's small plants produce pristine effluent most of the time, most 

do not have QC programs to the extent that this proposed rule will require. It appears that EPA may be far 

out of touch with the real world of small plant operation, or they value small advances in data quality over 

plant effluent quality. Data quality is important, but the proposed twelve checks will be costly, and they 

add to the already high level of regulatory confusion, and unfortunately are poorly timed. EPA should 

reconsider this part of the proposed rule change. 

Twelve Essential Quality Control Checks (FR page 5S071): Mandating these steps without additional 

clarification and or training will add a significant amount of uncertainty and confusion. First each step 

needs to be clarified by specifying which analyses the step applies. For example does Step 2 and Step 3 

(the LRB and the LFB) apply to the dissolved oxygen, residue-settleable, and e-coli test? Does Step 5, the 

matrix spike, apply to BOD testing? Federal and state regulators already give inconsistent answers to 

these questions on these subjects, this rule will add geometrically to that confusion. 

The terminology used in the twelve checks presents problems for many of the persons who will actually 

be doing the testing. Though most terms and abbreviations are taken from Standard. Methods, even the 

regulators don't use them. They use a different QA vocabulary. This of course adds to the confusion. EPA 

needs to provide training in what each of the twelve checks means for each analyses conducted. Without 

this precise training, local governments and their employees will find themselves under enforcement 

action for actions that may have been beyond their capability. Additionally, checks #S and #9 may be 

frequently used in manufacturing, but these quality assurance items are very unfamiliar to the utility 

industry. EPA needs to provide training in the use of control charts and root cause analyses before 

requiring compliance with such rules. 

QC step number one, Demonstration of Capability, is a duplicate of an existing regulatory requirement. 

Currently all major facilities and many minor facilities, annually perform the Discharge Monitoring 

Report-Quality Assurance (DMR-QA) test. Isn't this annual test process a demonstration of capability? If 

it is, the new rule is duplicating an existing requirement. If it is not, the proposed rule should eliminate the 

annual DMR-QA program in favor of the new requirement. 

The implementation of these twelve checks may have unintended consequences. Many small wastewater 

plants will simply opt not to participate and send all testing to their favorite commercial lab. This action 

will provide EPA with test data that has clearly documented QC checks, but will also result in wastewater 

plants being operated blind because of the two to three week delay in receiving effluent test data. As 

described above, this situation appears to show that EPA values data quality over effluent quality. 
2010 Methods Update Rule Response to Comments 133 March 2012 

Summary and Recommendations: The technical deficiencies of this proposed rule can be easily corrected. 

A modification of 40 CFR 503 and the elimination of the current DMR-QA program can be included in 

this proposed change to 40 CFR 136. The addition of twelve Quality Control checks on the other hand 

should be eliminated from this proposed rule change. Implementation of these requirements should 

instead be through a phased in approach over several years with significant training to assure that federal 

and state regulators and the NPDES permit holders fully understand what is needed and how to 

implement the QC checks. 

Comment 97 

Dewayne Culpepper 

Tennessee Association of Utility Districts (TAUD) 

This EPA docket proposes the addition of § 136.7 Quality Assurance and Quality Control, Twelve 

essential Quality Control Checks to 40 CFR Part 136 as follows and referred to in this comment. 

 § 136.7 Quality assurance and quality control. 

(Note from EPA: The list of 12 items from the Federal Register notice is not included here.) 

(b) These twelve quality control checks must be clearly documented in the written method along with a 

performance specification or description for each of the twelve quality control checks. 

 

This section is of particular interest to Public Owned Treatment Works (POTW) in Tennessee. These 

twelve checks will have a significant impact to smaller POTW’s in the following ways: 

 1) Financial. Section III, C, states that the economic impact will not be significant, and Section III, D 

states that the changes make “no regulatory requirement that might significantly or uniquely affect small 

government,” which TAUD has its concerns. To meet parts 136.7 a (1), (2), (4), (5), (7) continuing 

calibration, will have financial impacts as follows: 

 a) Many treatment works will be faced with increased laboratory costs for supplies and 

equipment. POTW’s will have an estimated 20-40% increase in laboratory expenses. If additional staff is 

needed it will result in significant additional expenses. Systems will have to weigh their options to either 

perform their analysis in house or use a contract laboratory. If they choose to use contract laboratories to 

run laboratory analysis, systems will lose the real time operational process adjustments due to the lack of 

on- site analysis. 

 

2) Personnel and Time Management 

a) Many POTW’s will need to increase staff. An estimated eighty percent of wastewater systems in 

Tennessee are considered small systems and have limited number of staff to perform a variety of daily 

tasks not only in the laboratory but in other areas in the water and wastewater system. These twelve 

quality control checks will require a significant increase in the time it takes to perform daily laboratory 

tests. Systems that cannot afford to hire another staff member to perform these checks will sacrifice time 

spent in other areas such as troubleshooting, research & education. Many of these small systems will need 

to employ another staff person which will have an additional financial impact. Many of these small 

systems will need to employ another staff person which will have an additional financial impact. 

Our Membership understands the importance to perform analysis correctly with certain checks and 

balances to insure reliable data to protect the public health and environment, which is in all parties’ best 

interest. To meet parts 136.7 a (2), (4), (5), (7), will have impacts on small wastewater systems. Our 

membership is required to use EPA approved methods and these methods have gone through an EPA 

approval process to be used to perform analysis and report the data generated to the EPA. We think that 
2010 Methods Update Rule Response to Comments 134 March 2012 

some of these additional requirements to be performed repeatedly to prove these EPA approved methods 

seem unnecessary and economically wasteful. 

Thereby, TAUD requests that EPA takes into account how the, “Guidelines Establishing Test Procedures 

for the Analysis of Pollutants Under the Clean Water Act; Analysis and Sampling Procedures, Proposed 

Rule” will impact POTW’s in the aforementioned manners. 

Comment 101.1 

New York State Department of Environmental Conservation 

Item I. NYSDEC strongly endorses the addition of essential quality assurance and quality control 

(QA/QC) at Part 136.7. NYSDEC believes the data quality in the SPDES program will improve if and 

when QA/QC procedures can be standardized across the diverse series of approved methods. Having 

standardized QA/QC will also prevent permittees and permittee laboratories from seeking out the method 

with the least rigorous QC requirements when choosing between two approved methods that use identical 

technology and techniques. 

Comment 105 

Sandra Dudley 

Water Authority of Dickson County 

The twelve essential quality control checks referenced on p. 58071 as a new subpart, 40 CFR 136.7, are 

undefined in either 40 CFR 136 or the proposed rule. Different organizations and regulations have 

different definitions for key terms. To make a valid, meaningful estimate of the additional time and 

resources required to comply with the twelve checks, it is critical to know the specific definition of the 

various terms used in the proposed rule. WADC respectfully requests that definitions be provided in an 

updated proposed rule to allow further commenting before finalization. 

 

Comment 106.1 

Charles Boepple 

Upper Occoquan Service Authority 

Comment I: This requirement is redundant. Essential, applicable quality control measures are already 

described in various method references as well as by various state and national laboratory accreditation I 

certification regulations. 

Comment 2: Many of these steps are not (?)-applicable 10 numerous common test methods (e.g. spiking 

pH, Coliforms or toxicity). The requirement that "'(b) These twelve quality control checks must be clearly 

documented in the written method...,. when a step is not applicable is unnecessary. 

Comment 3: The essential steps are too vague to be meaningful. Again, applicable and appropriate QC 

measures are described in detail for individual methods. 

Comment 4: These steps are not applicable or appropriate for field measurements. For example, a 

technician cannot be expected to input values into a control chart in the field (often under adverse weather 

conditions) before deciding to proceed with measurements. 

Comment 6: Ballooned, lengthy SOPs become an impediment, not a benefit for bench top analysts. 

Comment 7: (8) Control charts (or other trend analyses e.g. quality control results). What are these "other 

trend analyses"? The statement is vague. 
2010 Methods Update Rule Response to Comments 135 March 2012 

Recommendation: Remove section 136.7 Quality Assurance and Quality Control. 

Comment 107.1 

Patsy Root 

IDEXX Laboratories 

Page 58071: Propose that EPA add clear definitions to the proposed twelve essential quality control 

checks referenced here; since multiple accreditation bodies and any number of QA/QC officers will 

define these differently 

Again, we applaud EPA’s initiative to continually improve water safety. We appreciate the opportunity to 

be part of this process and hope to continue to partner with the EPA, and other stakeholders, in the 

protection of public health and our environment. 

Comment 109.1 

Andre Brousseau 

Maine Wastewater Control Association 

EPA states, in Part II Section I of the proposal, that if insufficient quality control and assurance 

requirements are available for an approved method, permittees and their laboratories "could" refer to QC 

in other published sources. EPA is proposing a Part 136.7 for Quality Assurance Control that lists twelve 

essential quality control checks. 

 

Does EPA propose to require that all twelve controls be established and performed for the following 

parameters found in NPDES permits: flow, pH, temperature, dissolved oxygen, biochemical oxygen 

demand, non-filterable solids (TSS), dissolved solids, total residual chlorine, turbidity, fecal coliform, and 

e. coli? 

The Biochemical Oxygen Demand approved method (reference Standard Methods 18th edition, 5210 B. 6 

"Precision and Bias") states that, "There is no measurement for establishing bias of the BOD procedure. 

The glucose-glutamic acid check prescribed in , 4c is intended to be a reference point for evaluation of 

dilution water quality, seed effectiveness, and analytical technique." Does EPA propose to require the 

analyst, permittee or laboratory to look further than this and establish additional QA/QC for the method, 

even when this conflicts with the method's prescribed QA/QC? 

The determination of an MDL for BOD seems contrary to the method's requirement for a dissolved 

oxygen uptake of at least 2.0 mg/L and residual dissolved oxygen of 1.0 mg/L. Does EPA find that there 

must be an MDL for biochemical oxygen demand? If so, as a very common test required in Clean Water 

Act permits, EPA should direct permittees as to where the proper procedure for establishing a MDL for 

BOD is found, so that this can be done consistently on a national basis. 

Comment 110.1 

Laurie Curra 

Texas Commission on Environmental Quality 

Minimum Quality Control Requirements: The TCEQ supports the standardization of terminology. The 

use of multiple terms to describe method detection limit continues to cause confusion among the data 

users making decisions regarding health and environmental impacts. 

Comment 112.1 

Colin Elliott 

King County Environmental Lab 
2010 Methods Update Rule Response to Comments 136 March 2012 

Comment: We agree that documenting all “essential QC requirements” is a good idea. However, it 

should be allowed for some requirements to be described in a central document (lab-wide QA Manual), 

otherwise this task would be redundant to include in 150 or so SOPs. With limited resources, this task 

should be as streamlined as possible. Another example to streamline this process would be to address 

how SOPs should address “essential QC” that does not apply (i.e. pH). pH does not have an MDL, LRB, 

LFB, MS, MSD, surrogate, ICV or CCV. Please also describe “corrective action” further. It would be 

very difficult to describe/predict all potential issues with data sets and the associated corrective action. 

Corrective actions can vary depending on project requirements, action limits, sample matrix etc. 

Comment 113.1 

Susan E. Butts 

South Carolina Department of Health and Environmental Control Office of Environmental Laboratory 

Certification 

Section 136.7 discusses Twelve Essential QC checks. These checks need to be defined or reference where 

they are defined. The memo released by Richard Redding dated May 7, 2009 outlines the criteria and 

goes into more detail. The language in this memo should be included in the rule. Each item in the list 

needs to be defined and/or clarified. For instance, number 7 in the original memo stated "Calibration 

(Initial and Continuing)". Section 136.7 goes on to mention an ICV. ICV needs to be defined since in 

some instances this refers to a second source standard. A second source standard is not included in most 

methods currently approved for wastewater. Number 6 under this section mentions internal standards and 

surrogates. Clarification is needed for this item. Some GC methods recommend but do not require an 

internal standard and/or surrogate. By adding this item in the list of QC checks, does this supersede the 

approved method and require internal standards and surrogates for all organic methods approved under 40 

CFR Part 136? 

A list of methods needs to be provided to which the QC checks would apply. For instance, the checks 

should not apply to pH or other simple inorganic methods. They should not apply to microbiological 

parameters. A list of methods and/or technologies will provide consistency in applying these QC checks. 

Clarification is also needed on whether these QC checks are designed for the laboratories or the method 

developers. 

Comment 116.1 

Wendy Harding and Mala Burton 

Joint Virginia Water Environment Association and Virginia American Water Works Association 

Comment 1: This requirement is redundant. Essential, applicable quality control measures are already 

described in the individual methods references, as well as state and federal lab accreditation / certification 

regulations. 

Comment 2: Many of these steps are non-applicable to numerous common test methods (e.g. spiking pH, 

Coliforms or toxicity). The requirement that “(b) These twelve quality control checks must be clearly 

documented in the written method...” when a step is not applicable is unnecessary. 

Comment 3: The essential steps are too vague to be meaningful. Again, applicable and appropriate QC 

measures are described in detail for individual methods. 

Comment 4: This should not to apply to field measurements and should be clearly stated as such. 

Comment 5: The MDL concept is antiquated in the fact that most laboratories assess at quantification 

levels (QL). 
2010 Methods Update Rule Response to Comments 137 March 2012 

Comment 6: Complicated, lengthy SOPs become an impediment rather than a benefit for bench top 

analysts. 

Comment 7: (8) “Control charts (or other trend analyses of quality control results)”. What are these 

“other trend analyses”? 

Recommendation: Eliminate section 136.7 Quality Assurance and Quality Control. 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

Section II.I We do not support the inclusion of this new section and language to 40 CFR Part 136, for the 

following reasons: 

(A) This language poses a problem for enforcement. Certification programs, such as ours, require 

laboratories to adhere to the requirements in their rules. Permitting authorities have their own rules which 

are incorporated into discharge permits. The proposal represents a third tier of regulatory requirements 

which either duplicate or conflict with existing systems. 

(B) The rule proposal appears to represent an abbreviated version of the drinking water program’s 

specific requirements which are outlined in a document titled, “Manual for the Certification of Drinking 

Water Laboratories”. If it is the agency’s intent to develop a similar set of certification requirements for 

waste water testing laboratories, we encourage the development of a separate document which is 

promulgated outside of 40 CFR Part 136. 

(C) The proposal lacks clarity of requirements. Clarification of the rule’s intent is discussed in the rule 

summary, yet this critical information is not included as part of the proposed rule language. If after the 

comment period, the agency decides to continue with its proposal, we respectfully suggest the agency 

incorporate the following language [from p. 58036] of the proposed rule] in 40 CFR Part 136.7 (a): “In 

addition to and regardless of the source of the laboratory’s QA and QC instructions, ...[the following] 

twelve essential quality control checks... must be in the laboratory’s documented quality system unless a 

written rationale is provided to explain why these controls are inappropriate for a specific analytical 

method or application. This written rationale will be included in the laboratory’s Standard Operating 

Procedure (SOP) for each method to which specific controls do not apply (e.g., internal standards, 

surrogate standards or tracers do not apply to analyses of inorganic parameters) as well as being included 

with the monitoring data produced using each method. “ 

 

(D) There are discrepancies between required Quality Control samples in the “12 essential elements” and 

approved testing methods. For example, most Standard Methods procedures require the analysis of 

sample replicates, which are not included as part of the “12 essential elements”. 

(E) As written, the proposal suggests that all elements are required for all tests, some of which are 

impractical. For example, the requirement for “Laboratory Fortified Blanks (LFB)” or Laboratory Control 

Samples (LCS). Are these appropriate for an analysis such as Total Suspended Solids (TSS)? Certainly it 

is feasible to create such a sample, but this is not standard practice. 

(F) The proposal includes control charts —or other trend analysis— as an essential element. We believe 

that, while control charts can serve as valuable analytical tools, their use should not be mandated. 

Furthermore, many existing methods require control charts to be updated at frequencies as often as every 

5 QC samples. For many large labs, this means at least daily, or more often. That represents a significant 

workload for minimal return in terms of data quality. 
2010 Methods Update Rule Response to Comments 138 March 2012 

(G) The proposal includes as an essential element, “(5) Matrix spike, matrix spike duplicate, or laboratory 

fortified blank duplicate (LFBD) for suspected difficult matrices.” What guidance will be issued 

regarding what constitutes a “suspected difficult matrix”? In addition, each of the three named QC 

samples provides very different information regarding data quality for an associated batch of samples, yet 

the use of the conjunction “or” implies that only one of them is mandatory. As a general practice, matrix 

spikes are something the industry is moving away from as a laboratory quality control measure, because 

the information they provide is reflective only of the specific sample spiked. 

(H) The proposed language for 40 CFR Part 136.7(b), “These twelve quality control checks must be 

clearly documented in the written method along with a performance specification or description for each 

of the twelve quality control checks” indicates that labs must provide either a performance specification 

(acceptance criteria?) or a description of each check. Not only should performance specifications be 

required, but they should be standardized, rather than allowing labs to simply establish them on their own. 

As written, the proposal would allow a lab to indicate that they use matrix spikes with acceptance criteria 

of 0 to 200% recovery, criteria which provide no utility in evaluating data quality. This is another reason 

why these requirements are best left up to certification programs, or, to permitting authorities for states 

without such a program. 

Comment 124.1 

Thomas Tourje 

Augusta County Service Authority 

Comment: The inclusion of the 12 steps of quality control, or a written rational for exclusion, into each 

and every SOP would be extremely onerous. Dictating this type of extensive treatment to even simple 

test procedures that will have little benefit to the accuracy of the results will be counterproductive, 

focusing more of operator and analyst time on documenting / control charting / etc. rather than the actual 

running of the test. Ballooned SOPs become an impediment, not a benefit for bench top analysts. Test 

methods that do require more extensive quality control should be required within that test method, 

without subjecting all test methods to what amounts to overkill. SOPs currently highlight required quality 

control parameters that are run and evaluated each and every run. The quality program as written in the 

lab quality manual should allow for the flexibility to bring to bear more advanced quality control 

measures e.g. control charts when basic QC measures highlight an issue. To dictate that all labs control 

chart all of their QC parameters on all the test methods that they run is inefficient and impractical, and 

will lead to less bench top analyst time being spent on actually running the tests. To effectively manage a 

lab, we need the tools to address quality problems, if and when they arise, without dictating that all 

quality tools be required on all tests all the time. E.g. A lab that has successfully run BOD for years with 

good PTs, blanks, seed control and GGA results should not be expected to publish ongoing control charts. 

The same lab, should it run into an issue with its BOD QC parameters, could reasonably be expected to 

utilize control charting in the process of investigating the problem and determining the proper corrective 

action. Once long term stability of the QC parameters was established, the control charting could be 

suspended, allowing the lab to focus on other more pressing QC issues on other test methods. 

Recommendation: Remove the proposed new quality assurance and quality control language at 

40CFR136.7. Instead, move towards defined QC requirements within each method where appropriate. 

Comment: An exemption from including the 12 steps of quality control in SOPs for all field parameters 

analyzed within 15 minutes from sampling is needed and warranted. Field operators running simple test 

procedures which require immediate analysis (within 15 minutes) do so using approved test methods 

following manufacturer’s instructions. Training documentation verifying Initial Demonstration of 

Capability, equipment calibration verification and individual method verifications are currently being 

done. To require field operators to carry around multi page SOPs filled with voluminous descriptions and 

exclusions is without merit. To require a field operator to be plotting control charts as they are running 

pH, DO or TRC check under adverse weather conditions is not practical. 
2010 Methods Update Rule Response to Comments 139 March 2012 

Recommendation: Exempt all simple test procedures requiring immediate analysis run in the field from 

the proposed requirement for 12 steps of quality control in SOPs. 

Comment 125.1 

John H. Phillips 

Ford Motor Company 

The paragraphs below address each of the 12 proposed mandated requirements. 

(2) Method Detection Limit (MDL) 

The EPA should not continue to perpetuate the use of the current MDL procedure, which is known to 

have numerous flaws and is not scientifically defensible. The Office of Water commissions a Federal 

Advisory Committee on Detection and Quantitation (FACDQ) and has received many sound 

recommendations from the FACDQ, which should be implemented as quickly as possible. The advisory 

committee recommendations not only included the MDL, but also the ML and the use of Data Quality 

Objectives (DQOs). Another example of how the current MDL and ML are unsuitable for use in 40 CFR, 

Part 136 was the recently proposed Sufficiently Sensitive Methods rule, which might have been 

supported, except for the unresolved issues surrounding the MDL, ML and DQOs. 

Comment 126.1 

Sterling Pierce 

Maine Department of Environmental Protection 

Maine DEP is a delegated State and currently issues discharge permits under the Maine Pollutant 

Discharge Elimination System. These permits carry requirements for the licensee’s to conduct certain 

analyses to demonstrate compliance with applicable licensed limits. These facilities are typically required 

to test for a variety of parameters including; total suspended solids, biochemical oxygen demand, 

chemical oxygen demand, pH, chlorine residual, fecal coliform, E. coli, conductivity, color, temperature, 

and dissolved oxygen. Currently, publically owned treatment works (POTWs) may perform these tests 

without obtaining certification under the Maine Comprehensive Environmental Laboratory Certification 

Rules. 

Maine DEP has oversight of the operation of these POTWs and the associated laboratories. The operators 

are required by the facility license to analyze all samples using methods in 40 CFR 136.3 as approved by 

EPA. Maine DEP also implements the annual discharge monitoring report-quality assurance (DMR-QA) 

study, which includes the major facilities and some of the minor facilities. 

The operators of POTWs in Maine have permission to conduct the following laboratory analyses without 

obtaining certification from the Maine Comprehensive Environmental Laboratory Certification Rules: 

Total Suspended Solids, Biochemical Oxygen Demand, Chemical Oxygen Demand, pH, Total Residual 

Chlorine, Fecal Coliform, E. coli, Conductivity, Color, Temperature, and Dissolved Oxygen. Is EPA 

proposing to require that controls be established and performed for all twelve of these parameters? 

If this is EPA’s intention to implement all controls for all 12 parameters, then this may drive the decision 

making of some of the operations staff from around the State to discontinue testing for these parameters at 

the treatment facility and seek out commercial laboratories to provide this service. Initially, there may not 

seem to be much of an impact from this change in approach, but eventually you will have operators that 

do not have the knowledge base to know how to perform these tests. This could leads to an inability to 

evaluate the tests that are being conducted by commercial laboratories, which is critical to the integrity of 

the data that is passed through the license holders to the regulators. So the desire to have better quality 

data, could potentially lead to the unintended consequence of data that doesn’t receive as much scrutiny 

as before. 
2010 Methods Update Rule Response to Comments 140 March 2012 

Comment 130.1 

Heather L. Beard 

Richland County Utilities 

We are concerned about the economical and practical aspects of implementing all twelve (12) quality 

control checks outlined in section 136.7 for each parameter the lab currently holds certification. We 

believe that most laboratories already implement applicable quality control checks for each method they 

are certified to run. Requiring labs to implement all twelve checks for all parameters, or provide a clear 

explanation for why all checks are not required for a certain method, creates undue burdens for smaller 

laboratories with limited budgets and staff. As an alternative, we propose that the laboratories be given 

the discretion to choose appropriate quality control checks for each method, following proper method 

protocol and procedures. We feel that the publishing authority has established adequate quality control 

protocol in the method as evidenced by the fact that it has been published in the Federal Register. Having 

to give detailed explanations for exclusion of inappropriate quality control measures serves no purpose in 

improving the quality of the data produced by the laboratory. 

Comment 132.1 

Paula Hogg 

Hampton Roads Sanitation District 

Comment: This requirement to address each of these items in SOPs whether or not they are relevant to 

the specific method is over burdensome for laboratories. 

Recommendation: HRSD recommends EPA provide clear definitions and applicability to methods for 

each of the twelve elements to avoid misinterpretation by regulatory agencies, data users and laboratories. 

HRSD also recommends laboratories only clearly define relevant elements in their quality system 

documentation and SOPs. SOPs should only include procedures and protocols that are relevant to the 

method to which they are written. 

For example: An SOP for microbiology should not include any information regarding Surrogates or 

internal standards, because these elements are not appropriate to the method. 

It is not clear if EPA intends for these elements to be included in the analytical methods prepared by 

consensus groups and promulgated through 40 CFR Part 136, or if it is intended for laboratories to 

include these elements in their SOPs. 

Recommendation: If the intent is for laboratories to document these elements in quality system 

documentation and/or SOPs, the language should be changed as follows: "These twelve quality control 

checks must be clearly defined in the laboratories quality system, including a written rationale for why 

any of these controls are inappropriate for specific methodologies. Each SOP or method must include the 

appropriate quality control elements along with performance specifications for each." 

Comment 133.1 

Terri Grimes 

Pinellas County Utility Laboratories 

I think this proposed section unnecessarily duplicates requirements already in existence which creates an 

undue burden on laboratories, especially small labs. 

This addition to 40 CFR 136 seems simple enough on the surface, but adding this requirement with 

QA/QC checks creates a couple of problems for labs. Certified labs are already using voluntary 
2010 Methods Update Rule Response to Comments 141 March 2012 

consensus standards bodies’ methods for CWA samples. In doing this, labs already comply with the 

QA/QC listed in the method or other part of the respective compendium. In addition, NELAC (soon to be 

TNI) certified labs also must meet similar criteria as listed in the NELAC Standard (2003) (soon to be 

TNI Standard). Keeping this in mind, there are already multiple sources that a lab must be 

knowledgeable of and comply with (EPA, state, NELAC/TNI, methods, etc.) To add another layer of 

redundant requirements in 40 CFR 136 is absolutely unnecessary. The simple, most economical and 

effective answer is to refer to what already exists: the methods and the NELAC/TNI Standard. A lab does 

not need to be a NELAC/TNI certified lab to refer their QA/QC requirements. And labs are already used 

to referencing the methods for specific QC checks. 

Besides the duplication of requirements, another problem with adding this section to 40 CFR 136 is that 

when the other sources (Standard Methods, ASTM, TNI, states. etc.) change their standards, there will be 

a conflict between 40 CFR 136.7 and these sources. It is already difficult enough for labs, especially 

small labs, to keep up with these changes from their current sources without adding to it. 

Lastly, adding this language gives opportunities for auditors to write unreasonable and time-wasting 

deficiencies. While many auditors are reasonable and knowledgeable about the methods used in 

laboratories, some are not. Over the years, since NELAC has been in place, labs have been fixing 

previous deficiencies, and therefore auditors need to come up with new ones. Since some of QA/QC 

checks listed in 136.7 don’t apply to all the methods used by laboratories, labs will be put into a position 

to define each and every of the twelve essential QA/QC checks in every SOP and/or include a rationale as 

to why they aren’t relevant. This is counterproductive. If anyone reviewing the SOP and data doesn’t 

understand why internal standards aren’t used for CBOD, then they should not be auditing labs nor 

reviewing data. Since labs (like businesses nationwide) are cutting costs and personnel, they too are 

struggling to keep up with all the demands placed on them regulatory entities, clients, etc. with less. This 

listing in 40 CFR 136.7 give auditors a ready-made checklist to use without any clarification as to its 

limitations. That is why it is so important to write clear standards/rules/regs. No matter how good the 

intent of the method or regulation writer is, the intent will not be understood by some labs and auditors. 

Please do not add this redundant language to 40 CFR 136. At most, a reference to other sources of this 

information is all that’s needed. 

Comment 151. 1 

Aaren S. Alger 

Pennsylvania Department of Environmental Protection 

The PA-DEP LAP, having mandated by law environmental laboratory accreditation in the water matrix 

(which includes NPDES testing), fully agrees with the concept of mandated QA/QC procedures. The PADEP's LAP commends the USEPA for clarifying the importance of and necessity of QA/QC and 

adherence to specified QC procedures outlined in approved methodology. The PA-DEP LAP requests that 

the USEPA expand the language relating to QA/QC to include frequency and possible minimum 

acceptance criteria for these procedures, where none exist in the approved methods. Currently, the PADEP LAP lists its minimum expectations/requirements in 25 Pa Code, Chapter 252 and believes that the 

USEPA could use this language as a starting point. 

While PA-DEP LAP agrees with the concept of USEPA's proposal for QA/QC, the PA-DEP LAP has 

several concerns with the way this section of the proposed rulemaking is written. Specifically, in the 

"Summary of Proposed Changes, Section I." of the proposed rulemaking, 

• USEPA states, "For methods that have insufficient QA/QC requirements, analysts could refer to 

and follow the QC published in several public sources." This statement would be interpreted by the 

regulated community as a suggestion, due to the use of the word "could," and a regulated entity could 

decide that an absurd QC frequency of once per year or even less frequent is "acceptable." 
2010 Methods Update Rule Response to Comments 142 March 2012 

• USEPA states, "EPA is proposing at 136.7 to specify 12 essential QC checks that must be in the 

laboratory's documented quality system ... This written rational will be included in the laboratory's SOP 

for each method...These 12 essential QC checks must be clearly documented in the written SOP." The 

proposed rulemaking does not include a requirement for a "documented quality system" or written SOP 

for "each" method, nor does the proposed rulemaking define "quality system". 

The PA-DEP LAP believes that a requirement for "(8) Control charts (or other trend analysis of quality 

control results)" is excessive. This requirement would not necessarily be useful to a laboratory/operator 

that does not have procedures in place to improve procedures. By adhering to established QC acceptance 

criteria, a laboratory would be able to demonstrate compliance with QC procedures without the additional 

requirement of control charting/trend analysis. 

Lastly, "Summary of Proposed Changes, Section 0" of the proposed rulemaking states, "EPA has 

determined that this rule contains no regulatory requirements that might significantly or uniquely affect 

small governments." By requiring a laboratory to have additional documentation/SOPs with the 12 

essential QC checks, the USEPA is adding additional requirements for regulators to evaluate while 

determining acceptance of compliance data. This could be considered a regulatory requirement that could 

impact small government that does not have trained laboratory accreditation personnel to evaluate 

QA/QC procedures. PA-DEP LAP fully believes documented polices, procedures, and training are 

essential to quality data, however, by including these requirements in this proposed rulemaking the 

USEPA has added an additional requirement that might not be readily evaluated by a agency that does not 

currently require laboratory accreditation. 

Comment 152.1 

James Matthew 

On Line Environmental Inc (OLE) 

We are concerned about the economical and practical aspects of implementing all twelve (12) quality 

control checks outlined in section 136.7 for each parameter the lab currently holds certification. We 

believe that most laboratories already implement applicable quality control checks for each method they 

are certified to run. Requiring labs to implement all twelve checks for all parameters, or provide a clear 

explanation for why all checks are not required for a certain method, creates undue burdens for smaller 

laboratories with limited budgets and staff. As an alternative, we propose that the laboratories be given 

the discretion to choose appropriate quality control checks for each method, following proper method 

protocol and procedures. We feel that the publishing authority has established adequate quality control 

protocol in the method as evidenced by the fact that it has been published in the Federal Register. Having 

to give detailed explanations for exclusion of inappropriate quality control measures serves no purpose in 

improving the quality of the data produced by the laboratory. 

Comment 154.1 

Sharon Mertens 

Milwaukee Metropolitan Sewerage District 

This section and preamble to the proposed rule references the standards published by NELAC (Ch5, 

2003). This document will be obsolete and no longer applicable after July 1, 2011. We would suggest 

that this language be revised as follows: 

For methods that have insufficient QA/QC requirements, analysts could refer to and follow the QC 

published in several public sources. Examples of these sources include the instructions in an equivalent 

approved EPA method or standards published by The NELAC Institute (cf. Volume 1: Management and 

Technical Requirements for Laboratories Performing Environmental Analyses.) 
2010 Methods Update Rule Response to Comments 143 March 2012 

 EPA’s proposal of minimum quality control (QC) analyses is commendable. These could provide the 

laboratories with consistency in definition and clarity on essential requirements. However, the proposed 

language at Part 136.7 lacks detail and as written, leaves these requirements subject to interpretation by 

labs, data users and auditors. Where specific requirements exist in mandated methods, (e.g., EPA, ASTM 

or Standard Methods), these should apply. However, where such QC requirements do not exist, EPA 

should require that a recognized standard be applied (e.g., The TNI Standard or state specific rules) as the 

specification for the minimum requirements. 

Comment 157.1 

Marlene Moore 

Advanced Systems, Inc 

The twelve items presented in this section are not limited to the quality control checks but are part of a 

management system program. These are the corrective action (9) and definitions of a batch (preparation 

and analytical) (11). 

Documenting the procedure for corrective action and definition of batch as part of each test method is 

unnecessary. If the intent is to ensure that the frequency for quality control be defined in the test method 

for all types of batches then this should be more clearly stated. Also if the intent for corrective action is to 

define how to address QC failures rather than corrective action this must be more clearly stated. 

b) Item (12) frequency for conducting quality control cannot be performed for several of these items such 

as corrective action, batch definition and quality control acceptance criteria. 

c) The quality control performance for methods must be more clearly defined as to the acceptable 

precision and bias for a method. The method performance found in the EPA and other reference methods 

do not always indicate acceptable performance, such as percent recoveries of zero to more than 200%. As 

long as the EPA methods allow for this type of performance, laboratories will argue that this type of 

performance is acceptable. This was acceptable in the 1980’s when technology did not provide for better 

quality. However modern analytical equipment is capable of providing better method performance. EPA 

must adopt a policy across all testing methods that data used for regulatory decision making must be able 

to demonstrate acceptable precision of < 20% RPD and bias of 50 to 150% recovery. If the method 

demonstration does not produce acceptable method performance then the method is not acceptable for 

regulatory monitoring. 

The commenter does recognize that many EPA and other reference methods presented in the tables for 40 

CFR Part 136, 141, etc. do not meet these criteria. It is the commenter’s intent that laboratories must be 

able to demonstrate that the regulated analytes meet the improved criteria rather than the published 

method criteria which was generated using older technology. This requires the laboratory to perform the 

method using improved extraction techniques and not allow for sloppy extraction techniques or certain 

analytes. Where this type of method performance is not demonstrated, then data users must be notified to 

know that less reliable data is generated for the given analyte. 

Please identify that data for compliance must be generated from a technically competent organization that 

operates a management system that is consistent with consensus standards such as ISO//IEC 17025 or the 

TNI standards. This along with defined method performance for quality control checks (RPD < 20%, Bias 

50 to 150%, Blank < LOQ) must be used to ensure data of known and documented quality is generated to 

make compliance monitoring decisions 

Comment 3: Reporting results for compliance 

a) The commenter wants to note that no data below or above the calibration range must never be reported 

for compliance reporting since the data is unreliable out side the calibration range. The reporting of 
2010 Methods Update Rule Response to Comments 144 March 2012 

unreliable results for permits or compliance monitoring must be discouraged since the comparison and 

enforcement of any values that are from unreliable results shall be contested. 

b) The commenter also discourages the monitoring of analytes (such as congeners) where no reference 

standard exists for each congener and no criteria exists on the toxicity of the specific congener. Method 

1668A provides for the reporting of 209 congeners where only a fraction are available as the native 

congeners for reference materials. A majority of the congeners are identified and quantified using 

relationships that are subject to laboratory and method conjecture. The commenter has reviewed the 

analytical data from a variety of expert laboratories and the demonstration of capability shows no 

comparison of techniques and reporting since the reference method options are allowed. The performance 

of the VER, IPR and OPR are only required for some of the reported congeners and therefore others are 

not subjected to the same level of scrutiny to ensure reliable results are reported. The use of a method 

performed by only three laboratories in the country is not an adequate demonstration of method 

comparability for regulatory reporting. 

Comment 158. 1 

Jerry Parr 

The NELAC Institute 

TNI generally supports the proposed actions published in this proposed rule and is providing comments in 

only three areas. 

1. Citation of NELAC standard - The preamble to the proposed rule stated: 

For methods that have insufficient QA/QC requirements, analysts could refer to and follow the QC 

published in several public sources. Examples of these sources include the instructions in an equivalent 

approved EPA method or standards published by the National Environmental Laboratory Accreditation 

Conference (cf. Chapter 5 of the compendium published in 2003.) 

The National Environmental Laboratory Accreditation Conference ceased operation in 2007 and the 

document referenced is now obsolete. TNI suggests the language be revised to read: 

For methods that have insufficient QA/QC requirements, analysts could refer to and follow the QC 

published in several public sources. Examples of these sources include the instructions in an equivalent 

approved EPA method or standards published by The NELAC Institute (cf. Volume 1: Management and 

Technical Requirements for Laboratories Performing Environmental Analyses.) 

Comment 161.1 

Carol Batterton 

Water Environmental Association of Texas 

We believe that minimum frequencies need to be defined for QC checks and a definition for analytical 

batch and prep batch. If EPA does not want to define the minimum frequencies, prep batch and analytical 

batch terms, then it should reference an acceptable source that does, such as Standard Methods or the TNI 

standards. 

The proposal also states that the quality control checks must be documented in the written method. 

WEAT suggests that the quality control checks be documented in the written method, Quality System 

Manual, or other laboratory document. If a laboratory has already defined analytical and prep batches in 

its Quality Manual, it should not have to define them in every method SOP. 

Comment 162.1 

Ed Saxon 
2010 Methods Update Rule Response to Comments 145 March 2012 

South Carolina Water Quality Association 

We are concerned about the economical and practical aspects of implementing all twelve (12) quality 

control checks outlined in proposed section 136.7 for each parameter for which our members' wastewater 

laboratories hold or will hold certification. Most laboratories already implement applicable quality control 

checks for each method they are certified to run. Requiring labs to implement all twelve checks for all 

parameters, or to provide a detailed explanation for why all checks are not required for a certain method, 

creates undue burdens for smaller laboratories with limited budgets and staff. As an alternative, we 

propose that the laboratories be given the discretion to choose appropriate quality control checks for each 

method, following proper method protocol and procedures. We feel that the publishing authorities for the 

analytical methods have established adequate quality control protocol in the methods themselves, as 

evidenced by the fact that they are in fact proposed for inclusion in Part 136. Having to give detailed 

explanations for exclusion of inappropriate quality control measures serves no purpose in improving the 

quality of the data produced by the laboratories. 

Comment 164.1 

Mark Haley 

Hopewell Regional Wastewater Treatment Facility 

This requirement to address each of these items in SOPs regardless of relevancy to the specific method is 

over burdensome and redundant for laboratories. 

If the intent is for laboratories to document these elements in quality system documentation and/or SOPs, 

the language should be changed as follows: 

"These twelve quality control checks must be clearly defined in the laboratories quality system, including 

a written rationale for why any of these controls are inappropriate for specific methodologies. Each SOP 

or method must include the appropriate quality control elements along with performance specifications 

for each." SOPs should only include procedures and protocols that are relevant to the method to which 

they are written. For example, an SOP for microbiology should not include any information regarding 

surrogates or internal standards, because these elements are not appropriate to the method. 

Comment 166.1 

Paul Wiegand 

National Council for Air and Stream Improvement 

EPA’s proposal to add a special section specifying essential elements of quality control implies that EPA 

has, or intends to have, approved methods that lack quality control data sufficient to properly characterize 

method performance. EPA must not approve methods without first verifying that they can provide results 

of known and acceptable quality as defined by EPA, which requires that the appropriate QC data are 

available prior to approval. Thus, there should be no need for the proposed language. 

EPA proposes addition of §136.7 specifying “essential” elements of quality control (QC). The stated 

reason for doing this is to provide guidance in cases where an approved method provides insufficient 

instruction for developing QC data. The inescapable implication is that EPA is proposing to approve, or 

has in the past approved, methods absent QC data sufficient to fully characterize method performance; 

that is, EPA proposes to add methods that have not been adequately validated. 

Disregarding for a moment the utility of the twelve specific QC elements proposed by EPA, NCASI 

questions the basis for approving a method if relevant QC data/criteria are not already incorporated in the 

method or otherwise commonly available. Put another way, EPA should not approve any method that is 

not already supported by QC results suitable for characterizing method performance. The basis for 
2010 Methods Update Rule Response to Comments 146 March 2012 

approving a method must be acceptable method performance as illustrated by relevant QC data (i.e., 

acceptance criteria or data sufficient to derive acceptance criteria for important/relevant QC metrics). 

Instead of adding a new section to the regulation specifying essential QC elements, EPA should only 

approve methods that already incorporate these elements and for which sufficient data exist to assess 

method performance. Under these conditions, only methods demonstrated to achieve a specified level of 

data quality would be approved for use and there would be no need for the proposed §136.7. Again, the 

fact that EPA feels it necessary to propose addition of this material to Part 136 suggests that EPA 

proposes addition of methods that have not been fully validated. 

With this in mind, NCASI suggests that EPA vet each of the methods being proposed vs. the level of 

validation that would be required if the method had been submitted under the Alternative Test Procedure 

(ATP) Program, and only approve those methods that would be acceptable as alternative test procedures 

for use under 304(h) of the Clean Water Act. 

Regarding the twelve “essential” QC checks proposed by EPA, our primary comment is simply that 

mandating specific QC tests in the absence of an overarching quality assurance (QA) plan is essentially 

meaningless. In addition, NCASI notes that EPA has not provided enough detail to assess the utility of 

any specific QC check, and certainly not enough to ensure that all analysts will perform the same checks 

in the same way. In the end, if EPA is concerned about the quality of data developed using any approved 

method it will need to address data quality on a more holistic level; that is, from a quality systems 

perspective. 

NCASI offers the following suggestions relevant to some of the twelve essential QC elements proposed 

by EPA: 

Demonstration of capability (DOC) - Traditionally, EPA has relied on Initial Precision and Recovery 

(IPR) analyses as a primary component of DOC (in addition to initial calibration and method detection 

limit). Because these analyses are performed using spiked blank matrices (e.g., laboratory water or sand), 

not real-world samples, the results provide an optimistic measure of method performance. Certainly, if a 

competent laboratory cannot generate acceptable results under these circumstances the ruggedness of the 

associated analytical method is open to question. 

Regardless, NCASI suggests that these kinds of data are insufficient to demonstrate method performance 

in any real sense; that is, they do not provide data sufficient to conclude that results from analysis of a 

real-world sample will have a specific level of accuracy. Thus, NCASI recommends that analysis of a 

more challenging matrix be required as part of any DOC. When available, this sample could be a 

relevant Standard Reference Material (SRM). Absent an SRM, use of fortified ASTM substitute 

wastewater (ASTM D5905) would still be an improvement over, for example, laboratory water. 

Method detection limit (MDL) - It should be clearly stated that EPA is referring specifically to the 

definition of MDL provided at 40 CFR 136 (Appendix B). Since the Appendix B procedure specifies 

analyses of fortified blanks (e.g., blank water), the issues raised above regarding DOC based on 

performance in, for example, blank water, are also relevant. 

Matrix spike, matrix spike duplicate, or laboratory fortified blank duplicate for suspected difficult 

matrices - Because matrix spike analyses are performed on real-world samples and laboratory 

fortified blank (LFB) analyses are performed on laboratory blank matrices they are not interchangeable, 

and results from LFB analyses do not effectively characterize method performance in real samples. 

Matrix spike analyses are absolutely necessary for characterizing method performance in real sample 

matrices (difficult or not). Thus the only way to characterize accuracy in a difficult matrix is to perform 

matrix spike experiments, so the requirement should be for matrix spike analyses only. 

 
2010 Methods Update Rule Response to Comments 147 March 2012 

Unfortunately, very few methods have been validated on a significant number of real-world sample 

matrices, so relevant acceptance criteria will often be lacking. In these cases, matrix spike analyses are 

more accurately considered QA metrics, not QC metrics. Regardless, NCASI agrees that matrix spike 

analyses are a critical and necessary component of an overall QA/QC program, and so should be 

performed as a matter of routine. 

Internal standards, surrogate standards (for organic analysis), or tracers (for radiochemistry) - The use of 

internal standards to correct for bias or variability in the final determinative step of an analysis has merit 

in many situations, but it comes with risk. These risks range from imparting undetected bias to analyte 

quantifications (due to interferents impacting an internal standard but not the associated analyte) to sloppy 

laboratory technique (resulting from over reliance on the internal standard correction). Interference can 

also affect interpretation of surrogate recoveries, but this is a less insidious issue than an interferent acting 

on an internal standard. Overall, NCASI fully supports a mandate to incorporate a surrogate or tracer in 

all analytical methods, but suggests that the use of internal standards be discretionary 

. 

Control charts (or other trend analyses of quality control results) - The use of control charts and so on to 

identify intra-laboratory trends is not a necessary component of method QC. Instead, trend analysis is 

more correctly considered a component of overall QA. As such, the requirement to develop and use 

control charts should be considered during laboratory certification/accreditation, and not as part of an 

analytical method. 

Corrective action (root cause analyses) - It is entirely appropriate and useful for an analytical method to 

contain suggestions on troubleshooting (i.e., to suggest corrective action). However, much as is the case 

with respect to control charting, how a laboratory approaches troubleshooting is more appropriately 

associated with QA, and so is more correctly considered to be part of laboratory 

certification/accreditation. 

QC acceptance criteria - The purpose of acceptance criteria is to ensure analytical results of known 

quality, and it is commonly understood that different decisions can defensibly be made using datasets 

exhibiting differing degrees of precision and/or bias (i.e., using datasets of different quality). Thus, it is 

necessary that analytical data be generated from a system under statistical control so that data users can 

assess the suitability of results for their own purposes. This is, however, different than prescribing a 

method to provide a specified level of performance. 

Overall, requiring that a method meet specific QC criteria is tantamount to specifying data quality 

objectives (DQO). However, EPA has not specifically proposed acceptance criteria for any of the 

proposed “universal” QC checks. Instead, EPA states that “These twelve quality control checks must be 

clearly documented in the written method along with a performance specification...” This language 

would allow for data of different qualities from different laboratories applying the same method. This 

may, in fact, be okay as long as relevant statements of precision and bias are provided with all analytical 

results. With this in mind, NCASI suggests that, as part of any new or additional mandate, EPA require 

laboratories to provide statistical statements of precision and bias with all reported sample results. 

However, as implied above, NCASI does not believe that batch-specific QC derived from analysis of 

blank matrices (e.g., blank water) provides data relevant to results obtained from real-world samples. 

Instead, QA or QC data should be developed using real-world samples (e.g., matrix spikes), and the 

associated results should be used to characterize acceptable precision and bias in real-world samples. The 

method-specific sections addressing QA/QC and reporting are the ideal locations for imparting this 

requirement. 

In any event, EPA’s intent here is unclear. Does EPA intend to specify that a method meet specific 

acceptance criteria (e.g., ±20% recovery from a LFB), or simply that the method mandate that, 
2010 Methods Update Rule Response to Comments 148 March 2012 

laboratories perform QC tests and report the results with associated laboratory-specific acceptance 

criteria? This is something that needs to be clarified. 

Overall, NCASI does not believe that EPA’s stated goals can be met by simply adding the proposed 

language at Part 136. In addition to needing to provide more detail on the specific QC checks proposed, it 

appears that EPA is conflating QC with the broader scope of quality assurance or quality systems. 

Finally, NCASI seriously questions why EPA feels this new section is necessary if all the methods being 

proposed have been fully vetted. 

Comment 169.1 

Judith R. Morgan 

American Council of Independent Laboratories 

Comment: 1. The 12 essential quality assurance checks are good additions and we believe that requiring 

these will go a long way towards improving the quality of data from older EPA and other methods that do 

not include rigorous QC requirements. The requirements are general in nature and should provide specific 

exemptions for the following: 

• The requirement for a method detection limit (MDL) (QC requirement #2). A detection limit 

determination should only be required when results are reported below the quantitation limit. MDL 

studies are not appropriate for some parameters (pH, BOD, microbiological, etc.) In addition, EPA 

should consider whether determination of a quantitation limit should be an essential Quality Control 

parameter. The Limit of Quantitation (LOQ) and Limit of Detection (LaD) are internationally 

accepted terms. Laboratories must establish an LOQ for reporting purposes and must further verify 

acceptable precision and accuracy at that limit. From the standpoint of solid and verifiable data, LOQ 

determination and verification are essential and should be a requirement. 

• Tests for which some of the quality assurance tests are not possible or inappropriate (QC 

requirements 2, 4, and 5). For the most part, these are tests for which spiking standards are not 

available, such as temperature, or pH. We suggest adding a section (c) after Section 137 (b) as 

follows: 

Proposed (c) addition - Quality assurance tests requiring spiking solutions, such as MDL, LFB, matrix 

spikes, etc., are not required for tests where the use of spiking solutions is not possible or inappropriate, 

such as pH, conductivity, flash point, temperature, dissolved or suspended solids, color, odor, dissolved 

oxygen, turbidity, BOD, COD and others. Method blanks are also inappropriate for certain tests, such as 

conductivity, temperature, flash point and pH. 

• The requirement for internal standards in organics analysis (QC requirement #6). We agree that 

internal standards should be required for GC/MS analysis, but they can be problematic for certain GC 

analyses that employ detectors such as FID, PID and ECD. It is possible to use internal standards with 

methods such as 602, 604, and 608 for some matrices, and certainly they will work well with the 

calibration standards, but there is a substantial risk of interference with the internal standard when 

analyzing complex and dirty matrices. Because of this potential problem, we believe that internal 

standards should be allowed, but not required, for GC analysis (and HPLC analysis when using a UV 

detector). 

2. Unfortunately, due to the general nature of the requirements, laboratories may have difficulty 

implementing the items without additional guidance. The obvious goal of this requirement is to establish 

consistency between laboratories while providing guidance for essential Quality Control (QC) and 

Quality Assurance (QA). We recommend defining the difference between QC and QA so that the 

laboratories understand that one is an action while the other is a record of the action. 
2010 Methods Update Rule Response to Comments 149 March 2012 

3. Many of the methods do not contain guidance for DOC's, QC Acceptance, etc. This written 

requirement should include approved references to help them to establish the information needed to meet 

this requirement. A reference to a known and approved standard such as the consensus standards 

published by The NELAC Institute (TNI) (specifically Volume 1: Management and Technical 

Requirements for Laboratories 

Performing Environmental Analyses). This standard is based on internationally accepted requirements as 

published in ISO/IEC 17025, General Requirements for the Competence of Testing and Calibration 

Laboratories, which contains other fundamental requirements that are essential to a solid foundational 

basis for a comprehensive QA/~ program.4. 136.7 (b) This statements should be more specific and we 

suggest the following language: 

• For each analytical method, these twelve quality control checks must be clearly documented in a 

laboratory prepared Standard Operating Procedure (SOP), which must include established 

performance specifications relevant to method requirements, where applicable. The procedure must 

include and describe the laboratory's specific approach to meet these 12 essential quality control 

check items. 

Comment 169.1 

Judith R. Morgan 

American Council of Independent Laboratories 

We welcome the requirement for basic QC parameters in general, and the reference to NELAC Chapter 5 

in particular, but note that the 2003 NELAC standards will be superseded in July 2011 by the TNI 

consensus standard "Management and Technical Requirements for Laboratories Performing 

Environmental Analyses". We suggest the following modification: Examples of these sources include the 

instructions in an equivalent approved EPA method; standards published by the National Environmental 

Laboratory Accreditation Conference (cf Chapter 5 of the compendium published in 2003.); or the most 

current and approved consensus standard published by The NELAC Institute (TNI). Specific comments 

on the 12 essential quality control checks are provided later in this document. 

Comment 171.1 

Lola Guerra 

Henrico County DPU 

Comment 1: This requirement is redundant. Essential, applicable quality control measures are already 

described in the individual methods references, as well as state and federal lab accreditation / certification 

regulations. 

Comment 2: Many of these steps are non-applicable to numerous common test methods (e.g. spiking pH, 

Coliforms or toxicity). The requirement that “(b) These twelve quality control checks must be clearly 

documented in the written method...” when a step is not applicable is unnecessary. 

 

Comment 3: The essential steps are too vague to be meaningful. Again, applicable and appropriate QC 

measures are described in detail for individual methods. 

Comment 4: This should not to apply to field measurements and should be clearly stated as such. 

Comment 5: The MDL concept is antiquated in the fact that most laboratories assess at quantification 

levels (QL). 
2010 Methods Update Rule Response to Comments 150 March 2012 

Comment 6: Complicated, lengthy SOPs become an impediment rather than a benefit for bench top 

analysts. 

Comment 7: (8) “Control charts (or other trend analyses of quality control results)”. What are these 

“other trend analyses”? 

Recommendation: Eliminate section 136.7 Quality Assurance and Quality Control. 

Comment 177.1 

Novelle C. Stokes 

South Central Wastewater Authority 

EPA is proposing to specify ``essential'' quality control at Sec.136.7 for use in conducting an analysis 

with an approved method and when insufficient instructions are contained in an approved method. 

Auditors, co-regulators, laboratory personnel, and the regulated community have noted the different 

amounts and types of quality assurance (QA) and quality control (QC) procedures practiced by 

laboratories that use 40 CFR part 136 methods. Some of these methods are published by voluntary 

consensus standards bodies, such as the Standard Methods Committee, and ASTM International. ASTM 

and Standard Methods are contained in printed compendium volumes, electronic compendium volumes, 

or as individual online files. Each organization has its unique compendium structure. QA and QC method 

guidance or requirements may be listed directly in the approved consensus method, or, as is more often 

the case, these requirements are listed in other parts of the compendium. 

For example, the publisher of Standard Methods for the Examination of Water and Wastewater 

consolidates the general quality assurance and quality control requirements for all methods. Each specific 

Part and section can contain additional QA and QC requirements (for example, see part 2020, 3020, 6020, 

and 9020). ASTM specifies QA and QC requirements in the analyte method's Referenced Documents 

section and in the analyte method. Both organizations require the analyst to reference this additional 

information within the respective compendiums to achieve the QA and QC expected for valid results... 

EPA is proposing at 136.7 to specify twelve essential quality control checks that must be in the 

laboratory's documented quality system unless a written rationale is provided to explain why these 

controls are inappropriate for a specific analytical method or application. 

Comment: Insertion of a minimum QC listing still fails to address inconsistencies between different 

approved methods. 

Recommendation: Consistent Quality Control is better addressed if the Agency publicized and adhered to 

a standardized method approval process. Accordingly, the approval of any method or subsequent method 

revision would have to meet at least the minimum standards required previously or by other equivalent 

methods. 

Recommendation: Do not insert a generic list for the entire rule but instead a more specific list for each 

analysis type (i.e. organic, inorganic, biological, etc.). This would reduce the number of individual 

exemptions as each list would be specific for the grouping referenced. Making the list too general simply 

invites further confusion and added inconsistency. 

Comment 189.1 

William Ray 

California State Water Resources Control Board 

We applaud EPA for taking to task the long standing comment on the lack of uniform quality assurance 

among all of the approved methods. However, we are not pleased with the lack of references for the 12 
2010 Methods Update Rule Response to Comments 151 March 2012 

elements listed in section 136.7.b. This will create difficulties when assessing whether the provided 

quality assurance is sufficient. In addition, several common sources of quality assurance or quality 

control practices differ in frequency or limits on performance. Arguments can easily occur because a 

laboratory chose a particular resource while a permitting agency prefers another. In this state in 

particular, the laboratory certification program has commonly cited requirements from EPA’s Manual for 

the Certification of Drinking Water Laboratories even when reviewing labs conducting permit related 

analyses. The requirements in that manual differ from those stipulated in Standard Methods... - 

particularly in the microbiological group of methods. Although EPA indicated in the preamble their 

thinking on resources, not placing references in the rule will lead to inconsistencies and arguments. 

Comment 190 

Lynn Egan 

Lachat Instruments 

The fact that editorial changes do not affect the function or performance of a method, even if the revision 

date has changed, needs to be strongly reiterated here. Revised methods will continue to come out 

AFTER publication occurs. If the changes to a method are editorial, that should not affect approval for 

use of the method. And, it should be noted that often, editorial changes to methods are directly related to 

new rules. The proposed MUR includes additional language regarding QC requirements at 136.7, which 

auditors are very likely to want included to the greatest possible extent, within written methods (once this 

rule has been finalized). This may necessitate additional revisions, albeit editorial, continuing the cycle ... 

USEPA has provided proper terminology for the twelve essential QC checks listed. However, clear 

wording on what each of these twelve QC checks must entail within the text of section 136.7 would also 

be helpful. The proposed rule, on P58071 (a) states: Twelve essential Quality Control checks and 

acceptable abbreviations are:" Then in (b) "These twelve quality control checks must be clearly 

documented in the written method along with a performance specification or description for each of the 

twelve quality control checks". 136.7 however, does not contain any details on what each of the twelve 

entails. Adding this descriptive text would be helpful to both auditors and labs. 

While descriptions/definitions are often part of a written method and are not difficult to include, the 

performance specifications for a given method come from a variety of places (NPDES Permit, the method 

itself, organizations like NELAC, etc.). It is not possible for us to maintain multiple copies of the methods 

that have the various requirements as part of the method in different regions or states Lachat customers I 

have spoken to state that the pass/fail criteria for a given QC test are typically documented within a given 

labs SOPs for each method. This is addressed on P58036 paragraph 3 in the proposed rule, but a clear 

restatement in 136.7 would also help strengthen and clarify this point. 

 - Alternate wording of this statement could document this separation more clearly: "These twelve quality 

control checks must be clearly documented in the written method. Each lab must also document current 

laboratory acceptance criteria (Le. the performance specification) for each of the twelve quality control 

checks. This can be done as part of the written method, or within the labs SOPs, or a combination of the 

two, but must be clearly documented." 

Section II.J Withdrawal of the Appendices 

List of Comments: 

Comment 79.1 - Richard Burrows, TestAmerica Inc. 

Comment 88.1 - Susan D. Hill, Wisconsin State Laboratory of Hygiene 

Comment 89 - David Howell, City of Tampa HFC AWT Plant Analytical Laboratory 

Comment 91.1 - Andrea Rex, Massachusetts Water Resources Authority 

Comment 94.1 - Scott D. Siders, Division of Laboratories, Illinois EPA 
2010 Methods Update Rule Response to Comments 152 March 2012 

Comment 100 - Carol Bell, City of Winston-Salem, North Carolina 

Comment 108.1 - George Noguchi, U.S. Department of the Interior, U.S. Fish and Wildlife Service 

Comment 117.1 - Kelly M. Thompson, Wisconsin Department of Natural Resources 

Comment 123 - Vincent Sapienza, Bureau of Wastewater Treatment, New York City 

Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District 

Comment 134.1 - Josh Kathrinus, American Bottoms Regional Wastewater Treatment Facility 

Comment 158.1 - Jerry Parr, The NELAC Institute 

Comment 169.1 - Judith R. Morgan, American Council of Independent Laboratories 

Summary of Comments: Many commenters noted a typographical error in the discussion of Method 

200.7, where the revision number was listed as 5.4, instead of 4.4. There was general support for the 

withdrawal of Appendices A and C, and some support for withdrawal of all of the appendices. However, 

several commenters requested that Appendix B, the MDL procedure, and Appendix D remain available 

on-line at some OW web site for the foreseeable future, even if they are withdrawn from the CFR. One 

commenter noted that if the withdrawal proceeds, then references to the appendices in other parts of 40 

CFR 136 needs to be removed as well. 

Response: EPA appreciates comments pointing out that a typographical error occurred in the preamble 

to the proposed rule and agrees that the correct reference for the approved version of EPA Method 200.7 

is EPA Method 200.7 Revision 4.4. 

EPA also appreciates the comments supporting the withdrawal of Appendices A and C. However, 

Federal regulations at 1 CFR Part 51.7(c)(1) prohibit the incorporation by reference of material previously 

published in the Federal Register. Thus, EPA is not withdrawing Appendices A or C. Because EPA 

Method 200.7 has been revised, EPA is replacing the current version of this method in Appendix C with 

Rev. 4.4 of Method 200.7. 

EPA did not propose to remove Appendix B, which contains the “Definition and Procedure for the 

Determination of the Method Detection Limit--Revision 1.11,” and Appendix B will continue to be 

published in the Code of Federal Regulations as part of Part 136. 

In response to comments asking EPA to make the current version of Appendix D online, EPA has added 

the previous version (prior to today's rulemaking) of Appendix D to the CWA Methods Web site for 

historical purposes at: http://water.epa.gov/scitech/methods/cwa/index.cfm 

Original Comment Text: 

Comment 79.1 

Richard Burrows 

TestAmerica Inc. 

Comment: We believe that there is a typo, and the version of 200.7 that should be referenced is 4.4 

Comment 88.1 

Susan D. Hill 

Wisconsin State Laboratory of Hygiene 

There is a mis-spelling of Coupled. Also, this section states “...the method has been superseded by Rev. 

5.4 of Method 200.7...” It should state Rev. 4.4. Table IB correctly lists rev. 4.4. 

We do not think it necessary to publish the current version of Appendix D for historical purposes. 

Comment 89 
2010 Methods Update Rule Response to Comments 153 March 2012 

David Howell 

City of Tampa HFC AWT Plant Analytical Laboratory 

I believe that there is a typo as indicated by the underlined number in the attached jpg file (not converted 

by EPA). The method number should be 4.4 instead of 5.4 for the method referenced (EPA 200.7). 

Comment 91.1 

Andrea Rex 

Massachusetts Water Resources Authority 

MWRA agrees with the logic of removing these appendices and for making the pertinent information 

available online. 

Comment 94.1 

Scott D. Siders 

Division of Laboratories, Illinois EPA 

Method 200.7, reference to Rev 5.4 Comment: We believe that there is a typo, and the version of 200.7 

that should be referenced is 4.4 

Appendix D Comment: Agree that the current version of Appendix D should be made available online at 

the CWA methods website for historical purposes. 

Comment 100 

Carol Bell 

City of Winston-Salem, North Carolina 

In the summary, on page 58036, J., middle column, first complete paragraph, the reference to Rev. 5.4 of 

Method 200.7 would be incorrect - perhaps Rev. 4.4??? 

Comment 108.1 

George Noguchi 

U.S. Department of the Interior, U.S. Fish and Wildlife Service 

We ask that EPA make available, at least temporarily, the current version of Appendix D online at the 

CWA methods web site for historical purposes. 

Comment 117.1 

Kelly M. Thompson 

Wisconsin Department of Natural Resources 

Section II.J We support the withdrawal of Appendices A and C, as these methods are (and will be) 

readily available from other sources. We would only support withdrawal of Appendix B if the information 

is stored and made readily available to the public. This is critical because the protocol for determination 

of method detection limit has been (and likely will be for some time) an integral part of environmental 

testing. Similarly, we would support withdrawal of Appendix D if the information is archived and made 

readily available to the public. 

Assuming this aspect of the rule is finalized, we believe that footnote 2 to the aforementioned Tables 

needs to be edited regarding the location of material in Appendices A through D. 

Comment 123 
2010 Methods Update Rule Response to Comments 154 March 2012 

Vincent Sapienza 

Bureau of Wastewater Treatment, New York City 

There is no revision 5.4 for Method 200.7. We assume this was a typographical error. The latest version 

for metal parameters in table IB is 4.4 (1994). 

Comment 132.1 

Paula Hogg 

Hampton Roads Sanitation District 

A revision 5.4 of Method 200.7 was not readily found. Method 200.7, Rev. 4.4 is listed in Table lB of 

40CRF 136. The reference to Revision 5.4 seems to be a typographical error. 

Comment 134.1 

Josh Kathrinus 

American Bottoms Regional Wastewater Treatment Facility 

The reference to “Rev. 5.4 of Method 200.7” is incorrect. The reference should be to Rev. 4.4. 

Comment 169.1 

Judith R. Morgan 

American Council of Independent Laboratories 

We believe that there is a typo, and the version of 200.7 that should be referenced is 4.4. All other 

references in the document are for rev. 4.4. 

Section II.K Proposed Revisions to 40 CFR 423 

List of Comments: 

Comment 101.1 - New York State Department of Environmental Conservation 

Summary of Comments: One commenter suggested that these changes to chlorine residual 

measurements have applicability beyond the steam electric power generating point source category, and 

thus they should be incorporated into 40 CFR 136 instead. 

Response: EPA thanks the commenter for this suggestion and may consider this change in a future 

rulemaking. The scope of the change is only applicable to the steam electric power generating point 

source at this time and EPA is promulgating these changes as proposed. 

Original Comment Text: 

Comment 101.1 

New York State Department of Environmental Conservation 

In this section, certain clarifications are made regarding the definitions for total residual chlorine (TRC) 

and total residual oxidants (TRO). Clarifications are also made as to how to measure for TRC/TRO. 

As written, these definitions and clarifications are only applicable to discharges from “Steam Electric 

Power Generating Point Source Category,” per the rules of Part 423. These definitions and clarifications 

have applicability outside this single point source category and should apply to all categories of 

dischargers. 
2010 Methods Update Rule Response to Comments 155 March 2012 

Moving the TRC/TRO clarification to Part 136.3 would be a more logical fit, especially considering all 

the tables of approved methods from the 40 CFR point source categories are being consolidated into Part 

136.3. 

Section II.L Proposed Revisions to 40 CFR 430 

EPA received no comments on this section and is promulgating the changes as proposed. 

Section II.M Proposed Revisions to 40 CFR 435 

List of comments: 

Comment 101.1 - Jason Fagel, New York State Department of Environmental Conservation 

Comment 127.1 - Roger Claff, American Petroleum Institute 

Comment 155.1 - Rob Kuehn, Offshore Operators Committee 

New York State Department of Environmental Conservation (Comment 101.1)

Original Comment Text: NYSDEC opposes moving the methods found at 40 CFR part 435, subpart A 

(Offshore Subcategory) to a separate EPA document titled “Analytic Methods for the Oil and Gas 

Extraction Point Source Category,'' EPA-821-R-09-013. 

The CFR is the legal reference for approved methods and typically takes precedence over other EPA 

reports and publications. In order to be effective, the approved analytical methods for monitoring point 

sources must be accurate, precise, and listed in a single legal reference document. By migrating the list 

of approved analytical methods (for oil and gas extraction permits) to an alternate source, the full force 

and effect of law provided via the CFR will be diminished. Losing this critical piece of enforcement will 

weaken the permitting authorities’ ability to protect and conserve water resources at risk from the oil and 

gas extraction process. 

Response: EPA disagrees with the commenter’s assertion that in order to be effective the approved 

analytical methods must be re-printed in the Code of Federal Regulations. EPA’s practice is to list the 

approve methods in Part 136 and in the various point source categories (e.g., Oil and Gas Extraction – 40 

CFR 435) and to incorporate these methods by reference. For example, Table IB in 40 CFR 136.3 lists 

(not re-prints) the approved analytic methods for inorganic parameters. EPA works with the Director of 

the Federal Register to incorporate these analytic methods by reference in Part 136 and in the various 

point source categories. See 5 U.S.C. 552(a) and 1 CFR 51. The approved analytic methods in Part 136 

and in the various point source categories may be inspected at EPA's Water Docket, EPA West, 1301 

Constitution Avenue, NW., Room B102, Washington, DC (Telephone: 202–566–2426); or at the National 

Archives and Records Administration (NARA). For information on the availability of this material at 

NARA, call 202–741–6030, or go to: 

http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. 

EPA also disagrees with the commenter’s assertion that this incorporation by reference procedure 

diminishes the enforceability of NPDES effluent limits derived from effluent guidelines. NPDES 

regulations at 40 CFR 122.44(a) and 125.3(a) require NPDES permit writers to develop technology-based 

treatment requirements and incorporate these limits as enforceable conditions in NPDES permits. NPDES 

permits issued to individual dischargers transform any generally applicable effluent limitations guidelines 

and standards, which are a type of technology-based treatment requirements, into effluent limitations that 

apply specifically to the individual discharger. See EPA v. California ex rel. State Water Resources 

Control Bd., 426 U.S. 200, 205 (1976). EPA has identified the failure of a permit writer to appropriately 

incorporate applicable technology-based treatment requirements into enforceable NPDES permit effluent 

limitations as a condition for EPA disapproval of the permit. See “Central Tenets of the National 
2010 Methods Update Rule Response to Comments 156 March 2012 

Pollutant Discharge Elimination System (NPDES) Permitting Program.”1 Consequently, EPA does not 

need to re-print the approved analytic methods specific to the Oil and Gas extraction point source 

category in the CFR to ensure that NPDES permit writers incorporate the use of these approved analytic 

methods as enforceable conditions in permits. The incorporation by reference of these approved analytic 

methods in Part 435 means that these methods are included in the effluent guidelines requirements and 

must be used by NPDES permit writers as enforceable conditions in permits. Additionally, oil and gas 

extraction permittees must use the approved analytic methods incorporated by reference in Part 435 to 

demonstrate compliance with their permit. 

In the final rulemaking EPA did not delete the analytic methods specific to the Oil and Gas extraction 

point source category from the CFR. Subsequent to the proposed rule the Director of Legal Affairs and 

Policy at the Office of the Federal Register informed EPA that Federal regulations at 1 CFR 51.7 (c)(1) 

prohibit the incorporation by reference of material published previously in the Federal Register. These 

regulations prevent EPA from deleting these methods from 40 CFR 435 and incorporating these methods 

by reference to this document. 

Roger Claff, American Petroleum Institute (Comment 127.1)

Original Comment Text: 

API concurs in total with the detailed comments submitted by the Offshore Operators Committee (OOC) 

in response to the Proposed Rule. The OOC's detailed comments pertain to the draft document, Analytic 

Methods for the Oil and Gas Extraction Point Source Category, EPA-821-R¬09-013, U. S. Environmental 

Protection Agency Engineering and Analysis Division, Office of Water, September 2009. In the Proposed 

Rule (75 Fed. Reg. 58036) EPA is proposing to move, and in two cases, revise analytical methods from 

40 CFR 435 Subpart A to this document, and included this document in the record for this rulemaking. 

The OOC's detailed comments address method updates and updates to current laboratory practice, provide 

important clarification, and address specific technical concerns with these analytical methods. API 

strongly recommends EPA adopt OOC's proposed modifications. 

Response: EPA thanks API for their comments and has responded to OOC comments. 

Original Comment Text: 

API also offers the following specific comments on Method 1655, Determination of Crude Oil 

Contamination in Non-Aqueous Drilling Fluids by Gas Chromatography/Mass Spectrometry, as 

referenced in the Proposed Rule: 

Section 6.4.3 -The section states glassware shall be cleaned by rinsing with solvent and baked at 400 

degrees C for a minimum of 1 hour. Volumetric glassware, however, should never be heated because the 

glass will expand, rendering the calibrations inaccurate. 

Response: EPA disagrees with this comment. Glassware must be scrupulously cleaned to avoid cross 

contamination. Volumetric glassware can be heated and then be allowed to cool and then stored inverted 

or capped with aluminum foil to avoid contamination. This procedure in EPA Method 1655 is a similar to 

the procedure in EPA Method 625 (Semivolatile Organic Compounds by Isotope Dilution GC/MS, 

Section 3.1.1) for reducing potential cross contamination. 

Original Comment Text: 

 

1

 Available at: http://www.epa.gov/npdes/pubs/tenets.pdf. 
2010 Methods Update Rule Response to Comments 157 March 2012 

Section 6.6.3.2 -The section states the mass spectrometer shall be capable of scanning from 35 to 500 

amu. The upper range should be changed to 600 amu, to be consistent with Table 6-1 of the method. 

Response: EPA agrees with the commenter and has changed the range in the method to state that the 

mass spectrometer shall be capable of scanning from 35 to 600 amu. 

Original Comment Text: 

Section 6.9.5.2 -The formula for RPD is incorrect. The correct formula is: 

RPD = [│D1-D2│ / ((D1+D2)/2)] x 100 

Response: EPA agrees with the commenter and has replaced the formula in the method with the above 

formula. 

Rob Kuehn, Offshore Operators Committee (Comment 155.1)

(1) Original Comment Text: 

OOC supports all the proposed changes to 40 CFR 435. 

Response: EPA appreciates the comment in support of the proposed changes to 40 CFR part 435. 

(2) Original Comment Text: 

OOC recommends incorporation of Appendix B-1 (Methane Measurement) of GMG 290000 as well into 

the proposed methods manual EPA–821–R–09–013. This will ensure all relevant protocols associated 

with the marine anaerobic biodegradation analytic method are in the proposed manual. 

Response: The commenter has overlooked the fact that Appendix B-1 (Methane Measurement) of GMG 

290000 is in EPA Method 1647 at Section 5.7. Additionally, Appendix B-2 (Concentration Verification 

Analyses) and Appendix B-3 (Program Quality Assurance and Quality Control) of GMG 290000 are now 

Sections 5.8 and 5.9 of EPA Method 1647. 

(3) Original Comment Text: 

OOC recommends incorporating Appendix 8 into the proposed manual EPA–821–R–09–013 and being 

assigned a method number (hereafter referred to in these comments as EPA Method XXX. Appendix 8 is 

the Reference C16–C18 Internal Olefin Drilling Fluid Formulation and as such appropriately belongs 

within the proposed manual. 

Response: EPA disagrees with this comment as the procedures provide a means to standardize the 

formulation of a reference C16–C18 internal olefin drilling fluid for use in determining the drilling fluid 

sediment toxicity ratio and compliance with the BAT sediment toxicity discharge limitation (see §435.13) 

and NSPS (see §435.15). These produces are not a method but provide the steps necessary for proper 

execution of other EPA analytic methods. 

(4) Original Comment Text: 

Page 1-1, (Red Line EPA–821–R–09–013) Revise as follows: 
2010 Methods Update Rule Response to Comments 158 March 2012 

EPA requires operators using this method to use Leptocheirus plumulosus as the test organism, the 

sediment preparation procedures specified in EPA Method 1646, and the specific test procedures included 

in the NPDES permit for the Western Gulf of Mexico (“Final NPDES General Permit for New and 

Existing Sources and New Dischargers in the Offshore Subcategory of the Oil and Gas Extraction 

Category for the Western Portion of the Outer Continental Shelf of the Gulf of Mexico,” GMG290000, 

Appendix A: METHOD FOR CONDUCTING A SEDIMENT TOXICITY TEST WITH Leptocheirus 

plumulosus AND NON-AQUEOUS FLUIDS OR SYNTHETIC BASED DRILLING MUDS. 

Additionally, EPA Method XXX (See Comment #3) provides specifications for appropriate reference 

drilling fluids. 

Rationale: Similar to Appendix B of GMG 290000 being necessary for performing biodegradation test, 

Appendix A of GMG 290000 is necessary for performing the drilling fluids toxicity test (EPA proposed 

method # 1619). OOC would prefer to see Appendix A incorporated into EPA-821-R-09-013 method # 

1619. Alternatively, EPA could incorporate Appendix A by reference (as shown in the proposed language 

at the left). 

Response: EPA agrees with incorporating these additional quality assurance procedures from the NPDES 

permit for the Western Gulf of Mexico (GMG290000). EPA has included Appendix A from the NPDES 

permit for the Western Gulf of Mexico (GMG290000) into Section 10 in this document (EPA Method 

1644). 

(5) Original Comment Text: 

Page 1-2 (Red Line EPA–821–R–09–013) 

Add: Where an approved NPDES permit is issued and the permit specifies modifications or enhancements 

to the methods herein, the permit shall take precedence. 

Rationale: OOC believes this clarification will allow Permit Writers flexibility in modifying the methods 

where supported by changing conditions, and provides certainty to Operators on the hierarchy for method 

compliance. 

Response: No additional language is needed as permit writers may modify an approved EPA analytic 

method as described at 40 CFR Part 136.6. The March 12, 2007 Methods Update Rule (MUR) that 

promulgated 40 CFR 136.6 allows the regulated community more flexibility to modify approved methods 

without EPA review. This regulation allows the analytical community greater flexibility to modify 

approved methods to lower the costs of measurements, overcome matrix interferences, or otherwise 

improve the analysis without EPA review. Laboratories that modify 40 CFR Part 136 methods may be 

private, public or commercial and may conduct analyses for one or more clients or facilities. 

(6) Original Comment Text: 

Page 1-3, Table 1-1, (Red Line EPA–821–R–09–013) 

Revise as follows: 

Drilling fluid sediment toxicity (4-Day Test)- Standard Guide for Conducting 10-day Static Sediment 

Toxicity Tests with Marine and Estuarine Amphipods ASTM E 1367–92, EPA Method XXX, and 

Appendix A of GMG2900000 

Rationale: Same justifications as Comment #3 and #4 
2010 Methods Update Rule Response to Comments 159 March 2012 

Response: EPA agrees with incorporating these additional quality assurance procedures from the NPDES 

permit for the Western Gulf of Mexico (GMG290000). EPA has included Appendix A from the NPDES 

permit for the Western Gulf of Mexico (GMG290000) into Section 10 in this document (EPA Method 

1644). 

(7) Original Comment Text: 

Page 1-4, Table 1-1, (Red Line EPA–821–R–09–013) 

Revise as follows: 

Base fluid sediment toxicity (10-Day Test)- Standard Guide for Conducting 10-day Static Sediment 

Toxicity Tests with Marine and Estuarine Amphipods ASTM E 1367–92 

after using and Appendix A of GMG2900000 Procedure for Mixing Base Fluids with Sediments 

EPA Method 1646 

Rationale: Same justifications as Comment #4. 

Response: EPA agrees with incorporating these additional quality assurance procedures from the NPDES 

permit for the Western Gulf of Mexico (GMG290000). EPA has included Appendix A from the NPDES 

permit for the Western Gulf of Mexico (GMG290000) into Section 10 in this document (EPA Method 

1644). 

(8) Original Comment Text: 

Section 1.3, (Red Line EPA–821–R–09–013) 

Revise as follows: 

This method is used to amend uncontaminated and nontoxic (control) natural or formulated sediments 

with synthetic-based drilling fluids or the.......... 

Rationale: Adds clarity to the sentence 

Response: This comment is outside the scope of this methods update rulemaking. EPA does not have 

data to determine the effect of the using formulated sediments in lieu of natural sediments. For example, 

the commenter did not provide and EPA does not have data on the potential affect the use of formulated 

sediments would have on the discriminatory power of this test. Additional data and information on the 

potential impacts of the use of formulated sediments on: (1) the ability of the test to discriminate the 

various technologies; (2) ecological relevance; (3) potential impacts on inter- and intra-laboratory 

variability; and (4) practicality for laboratory usage. 

(9) Original Comment Text: 

Page 1-10, Table 1-3, (Red Line EPA–821–R–09–013) 

Add new line item to table that creates a new EPA method for 40 CFR 435 Appendix 8 Reference C16-

C18 Internal Olefin Drilling Fluid Formulation 

Rationale: Same justifications as Comment #3 

Response: See response to Comment #3. 

(10) Original Comment Text: 
2010 Methods Update Rule Response to Comments 160 March 2012 

Section 3.3.2.1, (Red Line EPA–821–R–09–013) 

Revise as follows: 

Collection of water samples shall be made with appropriate acid-rinsed linear-polyethylene bottles or 

other appropriate non-contaminating water sampling devices. Special care shall be taken to avoid the 

introduction of contaminants from the sampling devices and containers. Prior to use, the sampling devices 

and containers should be thoroughly cleaned with a detergent solution, rinsed with tap water, rinsed with 

10% (or stronger) soaked in 10% hydrochloric acid (HCl), rinsed with tap water for 4 hours, and then 

thoroughly rinsed with deionized glass-distilled water. 

Rationale: These proposed changes reflect updates to the method based on current best laboratory 

practice and are consistent with the requirements of U.S. Environmental Protection Agency, October 

2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and 

Marine Organisms. EPA 821-R-02-012. Washington, DC, 5th Edition. 

Response: This comment is outside the scope of this methods update rulemaking. EPA does not have, 

and the commenter did not provide, data to determine the effect of incorporating these changes into the 

analytic method. Additional data and information on incorporating these changes into the analytic method 

are necessary to determine: (1) the ability of the test to discriminate the various technologies; (2) 

ecological relevance; (3) potential impacts on inter- and intra-laboratory variability; and (4) practicality 

for laboratory usage. 

(11) Original Comment Text: 

3.3.3, (Red Line EPA–821–R–09–013) 

Revise as shown in red line document. 

Rationale: These proposed changes reflect updates to the method based on current best laboratory 

practice and more recent guidance on allowed sample preservation temperature range. The change in 

mixing speed from “1000 rpm” to “1000 rpm to 2000 rpm” provides flexibility for ensuring that various 

sized samples are mixed homogeneously. 

Response: See response to Comment #10. 

(12) Original Comment Text: 

3.4.1, (Red Line EPA–821–R–09–013) 

Revise as shown in red line document. 

Rationale: Additional materials added under Apparatus. Glassware cleaning procedure edited to include 

plasticware and updated to be consistent with the requirements of U.S. Environmental Protection Agency, 

October 2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to 

Freshwater and Marine Organisms. EPA 821-R-02-012. Washington, DC, 5th Edition. 

Response: EPA Response: See response to Comment #10. 

(13) Original Comment Text: 

Revise as shown: 
2010 Methods Update Rule Response to Comments 161 March 2012 

Diluent seawater and exposure seawater samples are prepared by filtration through a 1.0 micrometer filter 

prior to analysis. Artificial seawater may be used as long as the seawater has been prepared by EPA 

methods, standard methods, or ASTM methods, has been properly “seasoned,” filtered, and has been 

diluted with distilled or deionized water to the same specified 20 ±2 ppt salinity and 20 ±2°C temperature 

as the “natural” seawater. 

Rationale: These proposed changes reflect updates to the method based on current best laboratory 

practice and are consistent with the requirements of U.S. Environmental Protection Agency, October 

2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and 

Marine Organisms. EPA 821-R-02-012. Washington, DC, 5th Edition. 

Response: EPA Response: See response to Comment #10. 

(14) Original Comment Text: 

3.4.3.1, (Red Line EPA–821–R–09–013) 

Revise as shown in red line document. 

Rationale: These proposed changes reflect updates to the method based on current best laboratory 

practice, more recent guidance on allowed sample preservation temperature range and, adds guidance for 

non –aqueous drilling fluid SPP preparation. 

Response: See response to Comment #10. 

(15) Original Comment Text: 

Revise as follows: 

Mix this mud/water slurry with magnetic stirrer(s) for 5 minutes. Measure the pH of water-base drilling 

fluid/water slurries and, if necessary, adjust (decrease) the pH of the slurry to within 0.2 units of the 

seawater by adding 6N HCl while stirring the slurry. Then, allow the slurry to settle for 1 hour. Record 

the amount of HCl added. Non–aqueous drilling fluid/water slurries can not be mixed homogeneously and 

measuring pH of these slurries is not practical. After non–aqueous drilling fluid/water slurries settle for 1 

hour and the SPP is decanted, measure the pH of the SPP and adjust to a pH 7.8 ±0.1. 

Rationale: These proposed changes reflect updates to the method based on current best laboratory 

practice and add guidance for non –aqueous drilling fluid SPP preparation. Non–aqueous drilling 

fluid/water slurries consist of multiple phases and measuring pH of these slurries is not practical. 

Response: See response to Comment #10. 

(16) Original Comment Text: 

3.4.3.5, (Red Line EPA–821–R–09–013) 

Delete: Measurement of the filterable and unfilterable residue of each SPP prepared for testing. 

Rationale: OOC recommends deletion of the residue measurement requirement. Residue measurements 

are not used in the test, related to the results, nor reported on DMRs. 

Response: See response to Comment #10. EPA also notes that the standard for whether a value is 

collected and retained by the permittee is not whether this data is reported on the DMR. EPA requires 
2010 Methods Update Rule Response to Comments 162 March 2012 

compliance monitoring data to be maintained by permittees above and beyond what is reported on the 

Discharge Monitoring Report (see 40 CFR 122.41(j)(2)). 

(17) Original Comment Text: 

3.4.3.6, (Red Line EPA–821–R–09–013) 

Delete: Record the time; and, measure DO and pH for Day 0. 

Rationale: This sentence should be deleted, as Section 3.5.5.6 more fully describes required water quality 

measurements 

Response: EPA agrees with commenter that this is redundant language and has made the recommended 

change. 

(18) Original Comment Text: 

3.5.1, (Red Line EPA–821–R–09–013) 

Revise as follows: 

Items listed by Borthwick [1] are required for e Each definitive test series, which consists of 18 test 

containers: 3 replicates of a one set of control and 5 SPP dilutions test containers, with three replicates of 

each. Test containers should be Pyrex or equivalent glass. For definitive tests, 5 SPP dilutions with 3 

replicates of at least 500 ml each are required. Twenty mysids per replicate, 360 per definitive test are 

required. 

Rationale: A range-finding test consists of at least 6 test containers: 1 replicate of a control and 5 SPP 

dilutions. The duration of range-finding tests may be less than 96 hours. Ten or more mysids per replicate, 

at least 60 per range-finding test, are suggested. Daily water quality measurements and observations are 

optional with range-finding tests. 

Response: EPA agrees with the clarifications as they clarify existing requirements. 

(19) Original Comment Text: 

3.5.3, (Red Line EPA–821–R–09–013) 

Revise as follows: 

The Suspended Particulate Phase (SPP) tests on drilling muds shall utilize the test species Mysidopsis 

bahia. Test animals shall be 3, 4, 5, or 6 to 6 days old with maximum of 24-hour range in age... 

Rationale: These proposed changes reflect updates to the method based on current best laboratory 

practice and are consistent with the requirements of U.S. Environmental Protection Agency, October 

2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and 

Marine Organisms. EPA 821-R-02-012. Washington, DC, 5th Edition. 

Response: See response to Comment #10. 

(20) Original Comment Text: 

3.5.5.1, (Red Line EPA–821–R–09–013) 

Revise as follows: 
2010 Methods Update Rule Response to Comments 163 March 2012 

Wash all glassware and plasticware thoroughly with a detergent solution, rinse with tap water, rinse with 

10% (or stronger) hydrochloric acid (HCl), rinse with tap water, rinse with pesticide-grade acetone, rinse 

with tap water, and then thoroughly rinse with deionized water. Wash all glassware with detergent, rinse 

five times with tap water, rinse once with acetone, rinse several times with distilled or deionized water, 

place in a clean 10% HCl acid bath for a minimum of 4 hours, rinse five times with tap water, and then 

rinse five times with distilled water.

Rationale: Glassware cleaning procedure edited to include plasticware and updated to be consistent with 

the requirements of U.S. Environmental Protection Agency, October 2002. Methods for Measuring the 

Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. EPA 821-R-02-

012. Washington, DC, 5th Edition. 

Response: See response to Comment #10. 

(21) Original Comment Text: 

3.5.5.2, (Red Line EPA–821–R–09–013) 

Revise as follows: 

Establish the definitive test concentrations based on results of a range finding test or based on prior 

experience and knowledge of the mud system. 

Rationale: Often, mud systems are routine and have been tested multiple times. This change clarifies that 

a range-finding test is not required prior to each definitive test. 

Response: EPA agrees with this clarification as prior knowledge of existing mud systems can often 

predict ranges. 

(22) Original Comment Text: 

3.5.5.3, (Red Line EPA–821–R–09–013) 

Revise as follows: 

Twenty organisms are exposed in each test dish. Nytex® cups shall may be used to help find surviving 

test organisms at the end of the test. If used, the Nytex® cups arebe inserted into every test dish prior to 

adding the animals. These “nylon mesh screen” nytex holding cups are can be fabricated by gluing a 

collar of 363-micrometer mesh nylon screen to a 15-centimeter wide Petri dish with silicone sealant. 

Rationale: These changes clarify that the use of Nytex cups (cages) within test dishes is optional. Cages 

are fragile and require construction with silicone and PVC glue. 

Response: See response to Comment #10. 

(23) Original Comment Text: 

3.5.5.6, (Red Line EPA–821–R–09–013) 

Revise as follows: 

Observations may be attempted at 4, 6 and 8 hours; they must be attempted with non–aqueous drilling 

fluid SPPs at 0, 24, 48, and 72 hours and must be made in all SPPs at 96 hours. Water-base drilling fluid 

SPP concentrations are usually very turbid preventing observations until the test is terminated. Daily 

observations in water-base drilling fluid SPP concentrations need not be attempted if the turbidity is 

obviously too high. Attempts at observations refers to placing a test dish on a light table and visually 
2010 Methods Update Rule Response to Comments 164 March 2012 

counting the animals. If Attempts at observations refers to placing a test dish on a light table and visually 

counting the animals. Do not lift the “nylon mesh screen” cups are used, do not lift them out of the test 

dish to make the observation. No unnecessary handling of the animals should occur during the 96 hour 

test period. Beginning at Day 0-before the animals are placed in the test containers DO, temperature, 

salinity, and pH shall be measured every 24 hours.DO and pH measurements must also be made at 0, 24, 

48, 72, and 96 hours. Take and replace the test medium necessary for the DO and pH measurements 

outside of the nytex cups to minimize stresses on the animals. 

Rationale: These changes clarify that test dishes with very turbid SPPs that prevent the test organisms 

from being counted need not be put on a light table daily and that test medium necessary for daily water 

quality measurements does not need to be taken out of test dishes and replaced. The EPA acute manual 

(EPA 821-R-02-012) does not directly address taking water quality measurements in test medium 

removed from test dishes or directly in test dishes. The M. bahia chronic test, Method 1007.0, in EPA’s 

marine chronic manual (EPA 821-R-02-014) does require that water quality measurements be made 

directly in the test dishes. Measuring water quality parameters directly in M. bahia SPP dishes is practical 

and will not adversely affect test results. 

Response: See response to Comment #10. 

(24) Original Comment Text: 

3.6.1.1, (Red Line EPA–821–R–09–013) 

Revise as follows: 

Reference toxicants such as sodium chloride (NaCl), potassium chloride (KCl), cadmium chloride 

(CdCl2), copper sulfate (CuSO4), sSodium lauryl sulfate or dodecyl sodium sulfate (SDS), and potassium 

dichromate (K2Cr2O7) are suitable for use in the NPDES and other Agency programs requiring aquatic 

toxicity is used as a reference toxicant for the positive control. The chemical used should be 

approximately 95% pure. The source, lot number, and percent purity shall be reported. 

Rationale: These proposed changes reflect updates to the method based on current best laboratory 

practice and are consistent with the requirements of U.S. Environmental Protection Agency, October 

2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and 

Marine Organisms. EPA 821-R-02-012. Washington, DC, 5th Edition. 

Response: See response to Comment #10. 

(25) Original Comment Text: 

3.6.1.2, (Red Line EPA–821–R–09–013) 

Revise as follows: 

Test methods are those used for the drilling fluid tests, except that the test material was prepared by 

weighing one gram of the reference toxicant sodium lauryl sulfate on an analytical balance 

Rationale: To make this paragraph consistent with Comment #24 

Response: See response to Comment #10. 

(26) Original Comment Text: 

3.8, (Red Line EPA–821–R–09–013) 
2010 Methods Update Rule Response to Comments 165 March 2012 

Revise reference Number 4 as follows: 

U.S. Environmental Protection Agency, September 1991 October 2002. Methods for Measuring the Acute 

Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. EPA 821-R-02-

012/600/4–90/027. Washington, DC, 4th 5th Edition. 

Rationale: Updates reference to latest edition. 

Response: See response to Comment #10. EPA will wait until there are additional data before updating 

this reference. 

(27) Original Comment Text: 

4.0, (Red Line EPA–821–R–09–013) 

Revise as follows: 

This procedure describes a method for amending uncontaminated and nontoxic (control) natural or 

formulated sediments with synthetic-based drilling fluids or the base fluids that are used to formulate 

synthetic-based drilling fluids and other non-aqueous drilling fluids. Initially, control sediments shall be 

press-sieved through a 2,000 micron mesh sieve to remove large debris. Then press-sieve the sediment 

through a 500 micron sieve to remove indigenous organisms that may prey on the test species or 

otherwise confound test results. Homogenize control sediment to limit the effects of settling that may 

have occurred during storage. Sediments should be homogenized before density determinations and 

addition of base fluid to control sediment. Because base fluids are strongly hydrophobic and do not 

readily mix with sediment, care must be taken to ensure base fluids are thoroughly homogenized within 

the sediment. All Base fluid concentrations are weight-to-weight (mg of base fluid to kg of dry control 

sediment). For test materials other than pure base fluids (e.g., whole mud formulations), concentrations 

are volume-to-weight (mL of test substance to kg of dry control sediment. Sediment and base fluidtest 

material mixing shall be accomplished by using the following method. 

Rationale: These proposed changes clarify that EPA Method 1646 is applicable for amending natural or 

formulated control sediment with synthetic base fluids, synthetic based drilling fluids, and other nonaqueous drilling fluids. 

Response: See response to Comment #10. 

(28) Original Comment Text: 

4.5, (Red Line EPA–821–R–09–013) 

Revise as follows: 

Tests for homogeneity of base fluid in sediment are to be performed during the procedure development 

phase at each testing laboratory. Because of difficulty of homogeneously mixing base fluid with sediment, 

it is important to demonstrate that the base fluid is evenly mixed with sediment. The sediment shall be 

analyzed for total petroleum hydrocarbons (TPH) using EPA Methods 3550A and 8015M, with samples 

taken both prior to and after distribution to replicate test containers. Base-fluid content is measured as 

TPH. After mixing the sediment, a minimum of three replicate sediment samples shall be taken prior to 

distribution into test containers. After the test sediment is distributed to test containers, an additional three 

sediment samples shall be taken from three test containers to ensure proper distribution of base fluid 

within test containers. Base-fluid content results shall be reported within 48 hours of mixingas soon as 

practical. The coefficient of variation (CV) for the replicate samples must be less than 20%. If base-fluid 

content results are not within the 20% CV limit, additional TPH samples from freshly mixed sediments 
2010 Methods Update Rule Response to Comments 166 March 2012 

are required. the test sediment shall be remixed. Laboratories must not complete tests for demonstrating 

permit compliance until they have demonstrated the ability to homogeneously mix base fluid (and/or 

synthetic-base drilling fluids) with sediment by achieving CVsTests shall not begin until the CV is 

determined to be below the maximum limit of 20% for multiple triplicate TPH samples. During the test, a 

minimum of three replicate containers shall be sampled to determine base-fluid content during each 

sampling period.After their development phase, laboratories that have successfully implemented these 

tests must at a minimum maintain records of annual certification of mixing capability for each laboratory 

mixing technician. 

Rationale: Clarifies that TPH measurements and demonstration of ability to homogenously mix base 

fluids and/or synthetic base drilling fluids with sediment are required by each laboratory initially and 

annually thereafter. 

Response: See response to Comment #10. 

(29) Original Comment Text: 

5.2.1, (Red Line EPA–821–R–09–013) 

Revise as follows: 

The concentration of base fluids is 2,000 mg carbon test material/kg dry sediment. 

Rationale: Clarifies that the concentration of base fluids is 2,000 mg carbon from the test material per kg 

dry sediment 

Response: This language is already incorporated in the method. 

(30) Original Comment Text: 

5.4, (Red Line EPA–821–R–09–013) 

Revise as follows: 

Of the seven serum bottles set up for each test or control condition, three are randomly selected for 

concentration verification analyses. These should be immediately placed at 0.1 to 6° C and 

Rationale: To make the paragraph consistent with current EPA guidance for preservation temperatures. 

Response: See response to Comment #10. 

(31) Original Comment Text: 

8.5.2.6, (Red Line EPA–821–R–09–013) 

Delete reference to Best Management Practices consistent with Comment #33. See Comment #33. 

Response: EPA disagrees with the commenter. EPA identified the use of BMPs are part of the 

technology basis for controlling NAF-cuttings dischargers. Consequently EPA has identified the 

parameters and conditions that should be incorporated with any BMP plan. Additionally, the use of BMPs 

directly relates to the frequency of sampling, which is directly tied to EPA Method 1674. 

(32) Original Comment Text: 
2010 Methods Update Rule Response to Comments 167 March 2012 

8.5.4.6, (Red Line EPA–821–R–09–013) 

Delete reference to Best Management Practices consistent with Comment #33. See Comment #33.

Response: See response to Comment #31. 

(33) Original Comment Text: 

8.6, (Red Line EPA–821–R–09–013) 

Delete entire section on Best Management Practices. 

Rationale: The use of Best Management Practices (BMPs) is not an analytical method and should not be 

included in EPA-821-R-09-013. The use of BMPs is an option for Operators to comply with the 

monitoring frequency requirements of the General NPDES permits GMG290000 or GEG460000, not an 

alternative to the test method itself.

Response: See response to Comment #31. 

(34) Original Comment Text: 

Table 1 of Appendix 8 of Subpart A of 40 CFR 435 

Revise Table 1 mud weight ranges as follows: 

8.5 – 11 

> 11 – 14 

>14 

Rationale: The table contains an apparent error/contradiction: as written currently, an 11 ppg SBM could 

be tested with the 9 or 11.5 ppg reference SBM. Adding a “greater than” sign in front of the 11-14 range 

clarifies the appropriate reference mud to use.

Response: EPA agrees with this error correction and clarification.