Response to Comments Document

for

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

March 20122010 Methods Update Rule Response to Comments i March 2012 Foreword

This document contains EPA’s responses to public comme nts 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 typogr aphical 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 me thods in the original proposal, most notably EPA Method 1668C, which was the subject of extensive comme nts. Therefore, this document does not contain responses to comments regarding Method 1668C. At su ch time as EPA makes a final determination on Method 1668C, the Agency will formally documen t 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 Method s Update Rule proposal cited above. A number of

detailed comments were received on this method. Th ese 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 Regi ster notice (76 FR 77742) for additional information

on this ASTM method.

The remainder of this document mirrors that of th e 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 doc ument, 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 th e EPA Docket website. Some comments have been aggregated as follows: comments supporting the additi on 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 suppor ting information in this document and notes that

fact at the end of each such comment.2010 Methods Update Rule Respons e 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 torc h 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 Me thod 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 Ve rsions of Approved Sta ndard 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 Assuran ce/Quality Control (QA/QC) ........................................................................... ........ 43

II.B.6 Alternate T est 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 Ve rsions 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 Te st Procedures (ATPs) .............................................................................. ............. 722010 Methods Update Rule Response to Comments iii March 2012 II.D.1 Hach Method 10360 ................................................................................................... ....................... 75 II.D.2 In-Situ Incorpor ated’s Method 1002-8-2009 ........................................................................... .......... 76 II.D.3 In-Situ Incorpor ated’s Method 1003-8-2009 ........................................................................... .......... 76 II.D.4 In-Situ Incorpor ated’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 instru ctions, 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 ......................................... 9 2 II.F.4 Revising Cyanide Sample Handling Inst ructions 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 Modi fication Provisions at 40 CFR 136.6 ............................................. 100

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

II.H.2 Use of Relative Standard E rror (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 ............................................................................... .......... 1552010 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, Jo int Virginia Water Environment Association and Virginia American Water Works Association Comment 166.1 - Paul Wiegand, National Counc il 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 comme nts regarding the method approval or withdrawal process as it applies to EPA methods, methods devel oped 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 co mments 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 b een approved in an attempt to reduce inconsistencies in quality assurance/quality control (QA/QC) practices across laborat ories. Alternate Test Procedures (ATPs) that were based on the older procedures are not being wit hdrawn because the approved ATPs refer to current

versions of Part 136 methods whic h have adequate QA/QC procedures. Older methods were withdrawn either because a procedural change was made th at 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 availabl e through several sources, including on the EPA web-site at: http://water.epa.gov/scitech/methods/c wa/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 ma ke them publicly available. They are generally available at the organization’s web-site for a fee.

Expanding the scope of the 600-Series methods deve loped for use in water monitoring programs to include compounds in the 8000-Series, which were de veloped 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 re garding method performance available when proposing new methods for the analysis of pollutants to allow the public to co mment on the proposed approval of these methods. In cases where updated versions of previously approve d methods are added, no new validation data are required, because the changes are editorial and do not a ffect 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 Met hods 614, 619, 622.1, a nd 632, EPA added these methods (previously included for Pesticide Active Ingred ients in Table IG) to Table ID for general use. As stated in the preamble to the proposed rule, th ese 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 additiona l validation data are needed to fu lly characterize the performance of

this method for various wastewater matrices.

EPA appreciates the commenters’ concern that con sensus methods should be subjected to the same validation required for nationwide approval of altern ate test procedures and will work with the VCSBs to

ensure that method validation data for new consensu s 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 a pproved 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 shoul d be allowed for this purpose. How will the EPA assure that the most curre nt version of an EPA required testing method or prescribed quality control and assurance step be ava ilable for view and use at federal repositories?

Comment 116.1 Wendy Harding and Mala Burton Joint Virginia Water Environment Association a nd 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 met hods 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 requireme nts 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 in2010 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 pub lish 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 Wh ich 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 wast ewaters 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 numer ous 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 requir es 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 regulat ed 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 fu lly 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 le vel of validation required in its own Alternate Test Procedure Program to the consensus methods. EPA s hould 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 validati on that it requires for nationwide approval of an alternate test procedure. Until that minimal valid ation is completed and ma de available for public comment, EPA should not add these methods to 40 CFR Part 136.

Comment 187 Peter Halpin Caltest Analytical Laboratory2010 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 ma ss 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 refere nces to mass spectrometers assume the use of mass spectrometry for confirmation when sensitivity allo ws. 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 primar y detector being a quadrapole mass spectrometer as opposed to an ECD, or NPD system. The current pr oposed 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 an d multiple reaction modes (‘triple quad’ for example)

as well.

II.A.1 Method 1664B and amending the RCRA regu lations 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 De partment of Health and Environmental Control Office of Environmental Laboratory Certification Comment 117.1 - Kelly M. Thompson, Wisc onsin 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 suppor ted the approval of Method 1664B, however, one commenter suggested that wording in the method allo wing 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 cons ider 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 a llowance to do alternate balance calibration checks is too vague. Two commenters expressed a desire fo r 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 an d 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 changi ng the definition is beyond the scope of today’s rule. Moreover, based on EPA’s substantial studies of this parameter th at 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 r esponse to commenters expr essing 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 th at 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 S ec. 1.7.1.5 of the method, blank subtraction has traditionally been an integral part of all EPA gr avimetric 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 balan ce 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 w ould need to be diluted and reanalyzed, or could allow the laboratory to report results to lower leve ls, 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 a dditional upper class “S” weight and/or a lower weight in order to bracket the expected final weighi ng value. In addition, in situations where more than 20 samples are analyzed per day, the frequenc y 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 H 2 SO 4 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 para meters as part of its changes to 40 CFR 136, yet falls short of being able to accept new methods th at include new technologies for Oil & Grease. MWWCA finds that the EPA's reasoning for not approv ing alternative test methods for Oil & Grease is contradictory to the Agency's "Summary" statem ent 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." Fu rther, 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 envi ronment where they live learn and work."

EPA has previously approved hexane extractable met hods for Oil & Grease, then reversed that decision because hexane was a hazardous solvent and required u se 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 mo st n-hexane waste is considered a RCRA hazardous waste by characteristic. According to the U.S. De partment of Labor, Occupa tional 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 th e 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 f ound 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 Ac t when approving test procedures for Clean Water Act permittees in 40 CFR 136. MWWCA believes that the fa ts, 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 onl y 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 m odifications is a helpful guide and we agree with most of the specific examples, with the exception of th e 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 sa mple 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 Envir onmental 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 a nd 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 shoul d 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 w ith method 1664B, we feel that there may be some benefit to establishing a sunset period for met hod 1664A. There is little difference between these versions. Many permits have been written to specifica lly reflect the use of 1664A. In addition, many certification programs certify by specific method. Wh ile 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, Wisc onsin Department of Natural Resources Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District Comment 169.1 - Judith R. Morgan, Amer ican Council of Independent Laboratories Comment 171.1 - Lola Guerra, Henrico County DPU

Summary of Comments: EPA proposed to approve EPA Met hod 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 r ecommended that EPA Method 200.7 be added to the list of approved methods for measurement of titanium a nd one of them stated that the method should be added to the list of approved methods for total ph osphorus 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 wastewat er since this method was originally developed for drinking water and stated that EPA Method 200.7, Re vision 5.0 should be finalized and approved instead, as it would be a more appropriate method for use in wastewater compliance mon itoring. 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 approve d 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 th e 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 th e 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 Secti on 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 develope d for different matrix types. The addition of EPA Method 200.5 as an approved met hod 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 met hod 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 rulemaki ng, 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 ax ial torch option is important in order to obtain the low detection and quantitation limits frequent ly required for wastewater analysis.

Comment 84.1

Scott Kuhn

Clean Harbors Environmental Services

Clean Harbors Environmental Services is the larg est 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 opera tions 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 limit ing and doesn't give the user any flexibility to use

alternative ICP methods that are available. At one Cl ean Harbors' location, there is only one laboratory in the area that is doing Method 200.8. Without additiona l alternative methods, the facility would be forced to use laboratories that are located significant distan ces 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 (a ttached) 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 me thods 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-establishe d as one of the backbones of metals analysis. However, it is not approved for NPDES compliance monito ring for some of the metals in its analyte list. I can well understand this when it comes to mercury, but I can’t understand w hy 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 sp ectral inferences. Please consider approving Method2010 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 eas ily be quantitated using Method 200.7 at levels appropriately low enough for NPDES complian ce 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 th e 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 be tter 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 sens itive and less bothered by spectral interferences from commonly occurring elements. Even though these two wa velengths aren’t mentioned in the method, the footnote to Table 1 of Method 200.7 states, “The wa velengths listed are recommended because of their sensitivity and overall acceptability. Ot her wavelengths may be substituted if they can provide the needed sensitivity and are treated with the same corrective techniques for spect ral 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 ap proved methods for phosphorus and titanium. Our laboratory has ATPs for both these analytes using Me thod 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—he re 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 torc h 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 (Deter mination 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 torc h 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 Me thod 200.7. When Method 200.7 was developed the2010 Methods Update Rule Response to Comments 10 March 2012 axial technology torch performance data was not ava ilable. 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 th e 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 shou ld 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. Howe ver, Method 200.5 and Method 200.7 are for different matrices and contain two very distinctive sets of cr iteria 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 enco untered in wastewater matrices. When analyzing wastewaters, lECs should always be used because th e concentrations and components of the wastewater matrix are variable and often largely unknown.

• Use of MCLs as action triggers and acceptance crite ria (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 inappropria te, at times meaningless and may jeopardize NPDES permit compliance.

• Laboratory Fortified Blank (LFB) and Laboratory Fo rtified 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 ca libration range and matrix spike concentrations are based on expected analyte levels. For analysis of lo w-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 concentrati ons 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 designat ed primary contaminants or MCLs. It is also unclear how or if the analyst is to appl y this requirement to the NPDES program.2010 Methods Update Rule Response to Comments 11 March 2012 • The acceptance range of 85%-115% for percent reco very of the LFM is much tighter than the 70%- 130% recovery found in Me thod 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 con centration of the LFB and should be taken into account. Methods 200.7,200.8 and 200.9 require the sa mple background concentration to be subtracted from the LFM, regardless of the concentration. Me thod 200.5 only allows subtraction of the sample background concentration when the sample con centration is >2.2xMDL. Again, the background concentration of the sample should be subtracted, rega rdless 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 tw o ICP methods, as well as other metals analytical methods, being used for the sa me program is imperative

Recommendation: In 2002, an EPA method validatio n 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 ge nerated from this study would be be tter 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 fo r 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 ne wer 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 to rch option is important in order to obtain the low detection and quantitation limits frequen tly 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 De partment of Health and Environmental Control Office of Environmental Laboratory Certification Comment 117.1 - Kelly M. Thompson, Wisc onsin Department of Natural Resources2010 Methods Update Rule Response to Comments 12 March 2012 Comment 169.1 - Judith R. Morgan, Amer ican 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 ingredient s. 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 s hould 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 pe sticide active ingredients for which Method 525.1 has been previously approved. EPA also appreci ates comments received regarding the substitution of

EPA Method 525.1 with EPA Method 525.2. At this ti me 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 addi tion 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 ru le. Additional comments were received regarding updating or expanding the 600-Series methods and these ch anges 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 liste d 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), Tabl e II takes precedence over information provided in approved methods. Therefore, if you are using Me thod 525.1 and 525.2 for Clean Water Act compliance monitoring of a pesticide active ingredient listed in Ta ble 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 holdi ng 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 De partment of Health and Environmental Control Office of Environmental Laboratory Certification Comment 117.1 Kelly M. Thompson, Wisc onsin Department of Natural Resources Comment 169.1 Judith R. Morgan, Amer ican Council of Independent Laboratories

Other comments:

Comment 94.1

Scott D. Siders Division of Laboratories, Illinois EPA2010 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 5 25.2 is a newer method and its analytical scope is broader. Method 525.2 also cont ains more updated analytical and QC instructions. Since all of the compounds in Method 525.1 are includ ed 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 Envir onmental Control Office of Environmental Laboratory

Certification

Table IC and ID include the methods for non-pestic ide and pesticide compounds respectively, Table ID now includes drinking water methods as approved for w astewater testing, Drinking water methods are not as applicable to wastewater analyses as SW-846 met hods due to sample matrices, The 600 series methods were created with now obsolete technology and ha ve 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 shoul d 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 met hods 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 requirement s 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, Wisc onsin Department of Natural Resources Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility2010 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, particular ly 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 met hods 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 comprehens ive 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 beviewed as disingenuous to the philosophy of moving technology and methodologies forward. The SW846 methodologies are more technically advanced, are upda ted with reasonable fre quency, 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 approvi ng 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 met hodologies 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 Jer sey Department of Environmental Protection Comment 117.1 - Kelly M. Thompson, Wisc onsin 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 me thods manual were more a ppropriate 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 Protection2010 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. Di scussions 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 nonconve ntional pesticide methods, which have been in use for more than 10 years, to Tables ID and IG for genera l 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-conven tional Pesticides in Municipal and Industrial Wastewater,’’ EPA 821–R–92–002, April 1992. Whil e 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 compendi um of methods published in SW-846 as well as other drinking water methods. In a sense, we strongly th e 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 upd ated 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 approvi ng 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 met hodologies 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, Wisc onsin 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 requ ested 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, updati ng 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 give n 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 met hods 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 comprehens ive 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 beviewed as disingenuous to the philosophy of moving technology and methodologies forward. The SW846 methodologies are more technically advanced, are upda ted with reasonable fre quency, 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 approvi ng 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 met hodologies 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 chlorpyr ifos. Chlorpyrifos is not a listed analyte in the CWA list of approved methods/analytes. Our regulator y agencies requested chlorpyrifos be included in the EPA 614 method. This method performs very well for th at analyte, but is not specifically listed. It would be helpful for the Clean Water Act to allow fo r 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 me thods 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 ru nning the EPA Method 617 compounds using the EPA Method 608 methylene chloride extrac tion 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, Wisc onsin 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 met hods 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 comprehens ive 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 beviewed as disingenuous to the philosophy of moving technology and methodologies forward. The SW846 methodologies are more technically advanced, are upda ted with reasonable fre quency, 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 approvi ng 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 met hodologies 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, Wisc onsin 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 me thods manual are more ap propriate 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 b ecome available which include an on-line automated derivatization step, it would be useful to have a path forward for usi ng 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 appr oved 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/m ethods/cwa/atp/atp_index.cfm to determine if the proposed ch anges 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 met hods 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 comprehens ive 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 beviewed as disingenuous to the philosophy of moving technology and methodologies forward. The SW846 methodologies are more technically advanced, are upda ted with reasonable fre quency, 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 approvi ng 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 met hodologies 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 tim e 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, Wisc onsin Department of Natural Resources Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District2010 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 express ed the desire to use conventional extractions as broadly as their performance allows, rather than separ ate, different extractions as in the case of Method 617 versus Method 608. A fifth commenter expr essed concerns about the use of Method 617 in pretreatment samples with a high organic solids conten t (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 flex ibility 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 co mpounds, today’s rule does not impose a requirement for the use of Method 617. If other methods approved at Part 136 ar e more appropriate for a given application (such as for samples with high organic solids conten t), 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 met hods 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 comprehens ive 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 beviewed as disingenuous to the philosophy of moving technology and methodologies forward. The SW846 methodologies are more technically advanced, are upda ted with reasonable fre quency, 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 approvi ng 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 met hodologies 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 he xane, 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 Me thod 608 and additionally m onitor for Perthane and Strobane (analytes from EPA Method 617). If EPA Me thod 617 is brought into the general use tables, then when analytes specific to that method are require d, 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 anal yses 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 exampl e, 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 me thods 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 ru nning the EPA Method 617 compounds using the EPA Method 608 methylene chloride extrac tion for informational purposes.

Comment 194

John Burnett Baltimore County, MD

I am deeply concerned about the proposed wholesal e 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 th e samples. There is no provision in Method 617 for any of the target analytes to account for the potenti al 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 possib ility 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 ch lorination (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 identify2010 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 anal ysis 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 wate rs that do not have the fl ora 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 roof top 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 trif luralin brought the attention of our state’s OSHA, and they asked me for information on methods for trif luralin. 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 tr ifluralin 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 conv ince 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, Wisc onsin 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, partic ularly those from the SW-846 methods manual were more appropriate and s hould 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 EPA2010 Methods Update Rule Response to Comments 22 March 2012 is being too restrictive in its approach. The met hods 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 comprehens ive 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 beviewed as disingenuous to the philosophy of moving technology and methodologies forward. The SW846 methodologies are more technically advanced, are upda ted with reasonable fre quency, 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 approvi ng 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 met hodologies 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, Wisc onsin 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 e xpressed concerns about the solid-phase extraction procedure in the method when the sample pa rticles 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 a pproved. However, other methods are approved for measurement of these compounds, and today’s rule do es 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 met hods proposed for addition are those as published in the 1992 publication, ‘‘Methods for the Determination of Non-conventional Pesticides in Municipal and2010 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 comprehens ive 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 reasona ble frequency, and have been used successfully in a variety of matrices, incl uding wastewaters, for many years. For example, how can the EPA consider approving methods 614 and 614. 1 for organophosphorus pes ticides, which have not been revised since 1992, yet not consider approvi ng 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 met hodologies 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 me thods 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 me thod 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 sens itive to interferences, especially to DeBDE. This method has not been fully validated, as only a single laboratory performance data is presented. The MDLs and MLs2010 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 reso lution 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 in cluded in the Methods Update Rule, EPA has decided to postpone consideration of Method 1668C until a la ter 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 De partment of Health and Environmental Control Office of Environmental Laboratory Certification Comment 166.1 - Paul Wiegand, National Counc il for Air and Stream Improvement, Inc.

Summary of Comments: One commenter noted that SM2540G for to tal, fixed, and volatile solids is not listed, but should be, in Table IB. A second comm enter expressed concern that these methods may not apply or do not perform as well in industrial wastewater s as they do in POTW effluents. That commenter submitted a technical report on the subject.

Response: The approved methods for solids assume total so lids 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 fo r 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 re garding the applicability of the methods and for providing the technical report of a study on the subj ect. 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 met hods have been approved or are available for use in wastewater. Permittees have the optio n of using any approved method for th e 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 Envir onmental Control Office of Environmental Laboratory

Certification2010 Methods Update Rule Response to Comments 25 March 2012 SM2540G, % total, fixed and volatile solids, is not lis ted in the updated Table IB. Because the biosolids procedures themselves are included in Table IA, Parame ter #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, me thods for Escherichia coli (E. coli) and enterococci produced widely varying results depending on which t echnique (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 wast ewaters, and those wast ewaters included in the validation studies conducted to support promulgati on 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 160 3) and enterococci (Methods 1106.1 and 1600) in surface waters and wastewater matrices, and for f ecal 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 mu ltiple well enzyme substrate methods are also approved for E. coli and enterococci measuremen ts. More recently, water quality-based permit limitations are being proposed for pulp and paper wast ewater discharges, although none of these methods have been validated using pulp and paper wastewater s. 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 a nd 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 hi gh variability among the various test methods. There

was no clear indication that one enterococci test me thod performed better than another when applied to pulp and paper wastewaters, but the results genera ted 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 a pproved methods for source identification of E. coli or enterococci involving pulp and paper final efflue nts could result in misleading conclusions and inappropriate water quality-based permit limitations.

II.A.8 Method 1627

No comments regarding Method 1627 were receiv ed. 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 De partment of Health and Environmental Control Office of Environmental Laboratory Certification Comment 117.1 - Kelly M. Thompson, Wisc onsin Department of Natural Resources Comment 123 - Vincent Sapienza, New York City Department of Environmental Protection2010 Methods Update Rule Response to Comments 26 March 2012 Comment 169.1 - Judith R. Morgan, Amer ican 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 th at 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 requireme nts 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 a bout 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. Sampl es 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 th e 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 di fferent preservation and holding time for these two analytes and submitted data in support of their asserti on 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) accepta nce 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 car te blanche approval of this method for these two analytes, EPA agrees that caution must be exercisedbecause EPA has not conducted an extensive multilab study. However, EPA supports th is change because many laboratori es have had experience with the

use of Method 624 for the determination of these two analytes and the Agency desi res to provide them the flexibility to use this method provided the labor atories 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 quantita tive determination of acrolein and acrylonitrile, provided that the laboratory has documentation to su bstantiate the ability to detect and quantify these analytes at levels necessary to comply with any asso ciated regulations, and i ndicating 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 Me thod 625 for analysis of benzidine, hexachlorocyclopentadiene, N-nitrosodimethylamine, and N-nitrosodipheny lamine, first appeared in 1984. The footnote2010 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 co mpliance if it continues using EPA Method 625 as the quantitative method for these compounds if other analy tical 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, Amer ican 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 in cludes acrolein and acrylonitrile and other volatiles, this also means that samplers must take two sets of samp les and the lab must analyze the samples twice. This all represents added sample bottle, documentation, sa mpling, 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 fo r additional compounds, including acrolein, acrylonitrile, benzidine, hexachlo rocyclopentadiene, N-nitrosodimethylamine, and Nnitrosodiphneylamine. This is a reasonable propo sal; however, there are no published QC acceptance criteria in the methods for these compounds. Will the lim its 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 a nd 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 re gulatory 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 est ablished in the facility’s laboratory or 625 is specified in their permit.

Comment 98.1 URS Corporation2010 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 acrolei n 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 pr eserving 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 th e 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 unpreserve d 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 preser ved 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 w ith HCl to pH<2 and analyzed within 14 days. We do agree with EPA on submitting an unpreserved sample for the analysis of 2-ch loroethyl vinyl ether.

Comment 113.1 - Susan E. Butts, South Carolina De partment of Health and Environmental Control Office of Environmental Laboratory Certification

Section II.A.9 discusses the removal of footnote 4 for Me thod 624, We are in agreement with the removal of this footnote, EPA Method 8260B has been used fo r years to analyze acrolein and acrylonitrile with no confirmation, Since EPA Method 624 has the same t echnology and analytical procedures as EPA Method 8260B, enough data has been generate d 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 th e compounds acrolein and acrylonitrile, we feel that offering a carte blanche approval at this time is premat ure. It appears from the summary that the removal of the screening restriction for these two analytes st ems from comments made by a single laboratory, rather than a more rigorous multi-laboratory testing st udy. We do not deny that some laboratories are capable of producing quantitative results of acceptabl e quality for acrolein and acrylonitrile using EPA method 624. It is our experience, however, that this is only possible using specific modifications to the2010 Methods Update Rule Response to Comments 29 March 2012 method, which should be required to be employed s hould a lab wish to use method 624 to produce quantitative results.

SW-846 method 8260B (1996), a much more recent vers ion of this GC/MS method, clearly specifies that these two analytes are associated with poor purging e fficiency. 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 fo r general quantitative determination of these two analytes, we believe that performance criteria, including sample introducti on technique, should be specified in a footnote to table IC. One suggestion would be to add the followi ng language to the proposed revision to footnote 4 in Table IC: Method 624 may be used for quantitativ e determination of Acro lein and Acrylonitrile, provided that the laboratory has documentation to su bstantiate the ability to detect and quantify these analytes at levels necessary to comply with any asso ciated 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 Wastew ater Treatment, New York City Department of

Environmental Protection

Summary of Comments: Many commenters supported EPA’s pro posal to limit the approved versions of Standard Methods to the most recent versions, altho ugh 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 suppor t. 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 lim it 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 Wast ewater Treatment, New York City Department

of Environmental Protection2010 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 C ounty Water and Sewer Department Regulatory Compliance Team Comment 99.1 - Jennifer Marques, Li nden Roselle Sewerage Authority Comment 113.1 - Susan E. Butts, South Carolina De partment 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, Milw aukee Metropolitan Sewerage District Comment 161.1 - Carol Batterton, Wate r 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 c oncern 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 manageri al 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 electroni c format at the discretion of the Standard Methods staff. Charges for these methods, whether in prin t 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 sensitive2010 Methods Update Rule Response to Comments 31 March 2012 to comply with the permit limit. EPA is not requi ring 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 do wnloaded from the web site and saved “locally” to a computer or network at the laboratory. The local PD F 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 c onclude that this change will present a significant

financial burden to laboratories.

Thus, EPA disagrees that more than one “seat” (subscr iption) 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 r ecent" 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 co sts $295). Although newer editions have newly revised quality assurance and quality co ntrol procedures, the use of the da ta should be balanced against the need for greater accuracy. Newer QA/QC proce dures do not always correspond to increased accuracy and even if the procedure increased accuracy minimall y, would it justify the need to spend money on new procedures verses spending on a worthwhile expendi ture 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 la boratories 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 additio n 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 approvi ng versions from the 18th, 19th, 20th, or online compendia. While this is a considerable simplificat ion 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 being2010 Methods Update Rule Response to Comments 32 March 2012 performed in their laboratory comports with the appr oved 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 Depart ment 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 th e same access multiple time s versus a more cost effective hardcopy version that is approved and usef ul over many years. We found that hardcopy editions were currently used for this reason by all of the ot her 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 a nd make available the changes sin ce 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 av ailable to those having purchased hardcopy SM editions some cost effective way to access the update d 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 ve rsion of a method published. Many of these methods

will be from the 21 st On-line edition of Standard Methods. As stated on the Standard Methods Committee website, www.standardmethods.org, access to the 21 st 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 beco mes 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. Inte rnet access may be only for the supervisor and not the laboratory technicians. Requiring the laboratory t echnicians to access the met hods online would result in a need to purchase additional computers for the labor atories 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 21 st 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 Envir onmental Control Office of Environmental Laboratory

Certification2010 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 subscr iption to Standard Methods to review the methods on-line. This is cost prohibitive for state certificati on 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 effec tive 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 Met hods 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 la boratory or wastewater facility to purchase a new version of Standard Methods on what would be potentia lly 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 la test edition is both an inefficient use of resources as well as a source of potentially frivolous litigation ov er the semantics of which edition is used. This would also lead to confusion over when a given la b 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 ava ilability 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 decr eased QA/QC method requirements, for example) this

would either force the EPA to allow an undesirabl e 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 la boratory or facility to refer to the most recent (approved) 40 CFR that outlines in table format wh ich source method editions are considered acceptable.

Comment 152.1

James Matthews On Line Environmental Inc (OLE)

We are also concerned about the requirement to u se only the most recently approved methods approved by the Standard Methods Committee, as discussed on pa ge 58028-9 of the proposed legislation. While

we understand the desire and need for consistency, being able to only re ference 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 certifi cate 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 certif ication for the laboratory with each revision as it is implemented? This could mean substantial backl ogs for states issuing certifications. Additionally, once2010 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 pro cedures, 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 fo rce the need for each lab to implement a LIMS system or require a

substantial increase in labor. For labs with limite d budgets, this monetary co mmitment 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 versi on 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 ev ery 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 requ ired specifications and there may be little, if any, improvement in data quality for the intended use. Me thod 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 i nvestments 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 la bs to use the best available methods as appropriate. This should not be regulated. EPA should approve methods by refe rence and technology but not by version or date. EPA could and should encourage the u se of the most recent version, however, the use of an earlier approved version should also be allo wed 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 approve d 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 compendium s, 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 publishe d by the Standard Methods Committee (e.g., Standard Method 2320 B–97). In some cases, EPA has approve d more than one version of a Standard Method. Approval of several versions of th e same Standard Method has led to in consistencies in how laboratories conduct these analyses especially in quality assurance/qua lity 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 dig its 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 me thod in the 21st edition of Standard Methods, you must follow the Quality Control requirements of the 21st editi on. For consistency, most labs utilize the same2010 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 wh ich 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 ve rsion of a method is usually on-line years before they are published in hardcopy. The least expens ive 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 prin ted versions of Standard Methods more frequently

and/or subscribe to the online version of Standa rd Methods. The proposed tracking requirements may force the need for each lab to implement a L1MS sy stem 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 met hods 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 onl y available online via www.StandardMethods.org which requires a costly online membership. Annua l membership fees start at $295 and increase based on the number of users needing access. Our 5 member la boratory would cost $495 per year just to have access to method texts and updates. As proposed, th ese method revisions would be approved as soon as released and therefore require immediat e compliance within the laboratory.

No other approved method source requires such outrage ous fees for cited method texts. Why would the Agency indiscriminately approve met hods 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 labor atory 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 regulat ory 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 C ounty Water and Sewer Department Regulatory Compliance Team Comment 113.1 - Susan E. Butts, South Carolina De partment of Health and Environmental Control Office of Environmental Laboratory Certification Comment 117.1 - Kelly M. Thompson, Wisc onsin Department of Natural Resources Comment 124.1 - Thomas Tourje, Augusta County Service Authority2010 Methods Update Rule Response to Comments 36 March 2012 Comment 134.1 - Josh Kathrinus, American Bo ttoms 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 manua l, 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 ve rsion of a given method and the effects of the different method identification systems on various asp ects 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 rulema kings. For example, Standard Methods are identified by the year in which they were “approved” for public ation by the Standard Methods consensus body (e.g., SM 3113-2004 was approved by the Standard Method s Committee in 2004). The year of approval by

Standard Methods is retained until the method is re viewed (and potentially revi sed). 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 cha nge 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 "approv es" the method. However, “approval” by that committee does not reflect any regulatory significan ce at part 136 or elsewhere. The Agency must propose any updated version of a Standard Method in th e Federal Register and provide the opportunity for public comment on the updated version before the met hod is approved at part 136 for use in wastewater regulatory programs.

If the version of a Standard Method that EPA has “ap proved” for use in compliance monitoring and listed in part 136 was “published” by Standa rd Methods at a later date than the version in the most recent hard copy edition of Standard Methods that you have, yo u may need to purchase that method from the on-line version of Standard Methods, at a cost of $69 per me thod. The hard copy edition generally lags and is not available as quickly as the on-line version. Methods ma y be purchased individually for less than the cost of a full subscription to the on-line service or of th e most recently published print edition of Standard

Methods.

The Standard Methods committee has taken additiona l 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 Met hods Committee. . .by listing only one version of the method with the year of publication designated by th e 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 a2010 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 paramete rs (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 versi ons 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 ha ve 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 B OD 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 Depart ment Regulatory Compliance Team

BCWS commends the United States Environmental Protec tion 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 con cerns 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 betwee n 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 refe rence 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 assu me 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 Envir onmental Control Office of Environmental Laboratory

Certification

Section II.B, Tables IA, IB, and IH address the appr oved 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 in consistencies across the laboratory community. It2010 Methods Update Rule Response to Comments 38 March 2012 also causes problems with the certification of laborat ories since each method may vary between editions and we must evaluate laboratories according to th e edition they are referencing. The approval of one approved Standard Method for each parameter will he lp solve the inconsistenc ies between laboratories

and will aid in the certification of laboratories in be ing able to hold the laboratories to one approved method. Also, it is our understanding that when Sta ndard Methods issues a new revision of a method, it contains improvements to the method. However, th ere are two comments we would like to make in regards to this change:

a) The method should not be listed with a 4 digit y ear, e.g., 2006, Instead, the Standard Methods should be listed with the last two digits of the approval y ear, e.g., 06, This will provide consistency with Tables IC and ID for organics which only list the last two di gits 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 ph enol 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 improve ments unnecessarily increases costs to all laboratories and regulatory authorities when there is relativ ely 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 Met hods 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 codifi ed reflect the “year of publication”. In the example above, “1997” would indicate the year of publicati on. 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 assessm ent of the proposed rule suggests that the “year”, as discussed in rule, actually reflect s 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 subscriptio ns, poses a significant financial burden to smaller regulated facilities, it seems reasonable that end user s should be able to quickly ascertain whether the copy of a particular method they own in a publishe d edition of Standard Methods reflects the identical method approved in 40 CFR Part 136. As an exam ple, 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 ha rd copies of Standard Methods 19th (published 1995) and 20th (published 1998) editions a nd 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 compar ed to the version in the 20th edition, however, one finds they are identical. The analyst should th en 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 coul d 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 appr oved 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 vers ions listed for a single method. In addition, the version of the method is not viewable at the link, rath er it is found in the footers of the pdf file after maneuvering through the SM website and downloading th e pdf. This is true for BOD, temperature and

chromium at least. This could be a cause for conf usion 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 rath er 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 publicati on 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 publicati on date will impact data management systems, accreditation data bases, PT provider data re porting systems, and regulatory programs.

Recommendations

For Standard Methods, cite methods based on editio n number and date and clearly associate the QA/QC section required for each method. Recommend to Standa rd Methods consensus body to include QA/QC requirements within cited methods.

Comment 189.1 William Ray

California State Water Resources Control Board2010 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). Howeve r, 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 w ill 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 versi on, 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, Jo int 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 suita ble 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 publi cation 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 th at 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 au tomatically approve future updated versions of the methods once the Standard Methods committee approv es a new version or if only the specific version listed in Table IA or Table IB is approved. Will la boratories 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 a ny and all corrections and description revisions made to methods published in th e "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) be lieves 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 ye ar, and other method references, including Quality Assurance and Control requirements?

Many, if not most, municipal and publicly owned tr eatment works (POTWs) that do self-monitoring use methods published in "Standard Methods for the Exam ination 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 "rep ublished" independently by the Standard Methods Committee, as published "online," even after the pr oposed rule is final. Will permittees and other laboratories performing permit required monitoring, using EPA approved "Standard Methods," be expected to purchase subscriptions to "Standard Me thods Online" (at $295 per year per seat) to meet

EPA's definition of current?

If EPA is indeed planning to approve "online" vers ions 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 particip ation and freedom of assembly, and also be a great burden of cost to many small entities. Allowing u se of independently update d methods would require expensive subscriptions to an online service or other t ypes of constant vigilance in trying to determine what EPA has approved as "current."

We believe that the EPA must assure the public's ri ght 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 ch anges 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 fa ll only on direct dischargers, but also on indirect dischargers subject to the National Pretreatment Pr ogram. 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 re view 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 me thod was used and that all necessary current quality control and assurance was done? As of today, pretr eatment 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 belie ves that EPA approval of2010 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 availabl e, 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 A ssurance (DMR-QA) study program.

As discussed in another part of our comments, mo st municipal and publicly owned treatment works (POTWs) that do self-monitoring use methods publishe d 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 "re published" independently by the Standard Methods Committee, following publication of the final rule. If th is 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 chang es 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 a nd Virginia American Water Works Association

Proposed Change: “For this reason, EPA is propos ing 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 approv es 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 auto matically approve future updated versions of the methods once the Standard Methods committee approv es 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 ru le, 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 pro posal that EPA desires to approve any and all corrections and description revisions made to the me thods 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 compilati on 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 propos ing 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 approv es 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 auto matically approve future updated versions of the methods once the Standard Methods committee approv es 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 Progr am Manager, REI Consultants, Inc. Comment 106.1 - Charles Boepple, Upper Occoquan Service Authority Comment 116.1 - Wendy Harding and Mala Burton, Jo int 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 Authority2010 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 reco mmended 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 appl icable QA/QC requirements, beginning with the publication of the 20 th edition of Standard Methods, the St andard 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 fo r 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 “essentia l” quality control checks that have been added at 40 CFR part 136.7 as part of this final rule (see Secti on II.I of this document). To improve consistency, laboratories performing any of the approved Standard Methods should adopt the QC procedures specified

in the 20 th or 21 st edition of the hardcopy Standard Methods or in the on-line version of Standard

Methods. These versions of Standa rd 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 onl y these later versions will lead to confusion because the new approach clearly identifies the version of the standard appr oved 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 Meth od followed by the year of publication to be very burdensome in deciding the appropriate QC to matc h with each method. Each version of Standard Methods has improved upon the QC/QA practices. But wh en 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 (whi ch 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 Standa rd 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 di fferent Part 1000 sections th at 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 Burton2010 Methods Update Rule Response to Comments 45 March 2012 Joint Virginia Water Environment Association a nd Virginia American Water Works Association

Part 1000 of Standard Methods (whi ch covers many QA/QC subjects) does not have an “approval date”

tied to it. Since the methods in tables IA and IB incl ude methods that were first released in either the 20th, 21st, or on-line versions of St andard 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, require ments 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 covere d in 3111A 7 with recovery and precision limits in Table 3111: III. Paragraph 7 lists an acceptabl e recovery as 85-115% as in 3020; however the table which is from ASTM (with permission) gives speci fic ranges for each individual metal ranging from .4- 12.5%. Also, only 17 metals are listed. Additionall y, 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 (whi ch covers many QA/QC subjects) does not have an “approval date”

tied to it. Since the methods in tables IA and IB incl ude methods that were first released in either the 20th, 21st, or on-line versions of St andard 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 rath er than Standard Method edition number. Some approved methods are currently not available in ha rd 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 complica tions relating to laboratory accreditation.

Currently laboratories use, report data and are accr edited 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. Th erefore it is unclear which QA/QC requirements are2010 Methods Update Rule Response to Comments 46 March 2012 to be followed. On-line Methods and QC sections ar e 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 Meth ods publishes methods. Currently, there is no clear mechanism to track publish date to source or cl ear requirements for QA/QC for all methods.

Recommendation

For Standard Methods, cite methods based on editio n number and date and clearly associate the QA/QC section required for each method. Recommend to Standa rd 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 th reatens to do just the opposite. EPA’s assumption that each successive modification of a particular Sta ndard Method carries with it legitimate and justifiable QA/QC measures is presumptive and shortsighted.

The necessity for standardized methodology both in th e laboratory and between them is clear, however such consistency should be mandated in a more simp listic 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 measur es 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, Jo int 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 contra diction in how Standard Methods and ATPs are

handled.

Response: Withdrawal of the earlier approved versions of St andard Methods is not intended to affect the acceptance of any vendor-developed me thods that were previously dete rmined to be acceptable versions

of those methods. Such Standard Methods were not w ithdrawn due to technical deficiencies. Rather, the Standard Methods were revised to impr ove clarity, increase method flexibility ( e.g ., use of a different solvent), or improve QC procedures, but the underlying technology was not changed. Therefore, the basis2010 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 th at will no longer be listed in 40C FR 136 continue to retain EPA approval for regulatory monitoring?

Recommendation 2: Please confirm that the commercia lly 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 a nd 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 re tain EPA approval for regulatory monitoring?

Recommendation 2: Please confirm that the commerc ially available ATP methods which are based on earlier, withdrawn methods are still approved.

Comment 3: If commercially available methods a pproved under the ATP progr am 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 number s 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 comm unity will understand all the available methods for regulatory monitoring.

Comment 132.1 Paula Hogg Hampton Roads Sanitation District2010 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 de emed "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 se tting 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 co nsistent 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 CF R Part 136 methods and 2) evaluation of method suitability through a defined process which includes in tra-laboratory and inter-lab oratory validation data, peer review and laboratory comments, selectivity of the methods for the parameters in question, applicable linear dynamic range, defined sensitivity, a nd 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 define d. 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 Revi ew 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, unacc eptable uncertainty in their effectiveness. Since methods have been updated to the latest versi on 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 s till considered equivalent by EPA.

Questions include:

• Since the previous letters referenced older vers ions of the approved methods, will vendors need to obtain updated letters from EPA and have info rmation 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 Cl ean 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 eith er of two approaches: I) EPA can generate this information after standard setting bodies have comp leted their internal processes of method development or 2) EPA can require standard setting bodies to co llect 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 164.12010 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 co mparing 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 diffe rent 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 lis ted 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 vers ions of the approved methods, will vendors need to obtain updated letters from EPA and have info rmation 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 Cl ean Water Act monitoring?

Recommendations

• Allow all currently approved versions of Sta ndard 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 equiva lent 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 AT P approval and are based on earlier versions of a Standard Method that will no longer be listed in 40CFR136 continue to re tain EPA approval for regulatory monitoring?

Recommendation: Please confirm that the commercia lly 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., 18 th2010 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 Examinat ion of Water and Wastewater. The proposed rule, through the use of dates within the approved t est method number removes the 18th Edition from the approved list. This will place local governments in a s ituation where full compliance is impossible. They

will be in violation of 40 CFR 503 or 40 CFR 136. Th ere 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 th is technique, specifically naming the test specified by the 18th Edition

of the Standard Methods for the Examination of Wa ter and Wastewater. WADC respectfully requests the

addition of Method 2540G and other methods that ar e 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, Jo int 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 o ccurring on a routine basis for the existing approved2010 Methods Update Rule Response to Comments 51 March 2012 methods ( e.g ., any laboratory’s quality system requirement s 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, regardl ess of this rulemaking. EPA anticipates that such state programs will allow some time period for comp lete implementation of any method changes resulting from today’s action. Given the diversity of the stat e 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 certifica tion agencies may require laboratories to resubmit applications, repeat PT studies, perform new Demonstr ations of Capability, MDL/PQL studies, etc. to maintain certification, which will be a si gnificant economic burden on laboratories.

Recommendation 6: Provide clear guidance to states and accrediting authorities regarding what should be required in this area for laboratori es 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 me thods and any associated additional QC requirements (e.g. new PT samples, Demonstr ation 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 a nd 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 pr oposed 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 significan t economic burden on laboratories.

Recommendation 6: Provide clear guidance to states and accrediting authorities regarding what should be required in this area for laborato ries 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 me thods 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 laborat ories sufficient time for re-writing methods, personnel training, participation in appropriate PT studi es, 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 appr oved methods coming from each of the 18th thru 21st additions, each with their own separate and differi ng QC requirements? Why are some methods published by Standard Methods show ing approval for 20th Ed, while othe r methods show approval in the 21st? Table IB (55) for TSS shows a referen ce 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 resubm it 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 la boratories 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 me thods 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 laborat ories sufficient time for re-writing methods, personnel training, participation in appropriate PT studi es, and other quality assurance requirements.

Comment 130.1

Heather L. Beard Richland County Utilities

We are also concerned about the requirement to u se only the most recently approved methods approved by the Standard Methods Committee, as discussed on pa ge 58028-9 of the proposed legislation. While

we understand the desire and need for consistency, being able to only re ference 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 certifi cate 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 certif ication for the laboratory with each revision as it is implemented? This could mean substantial backl ogs 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 pro cedures, 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 fo rce the need for each lab to implement a LIMS system or require a

substantial increase in labor. For labs with limite d budgets, this monetary co mmitment 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 132.12010 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 complica tions relating to laboratory accreditation.

Currently laboratories use, report data and are accr edited 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. Th erefore it is unclear which QA/QC requirements are to be followed. On-line Methods and QC sections ar e 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 Meth ods publishes methods. Currently, there is no clear mechanism to track publish date to source or cl ear requirements for QA/QC for all methods.

Recommendation

For Standard Methods, cite methods based on editio n number and date and clearly associate the QA/QC section required for each method. Recommend to Standa rd 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 di scussed on page 58028-29 of the proposal document.

While we understand the desire and n eed 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 cer tification certificate. The requirement to use only the most recently approved method would also require reissuance of the lab certif icate for each revision. Would this require reapplication for certificati on for the laboratory with each revision as it is implemented? This requirement c ould mean substantial backlogs for states issuing certifications.

Comment 164.1 Mark Haley Hopewell Regional Wastewater Treatment Facility

Approved methods are listed by publication date rath er 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 publicati on 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. Changing2010 Methods Update Rule Response to Comments 54 March 2012 40CFR citations from edition number to publicati on date will impact data management systems, accreditation data bases, PT provider data reporting sy stems, 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 editio n number and date and clearly associate the QA/QC section required for each method. Recommend to Standa rd 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, Jo int 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, Pennsylvani a 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 micr obiological 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. Si milar 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 co mmenters 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-lin e. 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 approve d these methods after publication of the 21 st edition and will be published in the 22 nd 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, and2010 Methods Update Rule Response to Comments 55 March 2012 Enterococci by SM 9230 B-2007 and SM 9230 C-2007 are th e latest available versions and are correct as proposed.

With regard to SM 5530 C not being listed in Ta ble IB as an approved method for phenols, SM 5530 B

and D were added to Table IB in the 2007 Met hods Update Rule to repl ace 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 de scription of parameter 48 in Table IB for Method 420.1 previously read “Phenols, mg/L: Manual distillati on, 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 procedur e is necessary to achieve greater sensitivity for specific discharges, the regulatory auth ority 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 ne w color procedure (spectrophotometric-single wavelength) that replaced the previous 20th edition ve rsion of SM 2120 C (which is not approved at 40CFR 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 spect rophotometric method) as well as the main ADMI procedure. With the 21st edition, the “alternate met hod” became SM 2120 F, but the main procedure in the earlier version of 2120 E was dropped. It was b ecause 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 tig hter 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 th e most recent version of the method were the result of careful deliberations by a group of experts a nd 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 521 0 B-2001 requires calculation of the relative percent difference (RPD) across samples from different diluti ons. An electronic search of the method found no occurrences of either “RPD” or “relative percent differe nce” in the entire text of 5210 A through 5210 D.

The reporting section of SM 5210B-2001 states “S amples 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 e ffect becomes repetitive, in vestigate to identify the cause.” However, the 30% metric is the “percen t 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 an alyst should investigate th e 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 criteri on comments, EPA is appr oving SM 5210 B-2001, and withdrawing approval for the 20th ed ition 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 im pacts 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 requirement s 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 measure ments. Duplicates should be required in order to measure precision and analyst observa tion on dilution differences can be u sed 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 dilutio ns 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 am ounts of solids. It is possible to have variability between dilutions that is not due to toxicity or analyt ical 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 EP A 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 Elliot2010 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, Anti mony, Arsenic, Barium, Beryllium, Cobalt, Copper, Gold, Manganese, Molybdenum, Nickel, Selenium, Tha llium, Tin, and Vanadium are listed with the 2004 revision. Cadmium, Chromium, Iron, Lead, and Silv er are listed with the 1999 revision. There should only be one revision for all metals.

In Table IB, Parameter #48 Phenols, SM 5530B an d 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 phe nol determinations? The chloroform extraction procedure is still included in EPA Method 420.1. Pl ease 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 equivale nt to SM 2120E. Will NPDES permits be allowed

modifications to move from the ADMI method to an a lternative 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 le tter 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 a nd Virginia American Water Works Association

Proposed Change: Addition a nd 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 pe er-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. Th e 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 (colorim etric). 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 pe er-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 C ouncil for Air and Stream Improvement, Inc.

Summary of Comments: One commenter raised concerns that were not readily characterized in the other subsections regarding the Sta ndard 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 AT P 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 a ll Standard Methods or other VCSB methods to

extensive validation. Standard Methods are re vised 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 met hod, it often works with the developer of the

method and the VCSB to ensure that validation effort s are appropriate for wastewater matrices subject to the Clean Water Act. EPA encourages the method de veloper 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 conti nue to evaluate the validation st udy data available for any newly2010 Methods Update Rule Response to Comments 59 March 2012 developed methods considered for rulemaking in the fu ture 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 subj ect to the Clean Water Act. Therefore, in considering new methods from any source, EPA examin es the available validation data for representative wastewater matrices, just as it does for ATP applican ts. EPA finds that ATP applications often represent vendor-specific methods with wide application across re gulated 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 wast ewaters 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 numer ous 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 requir es 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 regulat ed 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 fu lly 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 le vel of validation required in its own Alternate Test Procedure Program to the consensus methods. EPA s hould 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 C ouncil 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 cy anide. Another commenter expressed concerns about2010 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 va riety of industries subject to NPDES regulations.

Response: EPA approved new cyanide methods to allow dischargers and their laboratories to address potential positive and negative interfere nces 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 regardin g the nature of the samples to be analyzed. Information about the regulatory permit limits for any po llutant, 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 me thods 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 la boratories 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 perfo rmance, 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 met hods from ASTM, mostly for various forms of free, available, and total cyanide using a variety of inst rumental approaches. As mentioned later, cyanide testing is complicated due to the number of potentia l positive and negative interferences and the various ways to try to address these interferences. By si gnificantly 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 numer ous 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 regul ated in the NPDES program. If a regulated entity or2010 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 full y 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 leve l of validation required in its own Alternate Test Procedure Program to the consensus methods. EPA s hould 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 speci fic wastewaters such as those from pulp and paper manufacturing. EPA should limit the scope of each me thod approval to those wastewater matrices for

which method validation and detection limits studi es 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 intende d 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 complex es. However, these new free cyanide methods use the same determinative steps as methods for determin ing 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 th e 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 NP DES 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 validat ed 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 stud y 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 eliminat e interferences and different sample preservatives were noted to have significant effects on sample vari ability and detection limits for a variety of methods when applied to pulp and paper wastewaters. Althoug h 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 pr ocedures being proposed for approval were not included in NCASI’s evaluations, so extensive a dditional work would be needed to demonstrate equivalence with the current distillation proce dures, determine detection limits, assess potential interferences, and evaluate performance using th ese 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 en sure 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 applicab ility 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, Amer ican Council of Independent Laboratories

Summary of Comments: Three commenters supported the addition of these methods.

Response: EPA appreciates the commenters’ support a nd 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, Amer ican 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 C ounty Water and Sewer Department Regulatory Compliance Team Comment 153.1 - Debbie Webster, Cent ral Valley Clean Water Association Comment 169.1 - Judith R. Morgan - Amer ican 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 a nd it is including the method in the final rulemaking. EPA also appreciates the thoughtful pres entation 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 entr ies 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 °C 18 , 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 implem entation. 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 au thority is responsible fo r 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 me thod 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 , Amer ican Council of Independent Laboratories

Other comments:

Comment 95.1 Robert B. Leventry Butler County Water and Sewer Depart ment Regulatory Compliance Team

FR pages 58030 and 58031 In the pr eamble 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 appear s to require an immediate switch to the new method upon promulgation. This may not allow local labor atories 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 paramete r 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 rela ted 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 T oxics Standards for Inland Surface Waters, Enclosed Bays, and Estuaries of California (SIP) establishes pr ocedures 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 dom inated water bodies often receive average monthly effluent limits for cyanide as low as 4.1 μg/L. Consis tent compliance with this limitation is problematic, and numerous Central Valley POTWs employing secondary and tertiary treatment systems with chlorine2010 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 spectrophot ometric 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 a nd bias, particularly in complex matrices such as

POTW effluent.

The attached document Problems Associated w ith Using Current EPA Approved Total Cyanide Analytical Methods for Determining Municipal Wast ewater 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 objectiv e exceedances. Sodium hydroxide-related bias is recognized by experts in cyanide analytical chemistr y, 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 cyanid e 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 cyanid e 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 th e 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 a lternative 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 la test procedures detailed in ASTM D7365-09a. For this reason, we strongly support the regulatory flexib ility afforded by dealing with the local permitting authority in developing analytical fixes where inte rference and bias is involved. Furthermore, the possibility of utilizing an analytical method that meas ures the portion of cyanide that is truly bioavailable is needed and, therefore, we support inclusi on of the proposed “free” cyanide procedures.

Although our CVCWA membership is limited to the Cent ral 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-re lated 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 De partment 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 ru le, EPA added language to th e 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 fo r 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 ot her ASTM dissolved oxygen methods in a future rulemaking.

Original Comment Text:

Comment 113.1

Susan E. Butts South Carolina Department of Health and Envir onmental Control Office of Environmental Laboratory

Certification

ASTM Method D888-09 is listed as an approved bi ochemical 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 B OD 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 laborator ies are the acceptance of

the ASTM D888-09 Part C luminescence-based detecti on 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, Jo int 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 C ouncil for Air and Stream Improvement, Inc. Comment 169.1 - Judith R. Morgan, Amer ican Council of Independent Laboratories Comment 180 - Philip Yee, The Dow Chemical Company2010 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 procedur e uses the same instrumentation and materials as Method 625, and thus Method 625 also should be ap proved for these analytes. Two other commenters expressed concerns about ASTM D7065-06 and the l ack of validation data for specific industry

wastewater matrices. One commenter also noted th e lack of holding time a nd preservation requirements for the analytes in question. One co mmenter expressed concern that one of the surrogates described in the method is sometimes a target analyte.

Response: EPA thanks those commenters’ supporting th e 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 th e commenters. Absent a requirement for analysis of the five new analytes in every sample, laborator ies 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 considerati ons relevant to these analytes. Th e 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 a dding these analytes to Method 625. Furthermore, expanding the applicability of Method 625 to additi onal analytes is outside the scope of today’s rulemaking. If a laboratory/permittee wishes to use Me thod 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 laborator ies using reagent water and substitute wastewater prepared according to ASTM D5905. Substitute wastew ater 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 comp lex than reagent water. Substitute wastewater is

intended to be used as a material to be spiked with analytes or interfer ents of interest to evaluate the performance of test methods.

Utilization of substitute wastewater as a matrix in in terlaboratory 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 applicati on 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 represen tative 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 th e method for a specific matrix, the laboratory should

evaluate the method for that matrix or use a differe nt method that may be more appropriate for that

matrix.

With regard to the difficulties in making measuremen ts at the “part-per-quadrillio n” 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, H 2 SO 4 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 in terest, 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 th e 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, Amer ican Council of Independent Laboratories

Other comments:

Comment 116.1 Wendy Harding and Mala Burton Joint Virginia Water Environment Association a nd 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, accredita tion application, method validation, thus incurring significant additional costs to maintain capability. Fu rthermore, additional hazardous waste is generated. These additional costs are passed onto data user s 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 additi on to the inclusion of the proposed ASTM method to the Method Update Rule, EPA should to allow for th e 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 refe renced for these compounds requiring laboratories to use a separate method, develop a separ ate 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 are2010 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 Met hod 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 Met hod 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 u se is inappropriate because they have not been

validated for use with certain wast ewaters 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 tr eatment 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 matr ices until validation studies have been conducted.

Comment 180 Philip Yee The Dow Chemical Company

The Federal Register proposal further stated that th is 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 throu gh 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 c ited 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 w ill result in numerous difficulties for the regulated community to utilize this method and evaluate co rresponding 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 samp les at the part per quadrillion level, as presented in the method document. Section 5 contains many le ngthy required processes required to maintain the laboratory for this level. This w ould 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 testi ng at these low part per quadrillion levels may not yield meaningful results. The value of testing at these lo w 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 C ouncil for Air and Stream Improvement, Inc. Comment 169.1 - Judith R. Morgan, Amer ican 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 s upport for this method. This method has been tested by a single laboratory in several environmenta l waters, and may be useful for many applications. However, EPA has decided to postpone approval of th e 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 futu re 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, Amer ican 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 u se is inappropriate because they have not been

validated for use with certain wast ewaters such as those from pulp and paper manufacturing. EPA should limit approval of their use to only matrices for wh ich validation studies have been conducted.

EPA proposes addition of ASTM D7574-09 for determina tion 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 Company2010 Methods Update Rule Response to Comments 70 March 2012 Similar to Method ASTM D7065-06, there is no sa mple 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 C ouncil for Air and Stream Improvement, Inc. Comment 169.1 - Judith R. Morgan, Amer ican 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 aqua tic life criteria referred to in the proposal were only for saltwater, not freshwater and saltwater.

Response: EPA thanks the commenters who expressed s upport for this method. This method has been tested by a single laboratory in several environmenta l waters, and may be useful for many applications. However, EPA has decided to postpone approval of th e 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 futu re 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 a nd 6.6 ppb, respectively), and the method would be appropriate for measurements in those ranges. At su ch 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, Amer ican 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 a nd” 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 u se is inappropriate because they have not been

validated for use with certain wast ewaters such as those from pulp and paper manufacturing. EPA should limit approval of their use to only matrices for wh ich validation studies have been conducted.

EPA proposes addition of ASTM D7574-09 for determina tion 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 determ ination 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 valida tion 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 mi ght 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 “o il 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, Dece mber 14, 2011). The Agency will make a decision on the approval or disapproval of this method on ce 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 memb rane 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 detec tion limit and precision and accuracy samples, but we weren’t able to do a larger study comparing the me thod 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 extr action 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 pr evious freon method as well as the n-hexane method I have been exposed to these dangerous fumes. I r ead 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. Th is 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 de termination 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 extracti on. 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 HE M rather than “oil & grease”. While both “HEM” and “oil & grease” can be construed as method defined analyt es, 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 specifi c type of extraction. One must understand that no matter what extraction procedure is employed, the an alytes of interest will always be a method defined parameter as the term “oil & grease” is truly indefinabl e. 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 “g reener”. The supporting data provided by OSS does seem to indicate an equivalent option for the determ ination of the parameter “oil & grease” and eliminates the risks created by the use of n-hexane. While A STM method D7575-10 does not lead to the analyte of interest as HEM, it does provide an alternative extr action 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, Jo int Water Environment Association and Virginia

American Water Works Association Comment 117.1 - Kelly M. Thompson, Wisc onsin 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, Amer ican Council of Independent Laboratories2010 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 we re 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 fo r all parameters. Other commenters raised concerns about the status of prev iously approved ATPs relative to the changes in approval for various versions of St andard Methods and ASTM methods.

Response: EPA appreciates the comments in support of th e 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 luminescen t-based sensor technology in clude 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. Wh ere specific vendors are mentioned, those vendors developed methods that include use of their equi pment 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 u se are proposed and promulgated in the Federal Register

. These methods are then listed in the tables of approve d methods at 40 CFR Part136 or in industry-specific effluent limitation guidelines.

Withdrawal of older versions of VCSB methods su ch as Standard Methods or ASTM methods does not affect the status of alternative methods (ATPs) for whic h letters have been issued stating that the methods are acceptable versions of the VCSB methods. Wh ere older versions of VCSB methods have been withdrawn, the newer versions are equivalent to th e older versions. Therefore, methods that were determined to be acceptable versions of the older me thods 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 approv ed method, fall within the flexibility allowed at part 136.6. These methods do not require that new perform ance data be generated if the changes are merely editorial ( e.g ., clarifications) and do not affect the perfor mance 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, Wisc onsin Department of Natural Resources Comment 169.1 Judith R. Morgan, Amer ican 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 Burt on, Joint Water Environment Association and Virginia American Water Works Association Comment 171.1 Lola Guerra, Henrico County DPU2010 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 L DO technology were mentioned by name, those that were not (e.g. SKALAR, YSI, Orion) are also acceptable?

Recommendation 1: Include the phrase "o r 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 ap proved ATP methods and their effective publication dates. EPA should provide this list of approved A TPs on the EPA website and update it routinely as new methods are approved so that the regulated comm unity 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 approv al of Optical Probes for DO measurement by multiple methods when su pported 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 mo re 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 co mparing 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 diffe rent 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 lis ted 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 vers ions of the approved methods, will vendors need to obtain updated letters from EPA and have info rmation 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 Cl ean Water Act monitoring?

Recommendations2010 Methods Update Rule Response to Comments 75 March 2012 • Allow all currently approved versions of Sta ndard 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 equiva lent 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 pa rt of 40CFR Part 136 as approved and/or specify any previously approved ATPs using SM editions wh ich 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 De partment 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 a nd 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 approve d, 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 w ith the methods approved for measurement of biochemical demand (BOD) a nd carbonaceous biochemical oxygen demand (CBOD) by revising footnote 63 of Table IB to the fo llowing: “Hach Method 10360, ‘Luminescence Measurement of Dissolved Oxygen in Water and Wastewater and for Use in the Determination of BOD 5 and cBOD 5 , 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. Butts2010 Methods Update Rule Response to Comments 76 March 2012 South Carolina Department of Health and Envir onmental Control Office of Environmental Laboratory

Certification

The Hach LDO method 10360 is described in foot note 63 of Table IB as approved for BOD and CBOD analysis. This is a dissolved oxygen procedure, a nd does not contain the required QC or procedures for performing BOD analyses. As such, it should only be li sted 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 ve ndors 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 C ouncil for Air and Stream Improvement, Inc.

Summary of Comments: One commenter expressed concern a bout the approval of these turbidity methods because they do not a pply to colored wastewaters.

Response: Methods M5271 and M5331 have the same li mitations 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. A pproval of these methods for general use is intended to give the regulated community additional options wh en 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 me asuring turbidity in wastewater for nationwide

use. M5271 is titled “Determination of Turbidit y 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 dr inking, ground, surface, and any colorless water with2010 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 De partment of Health and Environmental Control Office of Environmental Laboratory Certification Comment 116.1 - Wendy Harding and Mala Burton, Jo int Virginia Water Environment Association and Virginia American Water Works Association Comment 118 - Andrew G. Wendell. ClearWater Laboratory Comment 123 - Vincent Sapienza, Bureau of Wastew ater 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 Bo ttoms Regional Wastewater Treatment Facility Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility Comment 166. 1- Paul Wiegand, National C ouncil 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 app lication 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 em ail inquiry that was received by EPA on November 9, 2009. The inquiry asked about manual grab sample s collected and then combined to make a 24-hour composite sample for NPDES permit complia nce 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 fina l manual grab sample is obtained. EPA’s response at that time was that each grab sample must be filte red 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 sa mples could be held prior to combining them to make a composite sample. EPA’s response was that th e 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 he ld 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 filtrati on requirement in orthophos phate 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 f ilter), hence the requirement to filter the sample immediately upon collection. This filtrati on 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 inform ation in EPA’s November 2009 responses more widely available. As noted in many of the comments, th e clarification applies to grab samples and does not address samples collected using an au tomatic sampler. Therefore, pe rmitting authorities should consider the filtration issue when allowing the use of automate d 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 sa me (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 sa mples 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 ha ve 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 propor tional to the flow over that same time period.” We have 5 full time employees including our office mana ger 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 minut es 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 clarifi es 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 Approve d Methods. We applaud EPA for restating that field filtration is required for ortho-phos phate 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, i mmediate filtration upon collection of each sample, including each separately collected aliquot of a co mposite sample, for analysis of orthophosphate. MWWCA finds this an unreasonable and egregious regul atory 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 filtra tion, 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 impo ssible to collect an au tomatic flow-proportional composite sample for orthophosphate and impractical to collect an automatic 24-hour time-proportional composite sample. There is no current technology fo r automatically filtering 96 separate aliquots of a composite sample every fifteen minutes. Even if t echnology were available, POTWs and other permittees would need to collect at least two separate compos ite 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 ha rdship for many small treatment plants.

To require permittees to do manua l sampling for 24 hour composites would be a significant cost and regulatory burden to small entities and municipalitie s, 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 auto matic 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, th e 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 filtr ation 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 Envir onmental Control Office of Environmental Laboratory

Certification

The summary of the orthophosphate filtration clarifica tion located in Section E.1 of the discussion cannot be clearly found in the proposed rule. The summary provides enough informati on 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 ar e required to analyze for dissolved orthophosphate on a composite effluent sample, and where a composit e 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 handl ed 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 samp les could range from a couple hundred dollars up to or even exceeding $1000 per sample (c ompared 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 f acility would be required to staff personnel over a 24- hour period for the sake of filtering each sub-sample ali quot (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 regu lation 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 filtr ation requirement in orth ophosphate 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 mi ght 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 form ation. 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 co mpositing 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 af ter 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 ac idic samples. This theory has virtually no merit when tested in actual samples. Our comparison st udy indicates that the difference is analytically insignificant as more than 99%ofthe samples for NPD ES compliance have pH values between6.8 and 7.2. This clarification would mean that, since grab samp les must be filtered within 15 minutes of sample collection, treatment plants would not be able to u se auto-samplers for sample collection for reporting of Ortho-P. Auto samplers allow us to get more repres entative 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 ca n 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 requir ed be their permits to obtain a composite sample for orthophosphate. Maine DEP has been requiri ng 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 au tomated 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 oper ational parameters such as total suspended solids or biochemical oxygen demand using an automatic co mposite sampler. The only way to collect a comparable composite sample would be to collect a nd 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 orthophospha te 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 individua l aliquots (either flow weighted or timed) and the sample is not complete until the end of the compositing period. If the rule is impl ying 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 collecti on and filtration? Manual co llection and filtration of multiple grabs will increase the poten tial for error and increase the risk of sample contamination due to the number of times the sample must be handled thro ughout 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 allo w use of automated sampling equipm ent 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 so lely used for ortho-P. Also, we could not find in Section 136.3 the language is that stat es the 0.45um filtration is required.

Comment 164.1 Mark Haley Hopewell Regional Wastewater Treatment Facility

Comment: It is unclear if this requirement is sugg esting that only grab samples can be collected for orthophosphate analyses, or if individual grab samp les 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 individua l aliquots (either flow weighted or timed) and the sample is not complete until the end of the compositing period. If the rule is impl ying 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 collecti on and filtration? Manual co llection and filtration of multiple grabs will increase the poten tial for error and increase the risk of sample contamination due to the number of times the sample must be handled thro ughout the collection period. Furthermore, data to support this requirement has not been provided. Wh ile reasoning states that conversion of particulate forms of phosphorous into orthophosphate occurs in s lightly 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 fo r 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 e ffluents 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 require ment 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 formati on.” This requirement may be difficult to comply with in situations where the laboratory is located remo tely 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 sour ces, 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 manua l and automated sampling equipment currently preserve and analyze Orthophosphate samples as define d in Table II based on a single sample quantity. The proposed language would force the manual collec tion and immediate filtration of multiple grab samples (as little as 4 and as many as 96 individua l 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 permit s 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 co mposite period would be analyzed separately and the results averaged for compliance reporting.

The proposed revision reduces the comparability of Orthoph osphate 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 co llection of orthophosphate samples would result in an excessive burden to th e 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 regul ated community. Subsequently, Dow recommends that this requirement be eliminated.

II.E.2 Correct missing citations for microbial me thods 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 appr oved 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 ambien t waters in the proposal and are included in the final ruling. EPA’s Alternate Test Procedures progr am may be used to evaluate new and alternate methods which require method validatio n 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-lis ting of approved methods in the proposal, see response in Section

II.F.

Original Comment Text: The following commenters supported the co rrection 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 include d 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 Ambien t water methods versus Wastewater methods

Comment 164.1 Mark Haley Hopewell Regional Wastewater Treatment Facility

Why were some methods approved in the previ ous MUR not listed in the Proposed MUR?

We recommend EPA implement a systematic approa ch 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 th e addition of the language stating that the instructions in Table II take precedence over informati on 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 a nd 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 Global2010 Methods Update Rule Response to Comments 86 March 2012 Table II (58066) - "Required Containers, Preserva tion 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 instru ctions, 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 De partment of Health and Environmental Control Office of Environmental Laboratory Certification Comment 117.1 - Kelly M. Thompson, Wisc onsin Department of Natural Resources

Summary of Comments: Commenters generally supported the clarification that Table II takes precedence over other instructions. However, comm enters were generally opposed to the proposed changes that would allow permitting authorities to appr ove changes to the Table II requirements. Among

the concerns raised are the burden that this re quirement would impose on the permitting authorities to review and approve changes, as well as the likeli hood that such changes would present a burden for laboratories that work across states, and the inconsis tency 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 th e 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 pro posed change and has removed the proposed language from the final rule. The revised language ma y be found in section 136.3(e) of the rule.

Regarding updating Table II for cons istency 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 prea mble for today’s rulemaking for additional information regarding Table II requirements.

Original Comment Text:

Comment 91.1

Andrea Rex Massachusetts Water Resources Authority2010 Methods Update Rule Response to Comments 87 March 2012 We applaud EPA for clearly stating that the requi red 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 author ity for permission to use alternate containers, preservation, and holding times to those found in Ta ble 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 sampli ng conducted in compliance with the NPDES/SPDES

programs.

Specific reasons to omit the proposed language include:

The proposed language places all the burden of establis hing review criteria and maintaining a program for allowing alternative procedures for required contai ners, 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 challeng es to its credibility. We are often challenged by permittees to “show” where it is required that they fo llow 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 a llow alternatives, the proposed changes will lead to inconsistencies in collecting samples, which subseq uently affect monitoring data. Consistency in sampling protocols is a critical component to mainta ining comparability of da ta 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 a lternate procedures, whether it is holding times or method analysis provides simplicity and consistenc y. 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 intro ductory 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 instruc tions provided in specific methods or elsewhere.” If EPA believes that it is necessary to provide the oppo rtunity for a regulated party to seek an alternative to the specifics in Table II then it should follow the same guidance as d eclared in 40 CFR 136.4 and 136.5 application and approval for alternative test procedures.

Comment 107.1 Patsy Root2010 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 th e 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 speci fic 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 enfor ced? How will it benefit effective enforcement of the

Clean Water Act?

The Maine DEP, by a Guidance Document sent to perm ittees 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 Tabl e 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 pe rmittees) 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 Method2010 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 do cumentation will be helpful. The current version specifies using the Alternate Test Procedure to documen t 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 Envir onmental 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 "Informati on in this table takes precedence over instructions provided in specific methods or elsewhere unless a part y documents the acceptability of an alternative to the Table II instructions. The nature, timing, and exte nt of the required documentation (i.e. how to apply and review as well as the amount of supporting data) ar e 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 provid es an opening for inconsistencies across state agencies and poses a problem for laboratories to adhere to st ate requirements when analyzing samples for multiple states. It also leaves a lot of room for interpre tation as to what containe rs, preservations, and holding times are acceptable. In some cases, it may put the deci sions 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 need ed to make this decision, e.g. changes to preservations and holding times must come from a pu blished and reliable sour ce. This change would work against the National Environmental Laboratory Accreditation Program in their pursuit to reduce the inconsistencies between states and EPA program ce rtification requirements for laboratories.

Another inconsistency across EPA programs is th e 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 protoc ols 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 ap prove those methods which direct users to the Table II in 40CFR Part 136.3 for sample handling and preserva tion 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 fl exibility into the sample handling process, it also facilitates the erosion of consistency, conformity, and the quality of data being ge nerated. 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 devel oping in which deviations from recognized sample handling protocols can or do occur, decisions regarding the use of the associated da ta 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 qua lity of Clean Water Act data generated by individual

states.

Many would argue that data quality and sample integrity begin with th e 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 pr opose that any suggested modifications to sample handling and preservation requirements be handled in th e same manner as modifications to the analytical procedures, i.e., the ATP process. Rather than havi ng individual regulatory authorities make decisions regarding modification to sample preservation or hol ding 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 Depart ment 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 De partment of Health and Environmental Control Office of Environmental Laboratory Certification Comment 116.1 - Wendy Harding and Mala Burton, Jo int Virginia Water Environment Association and Virginia American Water Works Association Comment 117.1 - Kelly M. Thompson, Wisc onsin 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, Amer ican Council of Independent Laboratories Comment 171.1 - Lola Guerra, Henrico County DPU

Summary of Comments: The majority of the commenters suppor ted 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 docke t item EPA-HQ-OW-2010-0192- 0035) and concluded2010 Methods Update Rule Response to Comments 91 March 2012 that, on a nationwide basis, the Agency was una ble 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 Coordina tor 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, Amer ican 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 exam ple, samples analyzed for fecal coliforms may be held up to 6 hours prior to commencing analysis - th is 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 Envir onmental Control Office of Environmental Laboratory

Certification

Table II, footnote 4, gives an example of the hold tim e 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 foot note to read ‘‘Sample analysis should begin as soon as possible after receipt; sample incubation must be star ted no later than 8 hours from time of collection.”

We believe this is too restrictive. We find that th is 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 wort h 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 cau se an exceedance, not to mention the cost of a round trip. If samples are properly cooled, microbial activ ity 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 requ irement with qualification or must samples be rejected? Arguably, samples collected for beach mon itoring activities are equally—if not more—critical to human health, yet there is no equivalent holdi ng time regulation imposed on these samples. These samples are routinely shipped to labs via overnight carri er. We feel that the risk is low if the permitted facilities are properly monitoring their disinfection pr ocesses. 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 evaluate d. Finally, if this proposed rule becomes final, there are provisions within the rule that would allo w 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, Cent ral Valley Clean Water Association Comment 164.1 - Mark Haley, Hopewell Regional Wastewater Treatment Facility Comment 169.1- Judith R. Morgan, Amer ican Council of Independent Laboratories Comment 177.1 - Novelle C. Stokes, South Central Wastewater Authority

Summary of Comments: EPA proposed to revise the cyanide sam ple 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 instructi ons. 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 require ment or listed as another source of information rather than a requirement. Those commenters we re 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 suppor t 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 inform ation in the ASTM standard is considered to be a requirement of Table II, as well as providing additiona l information that may not be specified in the2010 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 hi storical 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 cyan ide sample handling revisions to footnote 5. Comment 79.1 Richard Burrows, TestAmerica Inc. Comment 169.1 Judith R. Morgan, Amer ican 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, Amer ican Council of Independent Laboratories Comment 177.1 Novelle C. Stokes, South Central Wastewater Authority

Comment: The change to the ASTM method is suppor ted, 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 Tabl e 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 footno te 6. If it is considered another source, then cyanide samples must be preserved to pH > 12. On the ot her hand, according to ASTM D 7365-09a, adjusting pH to >12 may introduce potential problems as follows:

• Adding sodium hydroxide to pH 12 in sampl es containing formaldehyde, an ozone disinfection byproduct, can result in cyanide formation during sample storage.

• If the sample contains carbonate, low cyanide recove ry 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 cyanid e 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 accura te results. Cyanide preservation and treatment for interferences is exceedingly problema tic. 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, Poli na 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 difficult y sorting through the bewildering array of options and have no way to de monstrate that their choices were correct. Ultimately2010 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 ar t for this important and difficult analyte.

Comment 112.1

Colin Elliott King County Environmental Lab

Comment: We agree that the procedures defi ned 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 belie ve 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 rela ted 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 T oxics Standards for Inland Surface Waters, Enclosed Bays, and Estuaries of California (SIP) establishes pr ocedures 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 dom inated water bodies often receive average monthly effluent limits for cyanide as low as 4.1 μg/L. Consis tent 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 spectrophot ometric 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 a nd bias, particularly in complex matrices such as

POTW effluent.

The attached document Problems Associated w ith Using Current EPA Approved Total Cyanide Analytical Methods for Determining Municipal Wast ewater 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 objectiv e exceedances. Sodium hydroxide-related bias is recognized by experts in cyanide analytical chemistr y, 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 to2010 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 cyanid e 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 cyanid e 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 incl ude “free” cyanide analytical methods in the battery of approved methods for NPDES compliance monitori ng as well the language modifications to the Table II introduction that gives the local permitting authorit y 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 mitigat ed by approved procedures,” including the latest procedures detailed in ASTM D7365-09a. For this re ason, we strongly support the regulatory flexibility afforded by dealing with the local permitting authorit y 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 Cent ral 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-re lated changes in the proposed rule.

(EPA did not include attachment 153.2)

II.F.4 Revising Cyanide Sample Handling In structions 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 De partment of Health and Environmental Control Office of Laboratory Certification Comment 116.1 - Wendy Harding and Mala Burton, Jo int 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 C ouncil 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 sam ple 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 instructi ons. 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 require ment or listed as another source of information rather than a requirement. Those commenters we re 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 suppor t 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 ma y 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 met hod 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. Th erefore, the information in the ASTM standard is considered to be a requirement of Table II, as well as providing additional info rmation that may not be specified in the analytical test methods. EPA r ecognizes 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 th is standard to be the most appropriate approach to resolving those concerns.

Original Comment Text: The following commenters supported the revised cyan ide 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 preser vation 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 mu st 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 samp le containing formaldehyde, an ozone disinfection byproduct, can result in cyanide formation during sample storage.

2. If the sample contains carbonate, low cyanide recove ry 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 H ealth and Environmental Control O ffice of Laboratory Certification

Table II Footnotes 5 and 6 reference ASTM methodolog y 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 labora tories 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 additiona l 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 clarifi cation 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 Depart ment of Environmental Conservation, Division of

Water Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District Comment 160.1 - Robert Steidel, Virginia Associ ation 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 we ll 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 co mmenter 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 a pproach to review of ATPs by simply specifying a non-approved method in a discharge permit. These co mmenters expressed concerns about the quality of any discharge data subsequently collected in such situations.

Response: EPA appreciates comments submitted in suppor t of the proposed changes. The Agency agrees that an essential component of requiring comp arability data was inadvertently omitted from the proposed language for limited use ATP applications at pa rt 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 proce dure compared to the performance of the reference method." Data demonstrating method comparability n eeds 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 allo w for a three-tiered system of validation. Those requirements vary based on the intended use of a meth od: 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 n early 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 ap proved 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 pe rmit 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 lik e that used to approve ATPs could be used by2010 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 li mited 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 Associ ation 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 da ta 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 limite d uses through the relatively informal alternate test procedures approval mechanisms that EPA has established.

However, there are instances where state NPDES ag encies 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, a nd 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 a lternate 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 amendm ent, 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 re ferring 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 ge neral requirements for the application rather than following a specific protocol. Using the documentation protocol defined for nation-wide Alternate Test2010 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 modifi cations that require validation through laboratory studies. The protocols are designed to allow for a th ree 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 ty pes). Minor or “small” changes generally fall within the flexibility provided at part 136.6.

Comment 122.1 Jason Fagel New York State Department of Environm ental 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 “Applicati on 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 h as not made an application for nationwide use then there is no requirement to provide comparability da ta. 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 limite d 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 provisi ons for method modifications that are codified at 40 CFR 136.6. Part of that proposal was to pr ovide 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 De partment of Health and Environmental Control Office of Environmental Laboratory Certification Comment 169.1 - Judith R. Morgan, Amer ican Council of Independent Laboratories

Summary of Comments: A number of commenters offered gene ral support for the allowed flexibility and many thanked EPA for providing specific exampl es. 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 up dating the affected methods rather than relying on the approach of describing the allowed flexibilit y 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 u ser 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 cer tification or accreditation, EPA recommends that the permitting authority be not ified 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 affect ed 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 descr ibe allowable modifications where practical.

EPA was not able to fully respond to concerns fro m one commenter regarding enforcement concerns because it is not clear if “IDNR” refers to the Departme nt of Natural Resources in Illinois, Indiana, or Iowa, and the commenter did not include the refere nced memorandum with the comments. However, EPA notes that state and local regulatory authorities alr eady 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 th e affected dischargers and laboratories of such

restrictions.

Original Comment Text: The following commenters had the sa me (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 prohi bited 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 modi fied method....” Please clarify if it is an “and” or an “or.” Additionally. How does the USEPA foresee pe rmitting authority staff be ing able to understand all the requirements for method modifications? W ill additional guidance on this, for NPDES permit writers, be made available by the USEPA?

Comment 107.1 Patsy Root

IDEXX Laboratories2010 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 wi de 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 s hould allow analysts the flexibility to modify CWA methods without prior approval provided the user h as documented equivalent or better performance of the method in that particular matrix type.

In instrumental analyses, analysts may need to m odify approved methods in order to combat matrix

interferences and these modifications s hould 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 th e 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 fo r 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 Envir onmental 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 laborator y to use a modification that this unacceptable to regulators with no potential oversight until the next au dit, inspection, or evaluation is performed. This could result in substantial amounts of data being deem ed 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. Morgan2010 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 E rror (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, Wisc onsin Department of Natural Resources Comment 169.1 - Judith R. Morgan, Amer ican Council of Independent Laboratories

Summary of Comments: Four commenters supported the use of Relative Standard Error (RSE) to evaluate calibrations, and several of those commenter s suggested minor changes to the presentation of the equation and the terms involved. One commenter expr essed reservations about the use of RSE, noting it has been advocated by only a few parties, it may no t 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.

x i = 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 pr ovides an additional approach for laboratories and data users to evaluate calibrations. However, EPA point s out that the historical mix of calibration metrics ( e.g ., average RRF, regression coefficients, and “use the en tire 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 [r 2 ]). 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 lim it of the method will also meet the r 2 limit from another method. One advantage of the RSE is that the same acceptanc e limit for the RRF approach can be used for the RSE approach. And, as noted by one commenter, the R SE approach is more sensitive to deviations at the2010 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 inadequa te as a calibration assessment tool, because it allows very large relative errors at the low end of the curv e. 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 documen ts, RSE should be expressed in a slightly different way, as follows:

ܺ 100 ൌ ܧ%ܴܵ ඩ ෍ ݕൣ ௜ ᇱ െ ݕ ௜ ൧

ݕ ௜

ᇱ ଶ ሺ ݊െ݌ ሻ ൘ ௡

௜ୀଵ

Where: y’i = Predicted (or calculated) res ponse for the ith calibration standard yi = Actual response for the i th calibration standard n = the number of calibration points p = the number of terms in the fitting eq uation (average=1, linear=2, quadratic=3)

Comment 83.1 Anonymous Public Comment

Unknown

On xx/xx/xxxx we submitted comments on method 80 00D 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 e quation, 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 aver age type curve. However, the RSE based on responses trends very high in the special case where one of the predicted respon ses 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 ሺ ݊െ݌ ሻ ൗ ௡ ௜ୀଵ

Where:

x' i = Predicted (or calculated) amount for the ith calibration standard

x i = Actual amount for the ith calibration standard2010 Methods Update Rule Response to Comments 105 March 2012 n = the number of calibration points p = the number of terms in the fitting eq uation (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 th e chemistry of the analysis but simply provides a

more consistent and reliable calibration assessment th an 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 inadequa te as a calibration assessment tool, because it allows very large relative errors at the low end of the curv e. 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 documen ts, RSE should be expressed in a slightly different way, as follows:

(The equation could not be captured from the comment s, but is similar to the ones presented in comments 79 and 83).

Where: y’i = Predicted (or calculated) response for th e ith calibration standard yi=Actual response for the

ith calibration standard n = the number of calibra tion 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 re lative standard error (RSE) as an approved means of evaluating calibrations. Our main concern, after research ing 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 statis tics 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, th ere are other procedures available, most notably the use of the coefficient of determination as presente d 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 h as not been addressed is how to deal with multiple mechanisms for evaluating calibration data. Laborat ory 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-analyt e 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 laborat ory is focused on using the approach that allows them to report a set of data for a given analyte, ra ther than focusing on production of good quality data.2010 Methods Update Rule Response to Comments 106 March 2012 The first step towards a solution re quires the agency to work with al l its programs and present a unified approach to evaluation of calibration which is weight ed 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 inadequa te as a calibration assessment tool, because it allows very large relative errors at the low end of the curv e. 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 toward s 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, Wisc onsin 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. Tita nium 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 cove red 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 pr ocedures that are applicable to wastewater samples

described in Methods 200.7 and 2 00.8, as well as SM 3120 and 3125 involve strong-acid digestions that are usually carried out in open containers at te mperatures 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 disso lved 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 wa stewater samples include digestion procedures that are performed in closed vessels, and digested sample s 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 and2010 Methods Update Rule Response to Comments 107 March 2012 200.8 in Table IB as approved methods for measure ment 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 incl uded in Table IB as an approved method for measurement of iridium, osmium, palladium, platin um, 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, mo lybdenum, nickel, selenium, silver, and tin. In addition, SM 3113B-2004 states that it is also applicab le to analysis of bismuth, gallium, germanium, gold, indium, mercury, te llurium, thallium, and vanadium, but precision and accuracy data are not yet

available. EPA has included SM 3113 B-2004 in Tabl e IB as an approved method for measurement of gold, thallium and vanadium.

Cobalt and molybdenum are not on the analyte list fo r 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 torc h. By virtue of allowing the use of the axially viewed torch in Method 200.7, or the other appr oved ICP/AES methods, cobalt and molybdenum can be analyzed in the same fashion as in Method 200.5, pr ovided 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 reco mmending that EPA allow the additio n of analytes not included in an approved analytical method as long as the QA/QC requireme nts 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 NP DES 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 specifi c 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 sh ould 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 techni que in a modified method are essentially the same as an unmodified part 136 method, then the modified method is an equivalent and acceptable alternative2010 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, im prove precision, reduce interferences, lower laboratory costs, and promote environmental stewardship by re ducing 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 modi fication, 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, an d the analyte is listed as a target analyte in EPA method 200.7.)

Extending method target analyte lists - Method modifi cation 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, ye t 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 practic e to use ICP for the analysis of Titanium, as well as

for other trace elements for which ICP is not allowe d 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 pr oposed rule, a lab should be allowed to use ICP for the analysis of Titanium provided that it has determin ed the potential for inter-element interferences, can achieve an MDL that affords adequate sensitivit y, and has generated accep table demonstration of capability data. The fact that the EPA or a third pa rty has not published validation data to extend the analyte lists to include all of those analytes typica lly analyzed by a multi-analyte technology should not

serve as rationale to exclude them. Greater considera tion 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 an alysis 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 fo r 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 appr oved for the elements: Au, Ir, Os, Pd, Pt, Rh, Ru, Sn, and Ti?

Why is ICP/MS method SM3125 allowed for the analys is 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 gra phite 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 defe nsible and reliable monitoring of these analytes. Where feasible for a given technology, EPA should allow current EPA-a pproved 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 woul d 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 Parameter s

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 pa rameters, 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 t est procedures under the ATP program, the specifics for

which can be found at http://water.epa.gov/scitech/m ethods/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 th e type of vessels used such as graduated cylinders and pipettes that transfer sample) because the resu lts obtained with the method may not be directly compared to the results obtained with a modified me thod. For example, a cha nge 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 au thorities 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 me thod-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 16 38 be cited as an allowed modification for other digestions.

Response: EPA notes that digestion procedures are sim ilar 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 th e “total” measurement. The specific acids used and the overall acid strength will affect how much metal ma y 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, vers us 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 matr ix) across a hydrophobic semipermeable membrane to separate the analyte of inter est 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 comm enter, these measurements ha ve 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. M odifications 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 a pproved 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 spec ified 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 concen trations. 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 othe r 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 sp ecifications 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 concen trated 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 st ate agencies have specifically disallowed modifying the 200 digestion, although a more vigorous diges tion produces “equivalent or better performance” and2010 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 de part 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 clarifi cation 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 De partment of Health and Environmental Control Office of Environmental Laboratory Certification Comment 166.1 - Paul Wiegand, National C ouncil for Air and Stream Improvement, Inc. Comment 169.1 - Judith R. Morgan, Amer ican 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 th ought 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 effectivel y analyzed in full-scan mode. With respect to the specific criteria, EPA developed these criteria to en sure 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 likeli hood 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 ch ange 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 inte rest rather than scanning for all masses over a wide range of mass to charge ratios. EPA also disagrees th at the technique will most often be used to improve sensitivity. Although it is true that sensitivity genera lly 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 add itional 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, Amer ican Council of Independent Laboratories

Other comments:

Comment 113.1

Susan E. Butts South Carolina Department of Health and Envir onmental Control Office of Environmental Laboratory

Certification

Section 136.6 (b) (S) includes previously accepted m odifications. 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 speci fics on retention times, number of scans, ratio acceptance criteria, etc. Some of these criteria are more specific than wh at 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 Monitori ng 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 ve rify 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 fo rth 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 af ter very careful evaluation and validation.

The most probable reason for utilizing SIM is to impr ove 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 analys ts 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 misidentif ied. Thus, EPA’s proposal fails to provide any meaningful verification of selectivity in any type of samp le. 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 deve loped and adopted in the European Union (see Commission Decision of 12 August, 2002, implementing Council Directive2010 Methods Update Rule Response to Comments 113 March 2012 96/23/EC concerning the performance of analytical me thods 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 r espect to Selected Ion Monitoring until such time as EPA develops meaningful and th orough sensitivity testing and valida tion protocols, develops more robust ion and ion ratio criteria, tests these proce dures 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 a pproved 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 com port with section II.F of this proposed rule that describes how sample preservation and holding time re quirements 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 De partment 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 us ing 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 cu rve, 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 approa ch to calibration curves and acceptance criteria.

Response: EPA disagrees that it is appropriate to extrapol ate 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 a2010 Methods Update Rule Response to Comments 114 March 2012 “linear range” standard above the highest calibra tor be analyzed periodically as a check on such extrapolations. Therefore, EPA is maintaining its pos ition that all reported sample results must be within the range determined during initial calibration of the me thod. Any samples with results above this range must be diluted and reanalyzed for reporting purposes.

EPA disagrees that additional requirements on quadra tic calibration beyond those in the proposal (such as those in SW-846) are needed because calibration veri fication 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 accep tance 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 sc ope of today’s rulemaking. EPA may consider whether additional requirements are ne eded for calibration in the future.

Original Comment Text:

Comment 112.1

Colin Elliott King County Environmental Lab

Comment: Not allowing concentrations to be extrapol ated 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 exp ected accuracy of the method. We propose that concentrations may be extrapolated above the high est 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 al l other continuing ca libration standards.

Comment 113.1

Susan E. Butts South Carolina Department of Health and Envir onmental 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 quadra tic 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 us ually involves at least one or two points of inflection, the importance of verifying accu racy through the entire analytical range cannot be understated. This is especially important for the low est 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 ca libration standards with acceptable percent difference criteria specified. Also , additional language must be added to provide clarification concerning the conditions under whic h 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 calib rations must also not be used for methods or instruments previously shown to exhibit linear calibra tion for the analytes of interest. This language can

be found in section 7.5.3 of EPA 8000B of the SW-8 46 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 par tial 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 th e following document for a detailed review of how to evaluate calibration data that must be part of an y 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 B est 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 focu ses 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/Publica tionArticle.aspx? m=115&amid=472

The evaluation of the calibration is a critical element th at must be added as part of the calibration review (40 CFR 136.7 a. item 7). Laboratories not performing th is type of evaluation are subjecting data users to poor quality data as was demonstrated in the inter-la boratory study that resulted in this reference paper being generated and has been the case in many profic iency testing studies for the WS and WP programs.

(This may be one of the reasons many laboratories ar e 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 De partment of Health and Environmental Control Office of Environmental Laboratory Certification

Summary of Comments: One commenter requested clarificati on regarding the use of gas diffusion.

Response: In response to this comment, EPA has clarifie d 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 th e sample matrix may be used in place of manual or automated distillation in methods for analysis such as am monia, total cyanide, total Kjeldahl nitrogen, and total phenols. These procedures do not replace the di gestion 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 Envir onmental 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 lie u 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, Amer ican 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 improve d 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 appr oach under study and agr ees 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, Amer ican 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 de sirable, 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 detect or for metal analysis; however isobaric interference can cause problems for quantitative determination as we ll 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 cont rol 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 prob lem occurs not only with FGD wastewaters; UWAG

members have found the same overstatement of sel enium and arsenic using the unmodified method on discharges from ash treatment ponds.

In an effort to minimize such matrix specific in terferences, interference control cell technologies have been developed which attempt to break up or rem ove the molecular ion interferences (e.g., argon or calcium chloride, which mimics arsenic-75) and allo w accurate elemental measurements even in complex sample matrices.

UWAG provided detailed recommendations on using i nductively coupled plasma mass spectrometry for flue gas desulfurization wastewater in letters of Ma rch 19 and April 6, 2010, which are attached to these comments and expressly incorporated herein. See Le tter, 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 recomme nds, conducting the analysis of flue gas desulfurization wastewater with multiple mass numb ers 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, Wisc onsin Department of Natural Resources Comment 123 - Vincent Sapienza, Bureau of Wastew ater Treatment, New York City Department of

Environmental Protection Comment 132.1 - Paula Hogg, Hampton Roads Sanitation District Comment 169.1 - Judith R. Morgan, Amer ican Council of Independent Laboratories Comment 183.1 - Sanwat Chaudhuri, Ut ah 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 modi fications to Method 625, but noted that the bulk

of the 600-Series methods date to 1984 and wondered when these met hods would be revised. Another commenter supported changes to purge-and-trap met hods, 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 fo r 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 met hod 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 allo wing 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 stat e 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 incons istencies across EPA programs, EPA notes that the methods approved for the drinking water and wastew ater programs are intended for different uses and therefore may have different requirements. Unfortunate ly, 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 extrac tion pH, as the commenter notes, the prohibition stems from concerns with contamination of the sample by th e 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 “narro w range pH paper” or some other non-intrusive means. Alternatively, a laborator y 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) fo r 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 standa rds 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) allo ws 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 rec overies, 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 analyt es. 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 direc tly 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 provi de 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 labor atory may be required to t est representative materials from each “lot” of cartridges purchased from a supplier to determine their capacity to adsorb potential interferences and release target analytes. Tho se 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, ther e is no way that a laboratory, or a data user, can ensure that a2010 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 demons trate 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 becau se such changes are a fundamental change of the measurement technique and require a demonstration of performance unde r 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, mainta in 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 ty pes of glassware for sample preparation, and threepoint calibration. Also, the precision and accuracy st udies 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 tim es, we respectfully request that the agency work towards a unified position with r espect to this issue.

The drinking water program, in particular, specifical ly 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 provide d 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 th e methods. These procedures may not be changed. Specifically, the purge time, purge gas flow rate, a nd 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 agen cy-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 ch allenges, 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 ti ght control of pH is necessary for the more reliable analysis of the parameters and if the analyst can de monstrate that the procedure utilizing the pH meter and electrode will not compromise the integrity of the sam ple. 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 th e 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 accep table 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 met hods as long as QA/QC demonstrates acceptable method performance. Develop data quality objectives fo r programs that would facilitate this flexibility

and address the need for new methods.

Comment 169.1 Judith R. Morgan American Council of Independent Laboratories2010 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 13 6.6 to allow flexibility without departing "substantially from the underlying chemical principles employed in met hods 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 w ith 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 incl ude 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 ma ss 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 demons trated to be adequately extracted from the target water by solid phase extraction, we advocate allowi ng the solid phase extraction. This would result in much less use of the toxic methylene chloride solven t, 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 ph ase 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 (variati ons of the stir bar sorptive extraction can be used

to extract the solids in a wastewat er 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 effec tive. We also encourage the taking advantage of the improvement of the tools of analyses as they come ava ilable, some of which we listed in our comments. If we can be of any help feel free to contact us.

Comment 190 Lynn Egan2010 Methods Update Rule Response to Comments 122 March 2012 Lachat Instruments

The additional information in the proposed rule (sect ion 136.6) will help to further clarify acceptable modifications, as well as the requirements for the valida tion 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 a ddition 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 ta ken 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 h as documented equivalent or better performance...." Restate as "EPA strongly encourages regulatory author ities to allow analysts the flexibility to modify CWA methods without prior approval, provided th e 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 De partment of Health and Environmental Control Office of Environmental Laboratory Certification Comment 116.1 - Wendy Harding and Mala Burton, Jo int Virginia Water Environment Association and Virginia American Water Works Association Comment 117.1 - Kelly M. Thompson, Wisc onsin 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, Pennsylva nia Department of Environmental Protection2010 Methods Update Rule Response to Comments 123 March 2012 Comment 152.1- James Matthew, On Line Environmental Inc (OLE) Comment 154.1 - Sharon Mertens, Milw aukee 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, Amer ican Council of Independent Laboratories Comment 169.1 - Judith R. Morgan, Amer ican 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 coun terparts in microbiological methods). Other commenters expressed concern that the new language w as either duplicative or contradicted language in existing approved methods, or presente d conflicts with various state or national accreditation programs. Still other commenters objected to the perceived cost s of meeting the letter of this new language and suggested that the QC checks simply will not o ccur, 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 in terfere with results. Several commenters requested definitions of terms. One commenter suggested th at training was needed. One commenter wanted to know what the minimum acceptance criteria were fo r 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) elemen ts 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) a ppropriate 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 shoul d 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 e ither duplicative or contradicted in existing approved methods or accreditation programs, EPA has added a ne w section at Part 136.7 to address concerns that certain approved methods do not contain QA/QC pro cedures. 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 tho se instances. Standard Meth ods incorporated new QC requirements starting with the 20 th edition of Standard Methods sim ilar 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 appli cable. Similarly, EPA does not anticipate conflicts with laboratory accreditation programs because these pr ograms generally follow the QC requirements in the method or otherwise specified in regulatory program s. The purpose of this new section is to ensure that analyses conducted for compliance monitoring w ith CWA regulatory programs contain appropriate2010 Methods Update Rule Response to Comments 124 March 2012 QA/QC and the Agency’s view is that this is al ready occurring in most laboratories (with very few exceptions). This new requirement is added to clarif y that laboratories must implement proper QA/QC, as needed, for all CWA compliance rela ted analyses to provide quality da ta 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 requireme nt will be costly, proper QA/QC is essential for obtaining results of known and acceptable quality. In th e long run, it could be much more costly to use data which lacks proper QC in demonstrating or enfo rcing 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 th eir SOPs. EPA estimates that this would not have a significant impact on laboratories because the vast ma jority of Part 136 methods already include or reference QA/QC requirements. Further, most labor atories already implement the QC checks prescribed by the newer methods and are already documenting th ese 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 analy ses 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 sampl e, the QC costs would be typically 5-10% of the total costs, and are generally included in the labor atory 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 th an 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 defensibilit y where applicable to the methods used to measure pollutants for compliance monitoring purposes and ignoring these QC ch ecks, as a comment suggested, is in violation of Part 136 and Part 122. Subpart C, Part 122.41 (Per mit Conditions) in 122.41(e) states that the permittee “shall at all times properly operate and mainta in all facilities and systems of treatment and control...Proper operation and maintenance also incl udes adequate laboratory controls and appropriate quality assurance procedures...” In most cases, these pro cedures 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 re quirements when there are difficult matrices that interfere with results, the laboratory must make ever y effort to address potential interferences but it does not relieve the laboratory of c onducting 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, vol untary 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 La boratories Performing Environmental Analysis.

Regarding the comment suggested that training was needed, EPA agrees that laboratories must provide adequate training to analysts on the analytical pro cedures 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 requi rements 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 suppor ted such minimum requirements as essential for improving data quality. ELAB believes, however, th at the proposed language at Part 136.7 lacks sufficient detail and as written will present many prob lems, both for laboratories and laboratory auditors. The NELAC Institute (TNI) has a consensus standa rd, Management and Technical Requirements for Laboratories Performing Environmental Analyses, that represents the best professional practice in the industry, contains sufficient detail for laboratories a nd laboratory auditors to clearly understand what is required, and defers to QC require ments 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. Wher e 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 el ements required to establish a quality system that produces data of known and documente d quality.” No other such consensus standard exists; therefore, under the National Technology Transfer and Advancem ent 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, howev er, 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 demons trate competence as well as requirements for each analyst. TNI’s requirements contain both an initia l DOC and an ongoing a nnual demonstration to demonstrate continued proficiency. The TNI standard has detailed instructions for what activities should be performed and has appropriate ac tivities for chemistry, microbiology, and radiochemistry laboratories.

(2) Method Detection Limit (MDL) The proposed language at Part 136.7 implies that labor atories would have to perform MDL studies for all methods, including methods for parameters such as te mperature, pH, BOD, and presence/absence tests for microbiological parameters. MDL studies are not appropr iate 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 sta ndard uses the internationa lly accepted definitions of Limit of Detection (LOD) and Limit of Quantitati on (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 ex clusion 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 disc iplines, 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 extens ive 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 perform ed by the laboratory if unacceptable results are

observed. The TNI standard contains extens ive detailed language describing these activities.

(5) Matrix Spike, Matrix Spike Duplicate, or Labor atory Fortified Blank Duplicate for Suspected Difficult

Matrices ELAB supports requirements for such activities as matr ix spike and matrix spike duplicates to be a minimum QC requirement. The proposed language, ho wever, does not describe the frequency of such analyses, what constitutes an acceptable result, and wh at corrective actions should be performed by the laboratory if unacceptable results are observed. The TNI standard contains ex tensive detailed language describing these activities.

(6) Internal Standards, Surrogate Standards (for organic analysis), or Tracers (for radiochemistry) ELAB supports requirements for such activities as intern al standards and surrogates to be a minimum QC requirement. The proposed language, however, does not describe the fre quency 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 an d Continuing Performance So lution (also referred to as initial calibration verification [ICV] and c ontinuing calibration verification [CCV]) ELAB supports requirements for calibration a mini mum QC requirement. The proposed language, however, does not describe the frequency of such an alyses, 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 equipm ent (e.g., balances, ovens, water baths). The TNI

standard contains extensive detaile d 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 en sure it was implemented and preventative actions.

(10) QC Acceptance Criteria ELAB agrees that QC acceptance criteria are importa nt. The proposed language contains no detail, and thus a laboratory could decide their acceptance crite ria 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 sa mples analyzed during a 1-year period and perform the required QC checks once per year. TNI has establis hed 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 frequenc y, 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 dem onstrate 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 Ag ency 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 proc edures whether EPA or other method publishers have specified these procedures in a specific Part 136 me thod 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 voluntar y consensus standard body methods indicate that any analysis using such methods would also meet th e 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 w ith 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 Institu te (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 pa rameters in general, and the reference to NELAC Chapter 5 in particular, but note that the 2003 NELA C 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 Ins titute (TNI) NELAP standards adopted in 2009 for implementation in 2011.

Comment: With three partial exceptions we agree wi th the 12 essential quality assurance checks, and believe that requiring these will go a long way toward s 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/M S 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 substan tial 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 belo w the quantitation limit. In addition, EPA should consider whether determination of a qua ntitation limit should be an essential Quality Control

parameter.

Exception 3 concerns tests for which some of the qua lity assurance tests are not possible or inappropriate. For the most part, these are tests for which spiking st andards 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 soluti ons 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 ar e 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 ch anges 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 numer ous 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 situa tion. 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 w ill 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 regul ation will do one thing really well. It will cause less people to desire work at a Sewer Plant. What other C ity 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. Wh o’s going to do that when it takes a week for the results to come back from a contract lab? Nobody! Th ere’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 bu dget 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, “Laborat ory 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 sta ndards) 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 incl ude 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 ach ieving 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 elemen ts. 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 w ould 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 Wolf2010 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 writte n 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 comm only 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 elem ents 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 w ithin 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 an alytical methods themselves, quality assurance sections applicable to the analytical methods as i ssued 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 laborator ies which must revise numerous SOPs to address QA/QC checks which are not relevant (ex. internal st andards, surrogate standards or tracers)to the method but require a documented rationale for their absen ce 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 co mpliance costs, and represents a probable future

source of conflict with the alread y existing QA/QC standard sources.

Comment 94.1

Scott D. Siders Division of Laboratories, Illinois EPA

Comment: Welcome the requirement for basic QC para meters in general, and the reference to NELAC Chapter 5 in particular, but note that the 2003 NELA C 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 Ins titute (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 LF BD instead of MSD in a batch which contains difficult matrices even though this is not recommended by the specific analytical method? Also, certain2010 Methods Update Rule Response to Comments 131 March 2012 matrix interferences can never be fully removed ev en 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 wi th the 12 essential quality assurance checks, and believe that requiring these will go a long way toward s 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 standa rds 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 belo w the quantitation limit. In addition, EPA should consider whether determination of a qua ntitation 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 sec tion (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 soluti ons 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 ar e 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 pr oposed, the TML has grave concerns about an increase in the regulatory burden, in crease in the cost and an increase the level of confusion at the operational levels of municipal w astewater 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 enfo rcement. 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 ow ned wastewater treatment plants that will fit into2010 Methods Update Rule Response to Comments 132 March 2012 the "small entity" classification. Mo st all of these will experience a si gnificant cost increase because of this proposed rule.

Though most plants perform a degree of laboratory Qu ality Assurance/Quality Control, to fully comply with the proposed twelve Quality Control Checks (pag e 58071) will require an increase in laboratory time and cost in the range or 25-50%. Even at the low leve l this is a significant in crease in costs to pass along to ratepayers especially during a time of recession. There are some small publically owned wastewater

utilities whose user rates ar e 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 thr ee weeks for those test results, will be operating their plants blind. Though most of the state's small pl ants produce pristine effluent most of the time, most do not have QC programs to the extent that this propo sed rule will require. It appears that EPA may be far out of touch with the real world of small plant opera tion, 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 confusio n, and unfortunately are poorly timed. EPA should reconsider this part of the proposed rule change.

Twelve Essential Quality Control Checks (FR pa ge 5S071): Mandating these steps without additional clarification and or training will add a significant amo unt 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 st ate regulators already give inconsistent answers to these questions on these subjects, this rule w ill 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 abbr eviations are taken from Standard. Methods, even the regulators don't use them. They use a different QA voca bulary. This of course adds to the confusion. EPA needs to provide training in what each of the twel ve checks means for each analyses conducted. Without this precise training, local governments and thei r employees will find themselves under enforcement action for actions that may have been beyond thei r 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 fac ilities, 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 docum ented QC checks, but will also result in wastewater plants being operated blind because of the two to thre e week delay in receiving effluent test data. As described above, this situation appears to show th at EPA values data quality over effluent quality.2010 Methods Update Rule Response to Comments 133 March 2012 Summary and Recommendations: The technical deficienci es 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 y ears 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 cl early 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 Pub lic 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% incr ease 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 labor atory. 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 est imated eighty percent of wastewater systems in Tennessee are considered small systems and have limite d 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 increa se in the time it takes to perform daily laboratory tests. Systems that cannot afford to hire another st aff member to perform the se checks will sacrifice time spent in other areas such as troublesh ooting, 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 perfo rm analysis correctly with certain checks and balances to insure reliable data to protect the public h ealth 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 met hods 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 that2010 Methods Update Rule Response to Comments 134 March 2012 some of these additional requirements to be perform ed 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 Wa ter 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 sta ndardized across the diverse series of approved methods. Having standardized QA/QC will also prevent permittees a nd permittee laboratories from seeking out the method with the least rigorous QC requirements when choosin g 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 referen ced 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 va lid, 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 respect fully requests that definitions be provided in an updated proposed rule to allow furthe r 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 m eaningful. Again, applicable and appropriate QC

measures are described in detail for individual methods.

Comment 4: These steps are not applicable or appr opriate 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 im pediment, 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 im prove water safety. We appreciate the opportunity to be part of this process and hope to continue to pa rtner 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 A ssurance Control that lists twelve essential quality control checks.

Does EPA propose to require that all twelve contro ls be established and performed for the following parameters found in NPDES permits: flow, pH, temp erature, dissolved oxygen, biochemical oxygen demand, non-filterable solids (TSS), dissolved solids, tota l residual chlorine, turbidity, fecal coliform, and

e. coli?

The Biochemical Oxygen Demand approved method (refe rence 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 anal ytical 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 contra ry to the method's requirement for a dissolved oxygen uptake of at least 2.0 mg/L and residual di ssolved 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 wher e 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 s upports the standardization of terminology. The use of multiple terms to describe method detecti on limit continues to cause confusion among the data users making decisions regarding h ealth and environmental impacts.

Comment 112.1

Colin Elliott King County Environmental Lab2010 Methods Update Rule Response to Comments 136 March 2012 Comment: We agree that documenting all “essentia l QC requirements” is a good idea. However, it should be allowed for some requirements to be d escribed 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 exampl e to streamline this process would be to address how SOPs should address “essential QC” that does not appl y (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 w ith data sets and the associated corrective action. Corrective actions can vary depending on project require ments, action limits, sample matrix etc.

Comment 113.1

Susan E. Butts South Carolina Department of Health and Envir onmental 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 s hould 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 men tion an ICV. ICV needs to be defined since in

some instances this refers to a second source standa rd. 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 ite m in the list of QC checks, does this supersede the approved method and require internal standards and su rrogates for all organic methods approved under 40

CFR Part 136?

A list of methods needs to be provided to which th e QC checks would apply. For instance, the checks should not apply to pH or other simple inorgani c 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 ch ecks are designed for the laboratories or the method developers.

Comment 116.1 Wendy Harding and Mala Burton Joint Virginia Water Environment Association a nd Virginia American Water Works Association

Comment 1: This requirement is redundant. Essentia l, 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 m eaningful. 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 f act 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 anal yses 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 ru les. 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 abbr eviated version of the drinking water program’s specific requirements which are outlined in a documen t 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. Clarifi cation of the rule’s intent is discussed in the rule summary, yet this critical information is not include d 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 la boratory’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 cont rols 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 cont rols do not apply (e.g., internal standards, surrogate standards or tracers do not apply to analyses of inorganic pa rameters) as well as being included with the monitoring data produced using each method. “

(D) There are discrepancies between required Qua lity Control samples in the “12 essential elements” and approved testing methods. For example, most Standa rd 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 elemen ts are required for all tests, some of which are impractical. For example, the requirement for “Laborat ory 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 tr end analysis— as an essential element. We believe that, while control charts can serve as valuable an alytical 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 le ast 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 matr ix”? 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 la bs 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 spik es with acceptance criteria of 0 to 200% recovery, criteria whic h provide no utility in evaluating da ta quality. This is another reason why these requirements are best left up to certifica tion 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 c ontrol, 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 documenti ng / control charting / etc. rather than the actual running of the test. Ballooned SOPs become an impe diment, not a benefit for bench top analysts. Test methods that do require more extensive quality cont rol 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 a nd 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 highl ight an issue. To dictate that all labs control chart all of their QC parameters on all the test met hods 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 r easonably be expected to utilize control charting in the process of investigati ng the problem and determining the proper corrective action. Once long term stability of the QC paramete rs 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 qua lity assurance and quality control language at 40CFR136.7. Instead, move toward s 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 a nd warranted. Field operators running simple test procedures which require immediate analysis (with in 15 minutes) do so using approved test methods following manufacturer’s instructions. Training do cumentation verifying Initial Demonstration of Capability, equipment calibration verification and in dividual method verifications are currently being done. To require field operators to carry around mul ti page SOPs filled with vo luminous descriptions and exclusions is without merit. To require a field opera tor 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 defens ible. The Office of Water commissions a Federal Advisory Committee on Detection and Quantita tion (FACDQ) and has received many sound recommendations from the FACDQ, which should be impl emented 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 curr ent MDL and ML are unsuitable for use in 40 CFR, Part 136 was the recently proposed Sufficiently Se nsitive Methods rule, which might have been supported, except for the unresolved issu es surrounding the MDL, ML and DQOs.

Comment 126.1 Sterling Pierce Maine Department of Environmental Protection

Maine DEP is a delegated State and currently i ssues 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 li censed limits. These facilities are typically required to test for a variety of parameters including; total suspended solids, bi ochemical oxygen demand, chemical oxygen demand, pH, chlorine residual, fecal coliform, E. coli, conductivity, color, temperature, and dissolved oxygen. Currently, publically owne d treatment works (POTWs) may perform these tests without obtaining certification under the Maine Comp rehensive Environmental Laboratory Certification

Rules.

Maine DEP has oversight of the operation of these POTW s and the associated laboratories. The operators are required by the facility license to analyze all sa mples using methods in 40 CFR 136.3 as approved by EPA. Maine DEP also implements the annual disch arge 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 Dema nd, Chemical Oxygen Demand, pH, Total Residual Chlorine, Fecal Coliform, E. coli, Conductivity, Co lor, Temperature, and Dissolved Oxygen. Is EPA proposing to require that controls be established a nd 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 St ate to discontinue testing for these parameters at the treatment facility and seek out commercial laborator ies 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 commerci al laboratories, which is critical to the integrity of the data that is passed through the license holders to th e regulators. So the desire to have better quality data, could potentially lead to the unintended consequence of data thatdoesn’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 a pplicable 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 al ternative, we propose that the laboratories be given the discretion to choose appropriate quality cont rol 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 in appropriate 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 defi ne 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 laboratori es to document these elements in quality system documentation and/or SOPs, the la nguage should be changed as follow s: "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 re quirements 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 la bs. Certified labs are already using voluntary2010 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 resp ective 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, NELA C/TNI, methods, etc.) To add another layer of redundant requirements in 40 CFR 136 is absolute ly 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 th eir QA/QC requirements. And labs are already used to referencing the methods for specific QC checks.

Besides the duplication of requirements, another probl em 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 reasonabl e and knowledgeable about the methods used in laboratories, some are not. Over the years, sin ce 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/Q C checks in every SOP and/or include a rationale as to why they aren’t relevant. This is counterproduc tive. 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 nationwid e) 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 ch ecklist to use without any clarification as to its limitations. That is why it is so important to wr ite 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 langua ge to 40 CFR 136. At most, a re ference 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 environmen tal 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 ex ist 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 insuffici ent 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 "c ould," and a regulated entity could decide that an absurd QC frequency of once pe r 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 w ould 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 demonstrat e 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 re quirements 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 regulator y requirement that could impact small government that does not have trai ned laboratory accreditation personnel to evaluate QA/QC procedures. PA-DEP LAP fully believes doc umented 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 a pplicable 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 al ternative, we propose that the laboratories be given the discretion to choose appropriate quality cont rol 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 in appropriate 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 a pplicable 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 N ELAC 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 clar ity on essential requirements. However, the proposed language at Part 136.7 lacks detail and as written, leav es these requirements subject to interpretation by labs, data users and auditors. Where specific re quirements exist in mandated methods, (e.g., EPA, ASTM or Standard Methods), these should apply. Howeve r, 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 lim ited 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 frequenc y 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 performan ce found in the EPA and other reference methods do not always indicate acceptable performance, such as pe rcent recoveries of zero to more than 200%. As long as the EPA methods allow for this type of perfo rmance, 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 perfo rmance then the method is not acceptable for regulatory monitoring.

The commenter does recognize that many EPA and othe r 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 m eet 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 a llow 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 gene rated from a technically competent organization that operates a management system that is consistent w ith consensus standards such as ISO//IEC 17025 or the TNI standards. This along with defined method perfo rmance for quality control checks (RPD < 20%, Bias 50 to 150%, Blank < LOQ) must be used to ensure da ta 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 rang e must never be reported for compliance reporting since the data is unreliabl e out side the calibration range. The reporting of2010 Methods Update Rule Response to Comments 144 March 2012 unreliable results for permits or compliance monitori ng 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 laborat ories and the demonstration of capability shows no comparison of techniques and reporting since the refe rence 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 th e National Environmental Laboratory Accreditation Conference (cf. Chapter 5 of the compendium published in 2003.)

The National Environmental Laboratory Accredita tion 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 N ELAC 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 frequenci es 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 s ource that does, such as Standard Methods or the TNI

standards.

The proposal also states that the quality control ch ecks 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 Saxon2010 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 labor atories 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 lim ited 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 qualit y control protocol in the methods themselves, as evidenced by the fact that they are in fact propo sed 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 el ements 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 cont rol elements along with performance specifications for each." SOPs should only include procedures and pr otocols that are relevant to the method to which they are written. For example, an SOP for microbiol ogy 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 qu ality control data sufficient to properly characterize method performance. EPA must not approve methods wit hout 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 s hould be no need for the proposed language.

EPA proposes addition of §136.7 specifying “essential” el ements of quality control (QC). The stated reason for doing this is to provide guidance in case s 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 char acterize method performance; that is, EPA proposes to add methods that have not been adequately validated.

Disregarding for a moment the utility of the twel ve 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 anothe r way, EPA should not approve any method that is not already supported by QC results suitable for characterizing method performance. The basis for2010 Methods Update Rule Response to Comments 146 March 2012 approving a method must be acceptable method perform ance as illustrated by relevant QC data (i.e., acceptance criteria or data sufficient to derive accep tance criteria for important/relevant QC metrics). Instead of adding a new section to the regulati on specifying essential QC elements, EPA should only approve methods that already incorporate these elem ents 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 eac h 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 ove rarching 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 ensu re that all analysts will perform the same checks in the same way. In the end, if EPA is concerne d about the quality of data developed using any approved method it will need to address data quality on a mo re 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 a ddition to initial calibration and method detection limit). Because these analyses are performed using spik ed blank matrices (e.g., laboratory water or sand), not real-world samples, the results provide an optimis tic measure of method performance. Certainly, if a competent laboratory cannot generate acceptable r esults 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 accura cy. 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). Ab sent an SRM, use of fortified ASTM substitute wastewater (ASTM D5905) would still be an impr ovement 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 laborat ory fortified blank duplicate for suspected difficult matrices - Because matrix spike analyses are pe rformed on real-world samples and laboratory fortified blank (LFB) analyses are performed on labora tory blank matrices they are not interchangeable, and results from LFB analyses do not effectively ch aracterize 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 char acterize 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 validat ed 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 metr ics. 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 an alysis), 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 inte rnal 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 th is is a less insidious issue than an interferent acting on an internal standard. Overall, NCASI fully supports a mandate to in corporate a surrogate or tracer in all analytical methods, but suggests that the use of internal standards be discretionary

. Control charts (or other trend analy ses of quality control results) - The use of control charts and so on to identify intra-laboratory trends is not a necessary co mponent 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 consider ed 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). Howe ver, much as is the case with respect to control charting, how a laborator y approaches troubleshooting is more appropriately associated with QA, and so is more correc tly considered to be part of laboratory

certification/accreditation.

QC acceptance criteria - The purpose of acceptance crite ria 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 differe nt quality). Thus, it is necessary that analytical data be generated from a syst em 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 cr iteria 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 differe nt 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 th at batch-specific QC derived from analysis of blank matrices (e.g., blank water) pr ovides 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 reporti ng 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 resu lts 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 pr ovide more detail on the specific QC checks proposed, it appears that EPA is conflating QC with the broa der scope of quality assuran ce 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 ar e 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 requirement s are general in nature and should provide specific exemptions for the following:

• The requirement for a method detection lim it (MDL) (QC requirement #2). A detection limit determination should only be requi red when results are reported below the quantitation limit. MDL studies are not appropriate for some parameters (p H, BOD, microbiological, etc.) In addition, EPA

should consider whether determin ation 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 essen tial 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 s uggest adding a section (c) after Section 137 (b) as

follows:

Proposed (c) addition - Quality assurance tests requiri ng 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, disso lved 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 organi cs analysis (QC requirement #6). We agree that internal standards should be required for GC/MS anal ysis, but they can be problematic for certain GC analyses that employ detectors such as FID, PID and EC D. It is possible to use internal standards with methods such as 602, 604, and 608 for some matri ces, 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 th is 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. Th e 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 th e difference between QC and QA so that the

laboratories understand that one is an action wh ile 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 guidan ce for DOC's, QC Acceptan ce, etc. This written requirement should include approved re ferences to help them to establish the information needed to meet this requirement. A reference to a known and appr oved standard such as the consensus standards published by The NELAC Institute (TNI) (specifi cally 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 requi rements that are essential to a solid foundational basis for a comprehensive QA/~ program.4. 136.7 (b) Th is statements should be more specific and we suggest the following language:

• For each analytical method, these twelve quality co ntrol checks must be clearly documented in a laboratory prepared Standard Operating Pro cedure (SOP), which must include established performance specifications relevant to method requi rements, where applicable. The procedure must include and describe the laboratory's specific a pproach 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 standa rds 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 sta ndard published by The NELAC Institute (TNI). Specific comments on the 12 essential quality control checks ar e provided later in this document.

Comment 171.1

Lola Guerra Henrico County DPU

Comment 1: This requirement is redundant. Essentia l, 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 m eaningful. Again, applicable and appropriate QC

measures are described in detail for individual methods.

Comment 4: This should not to apply to field m easurements and should be clearly stated as such.

Comment 5: The MDL concept is antiquated in the f act 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 anal yses 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 contro l at Sec.136.7 for use in conducting an analysis with an approved method and when insufficient inst ructions 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) a nd quality control (QC) procedures practiced by laboratories that use 40 CFR part 136 methods. So me 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 co mpendium 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 c ontrol requirements for all methods. Each specific Part and section can contain additional QA and QC re quirements (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 ac hieve the QA and QC expected for valid results... EPA is proposing at 136.7 to specify twelve essen tial quality control checks that must be in the laboratory's documented quality system unless a writt en 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 fa ils to address inconsistencies between different approved methods.

Recommendation: Consistent Quality Co ntrol is better addressed if the Ag ency 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 st andards 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 grou ping referenced. Making the list too general simply

invites further confusion a nd 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. Ho wever, we are not pleased with the lack of references for the 122010 Methods Update Rule Response to Comments 151 March 2012 elements listed in section 136.7.b. This will cr eate difficulties when assessi ng whether the provided quality assurance is sufficient. In addition, sever al 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 permitti ng agency prefers another. In this state in particular, the laboratory certification program h as commonly cited requirements from EPA’s Manual for the Certification of Drinking Water Laboratories ev en when reviewing labs conducting permit related analyses. The requirements in that manual diffe r 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 func tion 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 lan guage regarding QC requirements at 136.7, which auditors are very likely to want included to the gr eatest possible extent, within written methods (once this rule has been finalized). This ma y necessitate additional revisions, albe it editorial, continuing the cycle ...

USEPA has provided proper terminology for the twel ve 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) stat es: 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 perfo rmance 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 possi ble for us to maintain multiple copies of the methods that have the various requirements as part of the me thod in different regions or states Lachat customers I have spoken to state that the pass/fail criteria for a gi ven QC test are typically documented within a given

labs SOPs for each method. This is addressed on P580 36 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 docume nt this separation more clearly: "These twelve quality control checks must be clearly documented in the wr itten method. Each lab must also document current laboratory acceptance criteria (Le. the performance sp ecification) 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 EPA2010 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, Wisc onsin 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 Bo ttoms Regional Wastewater Treatment Facility Comment 158.1 - Jerry Parr, The NELAC Institute Comment 169.1 - Judith R. Morgan, Amer ican 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, in stead of 4.4. There was general support for the withdrawal of Appendices A and C, and some support fo r 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 futu re, even if they are withdrawn from the CFR. One commenter noted that if the withdrawal proceeds, th en 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 th e 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 cu rrent 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--Rev ision 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 cu rrent 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 ve rsion 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 sectio n 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 892010 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 underl ined 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 a ppendices 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 belie ve 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 Appe ndices 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 fo r 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 1232010 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 2 00.7. 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 suggesti on and may consider this change in a future rulemaking. The scope of the change is only app licable 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 rega rding 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 s ource 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 docum ent 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 met hods 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 extrac tion permits) to an alternate source, the full force and effect of law provided via the CFR will be dimini shed. Losing this critical piece of enforcement will weaken the permitting authorities’ ability to protect a nd conserve water resources at risk from the oil and gas extraction process.

Response: EPA disagrees with the commenter’s assertion th at 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 refere nce. For example, Table IB in 40 CFR 136.3 lists (not re-prints) the approved analytic methods for i norganic parameters. EPA works with the Director of the Federal Register to incorporate these analytic me thods 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 info rmation 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 th at this incorporation by reference procedure diminishes the enforceability of NPDES effluent limits derived from effluent guidelines. NPDES regulations at 40 CFR 122.44(a) a nd 125.3(a) require NPDES permit wr iters to develop technology-based treatment requirements and incorporate these limits as enforceable conditions in NPDES permits. NPDES permits issued to individual dischargers transform a ny generally applicable effluent limitations guidelines and standards, which are a type of technology-based tr eatment requirements, into effluent limitations that apply specifically to the individual discharger. S ee EPA v. California ex rel. State Water Resources Control Bd., 426 U.S. 200, 205 (1976). EPA has identifie d the failure of a permit writer to appropriately incorporate applicable technology-based treatment re quirements into enforceable NPDES permit effluent limitations as a condition for EPA disapproval of th e permit. See “Central Tenets of the National2010 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 wr iters incorporate the use of these approved analytic methods as enforceable conditions in permits. The inco rporation by reference of these approved analytic

methods in Part 435 means that these methods are in cluded 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 appr oved analytic methods incorporat ed by reference in Part 435 to demonstrate compliance with their permit.

In the final rulemaking EPA did not delete the anal ytic 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 Sour ce 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 a nd updates to current laboratory practice, provide important clarification, and address specific tec hnical 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 glass ware, however, should never be heated because the glass will expand, rendering the calibrations inaccurate.

Response: EPA disagrees with this comment. Glassware mu st 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 spectrom eter 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 change d 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 = [ │ D 1 -D 2 │ / ((D 1 +D 2 )/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 (M ethane Measurement) of GMG 290000 as well into the proposed methods manual EPA –821–R–09–013. This will en sure all relevant protocols associated with the marine anaerobic biodegradation anal ytic 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. Addi tionally, Appendix B-2 (Concentration Verification Analyses) and Appendix B-3 (Program Quality Assu rance 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 C 16 –C 18 Internal Olefin Drilling Fluid Formula tion and as such appropriately belongs within the proposed manual.

Response: EPA disagrees with this comment as the pro cedures provide a means to standardize the

formulation of a reference C 16 –C 18 internal olefin drilling fluid for use in determining the drilling fluid sediment toxicity ratio and compliance with the BA T 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 Me thod 1646, and the specific test procedures included in the NPDES permit for the Western Gulf of Me xico (“Final NPDES General Permit for New and Existing Sources and New Dischargers in the Offs hore Subcategory of the Oil and Gas Extraction Category for the Western Portion of the Outer Contin ental 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) pr ovides 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 th e drilling fluids toxicity test (EPA proposed method # 1619). OOC would prefer to see Appendi x 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 additi onal 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 allo w 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 need ed as permit writers may modify an approved EPA analytic

method as described at 40 CFR Part 136.6. The Ma rch 12, 2007 Methods Upda te Rule (MUR) that promulgated 40 CFR 136.6 allows the regulated commun ity more flexibility to modify approved methods without EPA review. This regulation allows the an alytical community greater flexibility to modify approved methods to lower the costs of measuremen ts, overcome matrix interferences, or otherwise improve the analysis without EPA review. Laborator ies that modify 40 CFR Part 136 methods may be private, public or commercial and may conduct an alyses 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)- Sta ndard 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 #42010 Methods Update Rule Response to Comments 159 March 2012 Response: EPA agrees with incorporating these additi onal 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)- Sta ndard 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 Proced ure for Mixing Base Fluids with Sediments

EPA Method 1646

Rationale: Same justifications as Comment #4.

Response: EPA agrees with incorporating these additi onal 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 a ppropriate 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 dete rgent 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, da ta to determine the effect of in corporating 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- a nd 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 samp le preservation temperature range. The change in mixing speed from “1000 rpm” to “1000 rpm to 2000 rp m” 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 a dded under Apparatus. Glassware cleaning procedure edited to include plasticware and updated to be consistent with the re quirements of U.S. Environmental Protection Agency, October 2002. Methods for Measuring the Acute Toxi city 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 seawate r 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 met hods, 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 pre servation 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/wa ter slurries can not be mixed homogeneously and measuring pH of these slurries is not practical. Afte r 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 drillin g 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 unf ilterable 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 whethe r this data is reported on the DMR. EPA requires2010 Methods Update Rule Response to Comments 162 March 2012 compliance monitoring data to be maintained by pe rmittees 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 Sec tion 3.5.5.6 more fully describes required water quality

measurements

Response: EPA agrees with commenter that this is re dundant language and h as 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. Da ily 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 de tergent 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, rin se several times with distilled or deionized water, place in a clean 10% HCl acid bath for a minimum of 4 h ours, rinse five times with tap water, and then

rinse five times with distilled water.

Rationale: Glassware cleaning procedure edited to incl ude plasticware and updated to be consistent with the requirements of U.S. Environmental Protecti on 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 b een 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 construc tion 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 ma de in all SPPs at 96 hours. Water-base drilling fluid SPP concentrations are usually very turbid preventin g observations until the test is terminated. Daily observations in water-base drilling fluid SPP concentrati ons 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 visually2010 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 handli ng 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 hour s.DO and pH measurements must also be ma de 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 taki ng 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 requi re that water quality measurements be made directly in the test dishes. Measuring water quality para meters 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 (N aCl), potassium chloride (KCl), cadmium chloride (CdCl2), copper sulfate (CuSO4), sS odium 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 numbe r, 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 test s, except that the test ma terial was prepared by weighing one gram of the reference toxicant sodium lauryl sulfate on an analytical balance

Rationale: To make this paragr aph 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 un til 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 unc ontaminated 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 dr illing 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 dens ity determinations and

addition of base fluid to control sediment. Becau se 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. Al l Base fluid concentrations are weight-to-weight (mg of base fluid to kg of dry control sediment). For test materials other than pure base fl uids (e.g., whole mud formulations), concentrations are volume-to-weight (mL of test substance to kg of dry control sediment. Sediment and base fluid test material mixing shall be accomplis hed by using the following method.

Rationale: These proposed changes clarify that EPA Me thod 1646 is applicable for amending natural orformulated 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 th e procedure development phase at each testing laboratory. Because of difficult y 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 replicat e test containers. Base-fluid content is measured as TPH. After mixing the sediment, a minimum of three re plicate sediment samples shall be taken prior to

distribution into test containers. After the test sediment is distributed to test cont ainers, an additional three sediment samples shall be taken from three test contai ners 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 re plicate samples must be less than 20%. If base-fluid content results are not within the 20% CV limit, additional TPH samples from freshly mixed sediments2010 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 th e 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 cont ainers shall be sampled to determine base

- fluid content during each sampling period .After their development phase, laboratori es 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 drilli ng fluids with sediment are require d 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 fl uids 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 paragra ph consistent with current EPA gui dance 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 Manage ment Practices consistent with Comment #33. See Comment #33.

Response: EPA disagrees with the commenter. EPA iden tified the use of BMPs are part of the technology basis for controlling NAF-cuttings disch argers. 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 Mana gement 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 (BMP s) 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/c ontradiction: 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.