1 United States Environmental Protection Agency

R esponse to Public Comments on Notice of Data Availability; Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act; Analysis and Sampling Procedures (76 FR 77742, December 14, 2011)

F ebruary 2013

I ntroduction

T he comments in this document are arranged by topic (i.e., A, B. 1, etc). Each comment has a unique number that is a shortened form of the docket assigned comment identifier . For example,

if the docket identifier was EPA

- OW -2010-0192-0229, that identifier has been shortened to

"C omment 229," followed by the commenter's name and affiliation

. Where EPA references a response to a specific comment, EPA means the response to that commenter within the topic. For example, under topic B.3, EPA’s response to Comment 246, includes “See response to comment 244.” In that case, EPA means the response to comment 244 in topic B.3. Comments

are included verbati m.

T able of Contents

A

. Support for ASTM Method D7575

B. Opposition to Approval of ASTM Method D7575 B.1 OSS is sole supplier B.2 Method comparison of ASTM D75 75 to Freon vs. n- hexane methods B.3 Sampling requirements and preparation B.4 Matrix spikes requirements B.5 Method detection limit (MDL) B.6 Method applicability

B.7 Infrared ( IR ) measurement B.8 Working range of method

B.9 Calibration

B.10 Membrane d rying

B.11 Method- defined parameters and comparability B.12 Analysis cost

B.13 Handl ing waste
B.14 Method v alidation

B.15 Unfunded mandate

B.1 6 Method version (ASTM versions and EPA Method 1664 versions) B.17 Green chemistry B.18 National Technology Transfer and Advancement Act (NTTAA)

B.19 Accuracy of v endor information B.20 Number of oil and grease analyses per year B.21 NPDES permit limit adjustment B.22 Replacement of EPA Method 1664 with ASTM D75752 B.23 Method portability B.24 Time required to perform test B.25 Use of chromatography in the test

B.26 Blank must be lower than the MDL

C. Other com ments
C.1 Using the same side

- by -side comparisons when switching from Freon to N- hexane for N

hexane to infrared analysis

C.2 Document availability C.3 Requests for approval of IDEXX method

C.4 Preservation C.5 Comment period extension C.6 Transparency

C.7 Duplicate samples C.8 Appropriateness of paint shaker in a certified laboratory C.9 EPA is purposely delaying a final ruling to allow a single method to “catch up”3 A. Su pport for ASTM Method D7575

Sum mary : Many commenters expressed support for approval of this method for various reasons

such as its green technology basis, ease of use and its portability. Other commenters also recommended the approval of ASTM Method D7066.

Comment 221 C. Tunick : While there is considerable interest in a solventless method for analyzing oil and grease in water, the current method is not field-portable and cannot be used for on-site measurements. It would be ideal for use in a laboratory environment but not for on- site use such as on off-shore and on-shore oil drilling platforms or in manufacturing industries using oil and grease in their process who want a quick, easy way to check their wastewater effluent prior to discharge without having to wait for lab results. There is a current ASTM Method D7066 using infrared analysis and S-316 as an extracting solvent for measuring oil and grease in water.

This method is based on the tried and true EPA Methods 413.2 and 418.1 which have been used and accepted worldwide for the measurement of oil and grease in water for over 30 years. If the EPA is to consider ASTM D7575-10 as an alternate analysis and sampling method, they should give serious consideration to also approving and accepting ASTM Method D7066 as an additional alternate method. Infrared analysis for measuring oil and grease in water is accurate, cost effective, and easy to use by both non-technical personnel and skilled technicians but provides a method that can be used on- site, as well as in the analytical or testing laboratory. Today, it is still the most widely -used method worldwide for measuring oil and grease in water.

Response : EPA acknowledges the benefits of D7575. However, for the reasons explained in the notice, EPA is not promulgating D7575 in Part 136 for nationwide use. The commenter did not provide any additional data or analyses that are at odds with EPA’s conclusion that it should not adopt the method for nationwide use.

EPA thanks the commenter for his/her comments on ASTM D7066. ASTM has not requested EPA to consider D7066 nor did EPA discuss it in its proposal. Thus, it is outside the scope of

this action

.

Additionally, EPA notes that Part 136 methods must be used for compliance with CWA requirements. Part 136 does not govern other uses. As such, if a facility or researcher would like to use either of these methods for non CWA uses, the lack of inclusion in Part 136 does not prevent them from doing so.

Finally, as is the case with all methods, if a permittee wishes to use a method that is not promulgated in Part 136 for CWA compliance, the authority exists under Part 136.5 to request

the use of an alternative method for a specific application (i.e. limited use ATP).

Comment 222 Robert J. Polis, Metro politan Water Reclamation District of Greater Chicago (MWRD) : Comment 1: The Metropolitan Water Reclamation District of Greater Chicago ("District") concurs with the EPA’s decision to reconsider promulgating method ASTM

D7575- 10 as an alternative (not a re placement) for EPA Method 1664A. Additionally, pending further instructions from the EPA, the District would consider using ASTM D7575-10 after the useful lifespan of its existing equipment – used for method 1664A determinations – has expired.4 We applaud t he EPA’s continued diligence in considering green initiatives that will either minimize or eliminate the use of solvents in analytical procedures and the analysts’ exposure to

these solvents. Comment 2: The District likewise concurs with the EPA’s conclusion that permit limit adjustment based on side- by -side comparisons of EPA Method 1664A and ASTM D7575-10 is not appropriate.

Comment 3: If the EPA allows side

- by -side comparison of EPA Method 1664A and ASTM D7575-10 to establish a conversion factor, then the approach should be similar to the one used when the EPA promulgated EPA Method 1664A (which uses n-hexane as the solvent) to replace EPA Method 413.3 (which used Freon as the solvent).

Response : For the reasons specified in the notice, EPA has decid ed not to adopt this method for

nationwide use. Similarly, i n response to the second and third comments on the use of a conversion factor, EPA is not allowing the use of the permit limit adjustment, nor is EPA allowing side

- by

- side comparisons between EPA Method 1664A and ASTM D7575 to establish

a conversion factor.

Comment 223 Curt McCormick : The following comments are respectfully submitted on the following FR request for comments: Guidelines Establishing Test Procedures for the Analysis

of Pollutants Under the Clean Water Act; Analysis and Sampling Procedures; Notice of Data Availability Federal Register / Vol. 76, No. 240 / Wednesday, December 14, 2011 / Proposed Rules. Page 77742

- 77747. I am very impressed EPA has moved aggressively on this and sought to approve this alternate method while dealing concurrently with other important rulemaking activities.

Response : EPA thanks the commenter for his support.

Comment 224 Sandra Rintoul, Wilks Enterprise : Having a solvent- less oil and grease method would be a benefit. However, many applications of oil and grease analysis are improved by having an on-site method for quick results. Sending samples back to a laboratory can add costly delays both environmentally and economically. Both ASTM D7575 method and current EPA 1664 method require equipment that is not amenable to on- site (or offshore) analysis. ASTM D7066 is an infrared method that only differs from EPA 413.2 and 418.1 in the non-CFC solvent

that is used for extraction. The EPA should consider ASTM D7066 as well as ASTM D7575 as

alternate methods to EPA 1664.

Response : See response to comment 2 21.

Comment 225 Yarden : The ASTM D7066 and the ASTM D7575 would provide far superior advantages to the EPA 1664. These would allow portable, solventless methods where no enviromentaly harmful methods would be used. Such methods would also allow its application with no need of skilled laboratory technicians and costly lab environment.

Response : See response to comment 2 21.

Comment 226 Wilks (no name prov ided) : Many applications of oil and grease analysis are improved by having an on-site method for quick results. The solvent-less D7575 method like5 EPA 1664 requires cumbersome sample handling which is not ideal as an on-site method. The

on- site methods can avoid economically and environmentally costly delays which could be incurred while waiting for off-site results. D7066 was developed specifically for either on- site or laboratory use. ASTM D7066 is an infrared method that only differs from EPA 413.2 and 418.1

in the non-CFC solvent that is used for extraction. The EPA should consider ASTM D7066 as

well as ASTM D7575 as alternate methods to EPA 1664.

Response : See response to comment 221.

Comment 227 Dr. Rob Leishman, Western Resource Recovery, Western Australian DEC : I

would be most interested to see a solventless method alternative for the determination of FOG. Please give D7575 consideration as an alternative method for this determination.

Response : ASTM did not submit D7575 for consideration for the measurement of FOG, nor did EPA’s proposal discuss D7575 as a method for the measurement of FOG. Thus, this request is outside the scope of this action. Also see response to comment 221.

Comment 228 On behalf of Pensalab : 1. The solvent-less D7575 method like EPA 1664 requires cumbersome sample handling which is not ideal as an on-site method. D7066 was developed specifically for either on -site or laboratory use. 2. On-site methods can avoid economically and environmentally costly delays which could be incurred while waiting for off- site results 3. D7066 is based on well-established EPA 413.2 and 418.1 methods, used worldwide for over 35 years. The primary difference is the use of in the non-ODS solvent in D7066 for the

extraction.

Response : See response to comment 221.

Comment 229 Anonymous : As a soil chemistry researcher working in the area of oil

- based drilling mud, it would be very helpful if the ASTM D7066 and D7575 were approved as alternatives to EPA 1664. The D7066 method is a suitable alternative in regard to TPH and is much easier, fa ster, and cheaper than a GC method. Such an approval would allow us to conduct MUCH more research on the impact of oil -based drilling mud on soil quality and environmental

risk. Please consider that the D7066 method is a well established infra-red method based on EPA 413.2 and 418.1 methods, but utilizes a non ozone depleting substance during extraction.

Response : See response to comment 221.

Comment 230 L. LaRusso : While the solvent-less D7575 is good for laboratories, it would be advantageous to have and include as an alternate method D7066 for on- site infrared analysis.

Response : See response to comment 221.

Comment 231 Rebeca Rondón, Corporación Científica Venezolana : The EPA 1664 should

considerer the ASTM 7066 as well ASTM 7575 because the first one is very similar to EPA 413.2 and 418.1 and it could be used on site; that is one of the most important things to have in6 this kind of instruments. The D7575 is very attractive because it is a solvent- less method, but it is important to have another economic an easy method to do the same test.

Response : See response to comment 2 21.

Comment 232 Glen Blackstock, Micron Scientific Pty Ltd

. : On behalf of our existing customers and prospective customers using solvent extraction technology for TPH and FOG analysis in the field we request that the EPA consider both ASTM D7066 as well as D7575 as

alternate methods to EPA 1664. The Wilks InfraCal is a popular, potable analyser used for in field analysis of oil and fat

in water. If the EPA omit the solvent ext raction technique as a method, current users and prospective users will be hugely inconvenienced. Many laboratories would need to purchase new technology to perform the analysis which takes long purchase cycles and there will be long sample result periods while waiting for results from laboratories.

Response : See response to comment 2 21. Also, EPA is not considering removing the promulgated n-hexane methods for measuring oil and grease.

Comment 233 Michael Travers, VHG Labs : I would like to see ASTM D7066, as well as ASTM D7575, as an alternative method to EPA 1664. D7066 is ideal for quick on- site analysis of waste water effluent prior to discharge. It is an IR method that uses S- 316 as an extracting solvent for measuring oil & grease in water. It is commonly used and is based upon EPA Methods 413.2 and 418.1 which have been accepted for many years.

Response : See response to comment 2 21.

Comment 234 Anonymous : It would be beneficial to have an on- site method available such as ASTM D7066 to perform IR analysis rather than sending to an outside lab for testing.

Response : See response to comment 221.

Comment 235 Shanta Ramkissoon Cruickshank, ROSE Environmental Limited : Although having a solvent-less method for TOG analysis has its benefits it does not offer portability or quick field measurements capability. There is an ASTM Method D7066 using infrared analysis and a non-CFC solvent (S-316) for measuring oil and grease in water that correlates closely to the EPA 413.2 and 418.1. In an effort to promote environmental sustainability the EPA should acknowledge the ASTM D7066 and consider this as well and the ASTM 7575 as alternate

methods to EPA 1664.

Response : See respon se to comment 221.

Comment 236 Donald Lavery and Associates : ASTM D7575 - 11 Standard Test Method for

Solvent- Free Membrane Recoverable Oil and Grease by Infrared Determination is an appropriate choice for inclusion as an EPA alternate method. It does, however, require rather cumbersome equipment and the analysis is quite time consuming. The much simpler and quicker ASTM D7066 that uses S-316 solvent extraction will often be preferred where space is limited and7 analysis time is important. Adoption of both of these ASTM methods as EPA alternate methods would be appropriate.

Response : See response to comment 2 21.

Comment 256 D. Smith : EPA's requirement to test the amounts of oil and grease sample should require only green testing if the proper tests exist. In the instance for oil and grease, the green validation test exists and should be extensively used. These green tests have met established criteria for accuracy, in addition they are far easier to perform as I have actually performed oil and grease tests in laboratories years ago. I believe at this time our resources need to be conserved and contamination needs to be limited as much as possible.

Response : See response to comment 221.

Comment 258 Anonymous 24 : The major reason for seeking an altern ative to EPA1664 is the removal of hexane from the method, therefore ASTM Method D7066 using infrared analysis and

non- cfc non

- hexane S -316 as the extracting solvent seems more suitable. ASTM Method D7066 is based on the well established EPA Methods 413.2 and 418.1, it is a method that offers rapid on site measurements performed by non technical personnel and produces repeatable results that correlate well with EPA1664. ASTM Method D7066 is most widely used oil and grease method

worldwide and should be cons idered alongside ASTM D7575 -10 as an alternative to EPA1664.

Response : See response to comment 221.

Comment 270 E. G. Roy, Ph.D., Senior Scientist, OSS Inc. : The purpose of this comment is to reflect on the reactions from the independent labs that I trained during the single and multi laboratory validation and demonstration studies. In each case, the laboratory personnel were initially skeptical of D7575 technology, due to the simplicity of the process when compared to EPA 1664. However, after each 2 day test sessions, all technicians and analysts repeatedly commented on the advantages that D7575 has over EPA 1664 including: 1) D7575 does not require the use of a hood, while 1664, occupies a hood for a batch of samples while the hexane evaporates. This w as of particular importance to the smaller labs, where hood space is limiting 2) D7575 does not require solvents, and therefore does not require flammable storage or waste disposal. The technicians were also pleased that they were not exposed to a hexane, a

known neurotoxin. 3) The amount of technician effort per sample is much lower for D7575 when compared to EPA1664 or 1664A, raising the overall efficiency of the contract laboratory. In each case, the technicians were blown away by the number of sampl es that they were able to process in a <16 hour period (including training). Furthermore, the technicians noted that all pieces of the method that touch sample were disposable, thus eliminating the need to wash glassware and the possibility of contaminatio n from carryover. 4) Because D7575 is much simpler than EPA 1664, there are fewer opportunities for human error throughout the analytical process.8 5) Because D7575 requires a much smaller volume than EPA 1664 (10 mL vs 1000 mL), the contract lab manage rs and QA/QC officers liked that the remaining sample could be reanalyzed if something went wrong or could be saved as proof of a violation. 6) Because the equipment used in D7575 has a small footprint, spill response personnel appreciated that the techn ology could be deployed in a mobile laboratory.

Response : See response to comment 221.

Comment 272 Rachel Gettings, Orono Spectral Solutions : I am currently employed as a research technician by OSS and was brought on after the development of the ASTM D7575 method. I have had many opportunities since to run the method, both running figures of merit samples and many different real world samples. I have found the new technology to be simple and reliable, requiring minimal time and equipment. Using ASTM D7 575, I have processed a higher number of samples in a shorter period of time than with the current LLE method. As a research technician, being ableto process multiple samples quickly and accurately is a necessity and the ASTM method allows for this when a large number of oil and grease samples arrive. In addition to faster sample processing, there is very little prep -work and clean-up involved with the ASTM D7575; compared to the LLE method where apparatus set-up and waste disposal can become very time cons uming. The ASTM method uses cheap, disposable parts and does not require a series of complicated steps to process a single sample. As an advocate of green chemistry I also appreciate that the method is completely solventless and does not involve significan t exposure risks to the neurotoxin n-Hexane like the current EPA 1664 method does. I hope for the safety and ease of use of all the other technicians out there that ASTM D7575 soon

becomes available!

Response : See response to comment 221.

Comment 273 Jack Hall, Chairman ASTM D- 19 Committee on Water Methods : I strongly support the acceptance of the USEPA of the ASTM Method D7575 as a valid method for Oil and Grease since it is able to replace use of any solvents and has performed very well in comparability studies to the current method. The USEPA must be responsive to new technology to assure the public that approved methods are the best that are available. I support the letter

from ASTM which I have attached.

[ EPA Note: The ASTM letter from ASTM to EPA d ated 6/28/11 attached to the comment is not included here.]

Response : See response to comment 221.

Comment 275 Peter Rush, Portland Water District Portland Maine : The Portland Water District participated in an inter laboratory study in August 2009 using OSS solvent less oil and grease method. The driving force behind our interest in this method is the elimination of hazardous solvents. We had in the past performed oil and grease in our utility laboratory by EPA Method 1664, but found the added expense of disposing hazardous waste solvent prohibitive. Portland9 Water District considers the environment in all of its decisions therefore the green nature of this

method is an added attraction. We found the method proposed by OSS to be straight forward and fo llowing their standard operating procedures one that could be done with a minimum of training. The results obtained by the OSS method were comparable to the previous method used. Based on our experience, we would recommend acceptance of this method.

Respo nse : See response to comment 221.

Comment 282 Anonymous : I was personally involved in some of the early testing of OSS's ASTM D7575. Our lab was utilized in several ways. We supplied samples for them to analyze to compare results that we determined by 1664. We tested samples that they sent to us using our

own Ho rizon Oil & Grease machine. I was invited to their facility to observe their method first hand, as well provide insight and concerns. I would like to comment on my experience with

ASTM D7575. Given my own choice, I would personally prefer to be extracting and analyzing oil and grease sample by way of D7575. First of all, D7575 is a much more environmentally friendly and green method. This method eliminates the use of n-Hexane, which poses environmental and health concerns. With our instrument, if samples are especially dirty or there is not a perfect seal in a bottle cap, sample can leak out onto the counter, creating a hazardous mess. Part of my job is to dispose of hazardous waste. Oil and grease samples are generally received in duplicate. Once

the anal ysis is completed, we have an extra 1 liter bottle of sample preserved with sulfuric acid. Samples for D7575 could potentially be sampled with a simple disposable syringe. That would eliminate almost all of the sample waste and reduce the amount of contain er waste for 2 bottles to a small syringe. Our instrument takes up a lot of counter space and must be vented due to use of solvents. D7575 takes up much less space and could be portable. D7575 has also been determined to produce equal or better results in a fraction of the time. When we run a full batch of samples using 1664, it takes a full day of extracting and drying. Using the D7575, I was able to complete an entire batch in only a couple of hours. Using 1664 produces an MDL of 5mg/L can reached. D7575 produces results of 1mg/L. In summary, D7575 produces better, more efficient results without the hazards of 1664. D7575 creates less waste, is safer, and is easier to

use than 1664.

Response : See response to comment 221.

Comment 284 Charles Voinche, Petr oleum Laboratories, Inc. : The proposed ASTM D7575- 10 method may be a good alternate method to EPA 1664, it appears functional for research and testing laboratories use, but is far from having realistic application for field analysis, such as in the offshore oil and gas industry. If EPA grants alternate method status to ASTM D7575-10 it should realistically also approve ASTM D7066 method as an alternate method. The ASTM D7066 method is similar to ASTM D7575-10 method in that they both use IR technology. The existing EPA 1664 method uses a solvent with gravimetric finish, ASTM D7066 method uses a solvent with an IR finish, and ASTM D7575-10 uses no solvent with an IR finish, but may not be a viable candidate method for field application, all things being considered.

Response : See response to comment 221.10 Comment 285 Joe Boyd, Environmental Express : We at Environmental Express support the adoption of method ASTM D7575 in an effort to allow for the use of "greener" methods for various types of analyses. Supporting documentation shows that ASTM D7575 provides equivalent data results when compared to EPA Method 1664 and has many advantages, namely eliminating harmful solvents used in the 1664 method. The EPA has begun to support alternative technologies used in existing methodology to help laboratories reduce costs as long as results produced using th ose technologies are reproducible with the validated technology. This philosophy has helped numerous laboratories streamline their analyses and provide better data to their customers. The next step in method flexibility should be the allowances of techno logy that makes the analysis more friendly to the environment. Laboratories often test for pollutants yet create environmental hazards themselves while doing so. Any new technology that can eliminate or greatly reduce these hazards should be supported by the EPA and the regulatory community.

Response : See response to comment 221.

Comment 286 R. Schumann : When studying the effects of oil spills on marine life, having an

alternate on

- site EPA method is critical if spill offenders are to be targeted for responsibility for low levels of oil that could be detrimental to marine species. Neither the current EPA 1664 method nor the proposed D7575 method are field portable. D7066 has been in operation for 8 years and we have found this to be a suitable on- site meth od. We would ask you to consider making D7066 an alternate method as well as D7575 for those of us who are down in the trenches doing oil in water analysis.

Response : See response to comment 221.

Comment 305 B. P. Eynon : I am a professional statistician with over 30 years of experience in applying statistics to the environmental and biotechnology fields. In the early 1990s I was a statistical consultant to the US EPA Office of Water and provided statistical and data analys es of laboratory measurement data for Oil and Grease in the EPA Freon Replacement studies, including the Phase 1(US EPA, 1993), Phase 2(US EPA, 1995) and Validation (US EPA, 1995) studies that led to EPA Method 1664A (US EPA, 2000), in work done through SR I International and Dyncorp/VIAR (EPA Sample Control Center). These analyses formed the basis for the statistical tests of equivalence between analytical methods that is presented in the Analytical Method Guidance for EPA Method 1664A Implementation and Use (40 CFR part 136) (US EPA, 2000). I am writing today to support EPA’s proposal to approve the ASTM D7575-10 Solventless Oil and Grease method as a substitute for EPA Method 1664A. In light of previously submitted data and analyses I concur that the dem onstrated substantial agreement of the two methods in addition to the provision of solventless / greener alternative to the use of environmentally unfriendly and hazardous n-hexane used in EPA Method 1664A provide a more than sufficient justification for t he acceptance of ASTM D7575 -10 as an alternative method for

measurement of Oil and Grease.

Response : See response to comment 221 and 232.11 Comment 308 J. Betts : I am pleased to see a more environmentally responsible method proposed for analysis of "oil and grease", specifically one that does not use the dangerous solvent, n-hexane. Working with organic solvents is costly with respect to hazard training, permitting and management and is an unnecessary risk to human and environmental health. As an individual that has worked in the biofuels industry dealing specifically in lipid extraction and analysis, I am intimately aware of solvent hazards and the necessity for improved methods.

Response : See response to comment 221.

Comment 309 Anonymous : We believe t hat EPA should endorse multiple methods for oil and grease based on different extractants and determinative techniques than EPA Method 1664A. Reason 1: EPA 1664A is not suitable for all kinds of oil. Oils with low boiling point (e.g. condensates) are lost during the distillation step. This leads to underestimation of oil and grease

values in these cases.

Reason 2: New methods or technologies, better suited for oil and grease detection, should not be finally excluded due to a necessity to follow existing standards. The goal should always be to implement the best available technology (BAT).

Response : See response to comment 221.

Comment 315 Cam ille Turcotte, Wisconsin Department of Natural Resources : Issue 1. Yes

for the same reasons listed

Issue 2. Yes for the same reasons listed. [EPA Note: These comments are in reference to the 4 NODA request for comment issues. For issue 1, the commenter refers to whether EPA should promulgate this method. The commenter agrees with EPA’s reconsideration. For issue 2, the commenter agrees that the ASTM method is an acceptable choice.]

Response : See response to comment 221.

Comment 316 Thomas Schwarz, Research Scientist, Orono Spectral Solutions : I have worked for OSS throughout the entire development of ASTM D7575. During the Validation phase, it was my job to install equipment and train laboratory personnel on the proper procedure

for ASTM D7575. Befo re training, laboratories were provided with a copy of the method as well as an operating procedure for the equipment. At the end of a single day of training, laboratory end users were proficient at performing the method, and were able to autonomously

demo nstrate all of the figures of merit (calibration, detection limit, precision and recovery) required to perform ASTM D7575. In most cases, the analyst performing the method had little (if any) experience with infrared spectroscopy. In every case, the analyst finished the training with proficient understanding of the IR techniques needed to make accurate measurements of the IR absorbance peak used by ASTM D7575 to quantify Oil and Grease in a water sample without the help OSS personnel. One IR technique that was especially important was determining when the extractor was sufficiently dry enough to provide an accurate Oil and Grease measurement. As is outlined in the Operating Procedure, the analyst was trained to able to identify the IR peak in the spectrum12 associated with water on the extractor membrane. If the water peak interfered with quantification of the Oil and Grease peak, the analyst was trained to dry the extractor further

and rescan the extractor. When the water peak was reduced enough so that it no longer interfered with accurate quantification of the Oil and Grease peak, it was considered dry. This iterative drying procedure is analogous to a similar procedure found in section 11.4 of EPA

1664. In the procedure for EPA 1664, the extracted sample is heated to 70°C and weighed iteratively until no more significant weight loss is detected with no strict limitations on drying time. In the case of ASTM D7575, if there was a correla tion between extended drying time and lower analyte recoveries, it would have been reflected in the validation data, but this simply was not the case. In a final related note, in the time since the validation studies were completed,

extensive work has been conducted into developing automated software for the IR analysis step of the procedure. An automated software platform will be capable of determining dryness and quantifying the Oil and Grease peak without any intervention from the user. This software

pac kage eliminates the requirement for laboratory personnel to learn IR techniques to

conduct ASTM D7575. On the second day of validation testing, laboratory personnel autonomously processed the provided samples. It is important to note that OSS employees were not present for the testing of matrices during the single lab and multi lab validation studies for ASTM D7575. Once the analyst was properly trained, all data generated and reported in the validation study was produced by independent analysts without the help or influence of OSS personnel. Analysts were able to complete all of the testing in less than a day. At the end of the study, the only waste that had been generated was the solid waste (e.g. used extractors, syringes, paper towels, gloves) and aqueous waste from the tested samples. In the case of both ASTM D7575 and

EPA 1664, the aqueous waste can be neutralized and disposed of. ASTM D7575 does not
generate any more aqueous waste than EPA 1664. An alysts were generally pleased with the easy cleanup associated with ASTM D7575. There was very little (if any) glassware to clean and no solvent to dispose of. Analysts also expressed overwhelmingly positive sentiment regarding the ease of the entire testing process compared to EPA 1664, which could have easily taken over a week to complete the training, compliance verification, and sample testing that was completed in less than two days with ASTM D7575.

Response : See response to comment 221.

Comment 317 Ray A. Morales, Naval Surface Warfare Center Carderock Division (NSWCCD) : We are the In

- Service Engineering Agent (ISEA) and Life Cycle Managers (LCM) for Oil Water Separators (OWS) and Oil Content Monitors (OCM), installed onboard almost all US Navy surf ace ships. Navy policy is to use EPA approved methods for oil- in -water determination. However, the current EPA Method 1664A has many limitations for our application, especially for shipboard evaluation of OPA systems. Navy ships are all over the world and EPA Method 1664A definitely is not a field method. Transporting n- hexane all over is almost impossible due to hazardous material restrictions. Likewise, collecting, preserving, and shipping samples may not be practical in long ship's deployments.

Our l aboratory participated in a field trial of ASTM Method D7575-10. This method was easy to use, faster than EPA 1664A, did not required specialized equipment other than the solid phase extraction membranes and the IR that we already had, and do not use any hazardous materials. All the instrumentation and material required for this method are easy to transport for13 field application. ASTM D7575 is within our measurement range of interest (5 to 200 mg/L). Some samples of known concentrations were prepared at the laboratory and others were taken from our test stand for this trial. Not enough samples were taking for a comprehensive statistical analysis. However, the results obtained during this field trial suggested that this method is equal or better for our application that EPA 1664A. Based on the above narrative, we recommend EPA to promulgate ASTM D7575-10 in 40 CFR Part 136 as an alternative method to EPA Method 1664A for oil and grease determination. However, EPA should establish clear guidance to determine whether or not to consider future requests for other methods. [EPA Note: The following text is from the attachment to the comment . The second and third paragraphs of the attachment are not included here, as they are verbatim to the second and third paragraphs, respectively, from the comment (above) .]

We are the In

- Service Engineering Agent (ISEA) and Life Cycle Managers (LCM) for the Oil Pollution abatement (OPA) systems, including Oil Water Separators (OWS) and Oil Content Monitors (OCM), installed onboard almost all US Navy surface ships. The OWS system is install onboard Navy ships to treat the oily wastewater generated in the machinery spaces, while the OCM monitors the OWS overboard discharge to ensure compliance with the applicable regulations, currently not to exceed 15 parts per million (PPM). As part of our responsibilities, we conduct both, laboratory and shipboard test and evaluations of OWS and OCM systems.

R esponses to specific EPA comment requests are as follows: 1. Whether EPA should reconsider promulgating this additional method for oil and grease based on different extractants and determinative techniques than EPA Method 1664A. COMMENT: Based on the above narrative, we recommend EPA to promulgate ASTM

D7575-10 in 40 CFR Part 136 as an alternative method to EPA Method 1664A for oil and grease determination. 2. EPA's current view, based on the data it has reviewed to date, that ASTM D7575-10 is an acceptable choice for the determination of oil and grease for the range (5 to 200 mg /L) evaluated. COMMENT: Based on the information provided, we concur with this EPA's view. However, EPA should establish clear guidance to determine whether or not to consider future requests for other methods. 3. EPA's current conclusion that permit li mit adjustment based on side

- by -side comparisons of EPA Method 1664A and ASTM D7575-10 is not appropriate. EPA is particularly interested in obtaining comments from permitting authorities on this issue and estimates of the burden associated with reviewing such requests. COMMENT: No comments. We are not a permitting authority, nor are we directly responsible for a discharge permit.

4. If EPA were to allow a side- by -side comparison with limit adjustment as necessary, should EPA look to the approach used for n-hexane in place of Freon (see section III.C) or should EPA consider a different approach?

COMMENT: No comments.

Response : See response to comment 221.

Also, many of the applications specified by the commenter are not for CWA compliance, and there is nothing in Part 136 which prevent these uses. Modifying Navy policy is outside the scope of this action.14 Comment 319 Patsy Root, IDEXX Laboratories : Overall, IDEXX applauds the pursuit of methods, such as D7575

- 10, that are more “green” and remove health hazards for lab personnel.

We appreciate the opportunity to be part of this process and hope to continue to partner with the EPA, and other stakehol ders, in the protection of public health and our environment.

Response : EPA thanks the commenter for her view.

Comment 320 Rebecca Labranche, A & L Laboratory Inc. : During my participation in the laboratory trials for the ASTM D7575 method developed by Orono Spectral Solutions I found the method very easy to understand and execute. With only minimal training I was able to learn how to operate the instruments and proce ss the analysis on several samples. I believe that the method would be a valuable alternative for laboratories mainly because it is solvent- Free and

eliminates the use of n -hexane a known neurotoxin. Reducing exposure to n- hexane and eliminating hazardous waste would significantly reduce laboratories impact on the environment and help to improve the quality of health within the laboratory. The data supplied by the validation studies show that the infrared method produces results equivalent to those of the current EPA method 1664. The potential use of a more “green” method would be an attractive alternative for many laboratories. In a time when the EPA is striving to regulate chemicals for both the Clean Water and Clean Air Acts the removal of a regulated contaminate from any method is a step in the right direction. I hope the EPA will consider the approval of the ASTM D7575 method for use in the measurement of Oil and Grease and help laboratories reduce their impact on the environment.

Response : See respons e to comment 221.

Comment 323 Mark Citriglia, Manager of Analytical Services NEORSD : The Analytical Services department of the Northeast Ohio Regional Sewer District participated in field

- testing of

Solvent

- Free Membrane Recoverable Oil and Grease by Infrared Determination (ASTM Method D7575). The laboratory tested a wide variety of sample matrices including influent and effluent samples from three of our wastewater treatment facilities, and industrial waste samples. The method performed extremely well on all samples collected from our final effluent of our wastewater treatment facilities and samples containing less than 50 mg/L of total suspended solids. One recommended enhancement to the method would be the ability to use various syringe sizes from 5m l to 50ml. Using a larger sample volume for treated effluent samples decrease the method detection limit. The smaller syringes would make dilutions more

accurate. The method performance decreased and the time for analysis increased with samples having suspended matter greater than 500mg/L. The higher the suspended mater or turbidity of the sample made it much more difficult to obtain a representative sample. Additionally samples with highly complex matrices required multiple analyses which increased analysis time and cost. The most difficult sample to analyze using this method were those composed of industrial waste or waste with high concentrations of oil grease. Our recommendation would be to accept this method for use under the Clean Wate r Act for samples containing less than 50 mg/L of total suspended solids. For samples containing greater than 50mg/L of total suspended solids would require additional quality control such as duplicate or triplicate analysis to address sample variability. Another option15 would be to require duplicate analysis for every sample with a relative percent difference requirement. Additionally not using the hazardous solvent n- hexane reduces waste disposal costs and reduces risk to employees. Having a smaller sample volume for analysis allows for retaining sample for reanalysis if needed.

Response : See response to comment 221.

EPA notes that while the method currently specifies a 10 mg/L

, EPA agrees that smaller or larger samples could be used provided the acceptance criteria of the method are met.

EPA appreciates the comments on TSS but notes the commenter provided no data to support its assertion so EPA can not offer guidance on this to pic for specific uses.



### B. Opposition to Approval of ASTM Method D7575

Summary: Many commenters opposed the approval of this method for various reasons such as the use of proprietary materials, differences with the approved method, and a number of technical reasons. The comments are grouped below by general area of concern.

B. 1. OSS is the sole supplier

C omment 245 Anonymous : In considering the proposed ASTM 7575 method as an alternative to method 1664, I see that Orono Spectral Solutions is the only current supplier of this hardware / equipment. The EPA states in most of their methods that it does not desire to promote any one product over the use of another. Seeing that there is only one producer of the technology mentioned in ASTM 7575, this, by default, violates the EPA policy on non- promotion. If a new method is to be proposed, I think it only fair that the method be approved when other vendors have entered the market, and the end user has several choices of vendors. Until that time, I suggest this method not be allowed.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of

this method for a limited use through existing authorities in 136.5 , EPA is providing a response.

However, EPA approves test methods but does not endorse vendors. Even though the ASTM

method specifically states in footnote s 5 and 6 that the only known source of the apparatus is Orono Spectral Solutions, it also indicates that it will consider alternative suppliers. The same policy has been adopted by EPA in the past. An EPA method may refer to one or more suppliers for a specific pi ece of equipment or standard but it also adds “or equivalent” so that alternative suppliers could be used if and when available.

Comment 257 Anonymous : With regards to including ASTM D7575- 10 as an acceptable alternative to 1664, I find myself appalled. In reading the method I find that i t is written specifically to cater to Orono Spectral Systems as there are no other manufacturers for the products required for this test. In almost every EPA method that I have read there is a disclaimer16 stating that EPA does not wish to promote any one manufacturer of a particular product (whether its a consumable or a piece of equipment), however they are willing to make an exception when an investor in the company used to work for EPA? Does this not violate EPA's own po licies?

Response : See response to comment 245.

B. 2. M ethod compar ison of ASTM D7575 to Fre on vs. n-hexane methods

Co mment 254 Anonymous : This might be getting picky about the proposed 7575 method, but in Section 17 of the method, it mentions that the results were compared to those of 1664. Based on the information available, the average recovery as a percentage of EPA Method 1664 was 94%. It was stated in the Federal Register Vol 76 No 240, that hexane was found to extract 96% of the oil and grease that could be extracted by Freon. This means that the total error is somewhere along the lines of 10% from the original Freon method. For this test to be valid, the results should be compared to the original Freon method, so any errors are not compounded. If this is done and the results still show merit, than it might be worth reviewing this proposal again.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of

this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA disagrees. The current approved method has been in use since 1999 and EPA’s policy is to compare candidate test methods to a currently approved method. The Freon method was withdrawn years ago and thus it is not appropriate to compare ASTM D7575 to th at method.

Comment 271 Debra Waller, NJDEP : Side by side comparison appropriate? Freon or n

hexane? T he NJDEP agrees. Since there are changes to both the extraction and determinative steps, a straight forward comparison may not be successful. However similar to the removal of

Freon and the switch to n

- hexane, this method may not yield comparable results and could cause permittees currently in compliance with any NPDES permit limits to become non

complaint. So the method comparison when done sho uld be against hexane and not Freon and permittees with difficult matrices should be given special considerations as a result of the change in the determinative step and extraction. Thank you for the opportunity to comment.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA agrees with the commenter in that the method may not yield comparable results in all cases and that method comparison should be done agains t hexane and not F reon.

Comment 296 Anonymous : In section 17 it is mentioned that the results of the ASTM D7575- 10 method were compared to those of the 1664 method. Based on the data available in this method, the average recovery on the different matricies as a percentage of 1664A is 94%. As it is stated in the Federal Register Vol 76 No 240, "n-hexane was found to extract 96% of the total oil17 and grease that could be extracted by Freon". This means that the total error is somewhere along

the lines of 10% f rom the original Freon method. For this test to be valid, the results should be compared to the original Freon method so that the errors are not compounded. Until that data is available, I would not recommend that this method be included as an alternative.

Response : See response to comment 254.

Comment 315 Camille Turcotte, Wisconsin Department of Natural Resources : [ EPA note: The comments are in reference to the 4 NODA request for comment issues. ] Issue 3. No the EPA should allow side by side comparisons and permit adjustment based on those results as we know the method provides 20% lower recovery

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for

nationwide use. [ EPA Note: The commenter does not agree with a blanket approval and recommends side by side comparison.] EPA is not in agreement with the commenter statement regarding the lower recovery of the ASTM compared to EPA Method 1164 . Please see Table 2

in the ASTM method and Section 17.0 Table 1 for the recoveries

.

Comment 318 ASTM D19 SUBCOMMITTEE ON D7575 : Commenters have discussed that ASTM D7575 development testing should have been compared to Freon. Response: Freon is banned. EPA 1664 was the method of record during ASTM D7575 development. EPA was involved in the development and approval of test plans and matrices.

Response : See response to comment 254.

B. 3. S ampling require ments and preparation

C omment 244 Anonymous : I was just made aware that the EPA was considering the proposal of the ASTM 7575 method for Oil and Grease, and felt compelled to respond. There are many parts of the method which I strongly disagree with, but here is one observation.

In N ote 10, it states that if the sample (10 mL volume) plugs the extractor (which I guess means the filter) that a smaller sample size should be used, or alternatively, dilute the sample (I guess so it will flow through the filter?), and re -run the analysis. I am trouble by this suggestion, as once I have taken a portion of the sample from the original sample bottle, I do not now have the same sample that I started with. I have reduced the O&G concentration of the sample. As I do not know how much O&G I have lost due to a plugged filter, the final value I report will not be correct, it will be low. I guess this means I could pretend to always plug my filter and continue

re -running the sample until a get a report value that I like. Seems a strange way to propose a method. While I am not in love with 1664, at least I am processing the entire sample, and the results I report are from the entire, original sample, and there is no guess work or additional manipulation required on my part. I suggest not moving forward with this method.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part18 136 for CWA compliance. Because EPA recogniz es that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA disagrees with the statement that once a portion of the sample is taken out that the O&G concentration of the sample has been reduced. It is true that the total O&G amount has been decreased from the total sample volume but not the concentration of O&G in the homogeneous sample. The withdrawal of a portion of the sample would affect an O&G measurement using

Meth od 1664 because this method measures the total weight from the original sample.

Comment 246 Anonymous : While I applaud the EPA for looking towards the future and considering new analytical methods, to improve on the sample preparation steps, I am very concerned about the proposed ASTM 7575 method. Let me explain. Per the ASTM method, the sample bottle should not be completely filled, as there needs to be room in the bottle to properly mix, or homogenize the sample, by shaking. As a side note, I can guarantee that a bottle would arrive in the lab that is completely filled, and that the end user would simply pour out some of the sample. Already I have a new problem. Plus, all sample collects would need to be retrained, which I think is even beyond God's ability to do. But back to

the issue. Per Note 3, about 5-10% of volume head space (represents about 50 to 100 mL of sample) is needed to perform the proper sample mixing. But what if a smaller sample volume is collected, and I can reach the syringe barrel down into the sample bottle. What do I do now? I guess I could add reagent water to bring the sample back up to a point where I could reach the sample with the syringe, but now I have to factor in the dilution of the sample. As a lab manger responsible for processing samples quickly and with minimal issues, I see the end user having to make many, real time decisions on how to properly treat, and deal with samples of varying volumes. I can immediately see the recovery and reported values starting to look like a shot gun pattern - very little consistency. I suggest the EPA hold off on any approval, until se veral more years of test data can be submitted, whereby the ASTM method has worked out all of these little potential problems that will quickly become issues in a real lab environment. Thanks for the chance to share my thoughts and concerns.

Response : S ee response to comment 244.

The total sample volume is not a critical aspect for ASTM D7575 as it is for Method 1664

because ASTM D7575 measures a concentration directly , not a weight that it is then converted to a concentration (which is the case for Method 1664). The addition of reagent water to the bottle is not necessary, nor the need to make decisions on how to treat samples of varying volumes. With respect to instruction to sample collectors, EPA asserts that training of sample collectors should be a standard practice regardless of the method(s) used

.
Comment 247 Anonymous : First, I must say that I am very surprised (shocked might be a better word) that the ASTM committee could allow a method like 7575 to be approved for routine use. I have never seen a more awkward and unscientifically sound procedure for sample prep testing and analysis. I suggest everyone read this method in detail, and I am sure you will come to the same conclusions, and understand why your local auditor will be all over you for reporting

random and inconsistent results.19 Here is one key point. Since the begin of time when samples were collected for Oil and Grease analysis, it was well known, tha t once a sample was collected, if an aliquot was taken from the original sample, that the "nature" of the original sample was changed, and if another aliquot was taken, that a different result would be reported. The entire sample needs to be processed, not a smaller aliquot. After years of processing the "whole" sample, someone on the ASTM committee thinks that is is now OK to remove small aliquots, and that the results be correct? If these were clean water samples and I were looking for pharmaceutical by -products, and using LC/MS/MS, a smaller sample is OK, as the MS can provide the sensitivity and resolution to identify compounds. The 7575 method talks about using a small aliquot from an extremely dirty sample, and pretends that I will get a "true" value when passing an IR beam through a mud caked filter.

Give me a break. Maybe what they should consider is using Raman with the proper embedded library. It would get much closer to the "true" answer. Lastly, in case you cannot tell, EPA, don't waste your time with this method.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA reco gnizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA disagrees with the commenter’s premise that in the ASTM method, an aliquot of a presumably homogenized sample is not representative of the original sample. If the proper procedure for sample homogeneity is followed, multiple aliquots from the original sample should be representative. The ASTM method has demonstrated sensitivity to make measurements at

conce ntrations similar to Method 1664 based on the MDL provided in Table 1 of the method. EPA may consider other techniques such as Raman if the Agency becomes aware of a specific method that uses this technology. With respect to the comment regarding extremel y dirty samples, this method may not be appropriate for such samples, and Method 1664 must be used for these cases (see N ote 2 in the method , which states that a different measurement technique may be necessary for samples where the solid matter is not sufficiently IR transmitting ).

Comment 249 Anonymous : As the EPA asked for my comments on the proposed ASTM 7575 method, here is one observation. I am making this comment based on information (literature and PowerPoint presentations) I found on line.

It looks like the method proposes collecting the O&G sample in a one liter bottle, but making sure not to totally fill the bottle so as to leave a "mixing" headspace, insert a syringe into the sample and remove 10 mL of a truly homogenous and representation sample from the bottle. For many of the typical O&G samples that need to be run in a commercial lab, there is no convenient, nor scientific way to take a 10 mL aliquot from one liter, and make the assumption that this is a truly homogenous and representative sample. It just is not so. Therefore, to see that the ASTM method thinks it is, clearly indicates that this method is seriously flawed and is not ready for prime time play. While I applaud the effort to always be on the look out for new technologies that will improve the sample prep procedures, this is not one of them. I see nothing but confusion in the lab industry with this particular method, and therefore propose this method be sent back for rethinking and better proof of concept.20 Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA disagrees with the commenter in his/her assertion that a sample cannot be made homogeneous and that a 10 mL aliquot is not representative of the o riginal samples. The comparability replicate data demonstrates that the results were very close in almost every case to the results obtained using EPA Method 1664. Detailed instructions on sample homogenization are given in section 14.2 of the method and in Note 9. For particularly challenging samples, if sample homogenization is not achieved, ASTM acknowledges a different method may be required (see Note 9)

.

Comment 252 Anonymous : In regards to whether the ASTM 7575 method should be approved, I want to offer the following concern over the validity of the method. For many years, Bill Telliard was adamant about nothing coming in contact with the Oil and Grease sample, such as a stir bar, mixing rod, or even pH paper, as anything that touched the sample would change the samples integrity. The labs have all accepted this approach and currently respect this technique. Now, it appears due to deficiencies in this proposed ASTM procedure, see Note 9, that it is OK to make contact with the sample to try and make it homogenous. Picture a typical Oil and Grease sample with a thick layer of oil floating on the top, and this method now would allow me to mix the sample with a stir rod, and then ignore the residual oil coating the rod. How can the rules change so quickly? It almost feels like there is an ulterior motive hidden behind the desire to have this method approved, versus being based on trying to make an easier method for oil and

grease testing. I say no approval.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

Note 9 in ASTM D7575 clarifies that for challenging samples, a paint shaker or ultrasonic vibration may be used and that contact mixing (i.e., ultrasonic homogenization, stand mixer etc.) has been not been found to cause interferences. EPA Method 1664A allows stirring (Section 11.3.5) if an emulsion forms between the organic and aqueous phases during extraction.

Comment 278 Anonymous : The proposed ASTM 7575 method specifies a sample volume of 10 mL, to be passed through the IR membrane. As the method does not seem to indicate the original starting sample container, I am guessing that any c ontainer could be used? Plastic, metal, etc?

This is a concern. But the bigger issue is trying to get a homogenous sample from the original sample container. The method references a "paint shaker" or even a contact mixer. I struggle with how this proposed method has drifted so far from the current 1664 procedure - that is, a one liter sample, that nothing should contact the sample before use, that all of the sample should be used, that an aliquot should not be taken, etc, etc.21 While I am sure everyone is always looking for better technology to improve current sample prep steps, the drive to approve these changes appear to be very self serving for a few individuals, or companies. If all revenue generated by this proposed technique were to be donated to the American Cancer Foundation, than I might consider suggesting approval of this method. Until that time, I say do not approve this method!!

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

In response to the sample container, EPA refers the commenter to Table II in 40 CFR part 136 which specifies appropriate containers (glass for oil and grease) . With respect to sample homogenization, Note 9 provides information on this step. With respect to sample volumes and taking an aliquot, see response to comment 246.

Comment 279 Anonymous : Regarding the proposed ASTM 7575 method, I question the recommendation to insert the tip of the sample syringe into the actual sample, and then pull the sample. I realize that this is the only physical way to remove an aliquot of sample, but as the outside of the syringe is now contaminated with the sample, I am sure this would be wiped off before attaching the IR membrane. The method also mentions that th ere might be times when another aliquot needs to be taken from the same bottle. Extensive work was done for the development of Method 1664, and now it seems that all of that knowledge and work is being ignored to serve the benefit of a few. If maintaining sample integrity is/was such an issue in the past, why does this proposed method feel that its approach is better and the rules should now be changed. Too many moving parts in this proposed method which scientifically have not been proven out. I recommend the EPA not move forward with approval of this method until these

issues are a ddressed and resolved.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. For the reasons specified in the notice, EPA has decided not to adopt this method

for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a

response.

With r egard to contamination of the outside of the syringe with sample, t he syringe with the withdrawn sample is attached to an extractor and the entire withdrawn sample goes through the

extractor . The outside is not wiped off. With respect to the comment on taking another aliquot, EPA refers the commenter to the response to comment 244. As indicated above, the concentration of the homogenized sample should not be affected.

Comment 287 Anonymous : I don't know if this should be posted here or not, but I have a question with the ASTM method mentioned. In the lab that I work in, we have a subcontractor who performs all the sampling for us. They charge us extra for any special conditions placed on the sampling. Since the ASTM method requires us specifically to leave 50 to 100 mL of space in22 a 1 liter bottle for homogenization purposes, this is a change from what we currently do and would require special conditions. If we don't put the special conditions on the sample, and we recieve it in for this test, it would re quire us to either empty out some of the sample or transfer the sample. Either way would result in lower recoveries and loss of analytes. This method does not seem up to the standards currently employed by most EPA methods and definately should

not be included in the 1664 method.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA rec ognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA cautions the commenter that emptying out some of the sample prior to homogenization could adversely affect the results. Arrangements between a lab and its subcontractors are outside the scope of EPA’s authority and this action.

Comment 288 Anonymous : In ASTM section 10.2 it makes mention of an equivalency equation that would adjust the final concentration of the sample based on the amount of acid added. The use of the equation does not seem mandatory and is contradictory to all our current practices with ANY other EPA method. I worry that some labs may use this equation and others may not resulting in inco nsistent data across laboratories. This would also require a retraining on the part of my analysts who produce the data. Any inclusion of this method will result in a high level of confusion amongst labs running this method and may result in mis-reported d ata.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

Both Method 1664 and ASTM D7575 require the adjustment of the pH to 2 using sulfuric or hydrochloric acid if the sample is not analyzed within four hours. For Method 1664, the total amount of oil and grease is not affected by the additional volume of acid since the measured value is a weight, not a concentration. For the analysis of samples using ASTM D7575, the amount of acid added could be a few drops or more. Thus, for a large sample volume a correction of the concentration may be unnecessary when a very small amount of acid is added; however, when a large amount of acid is added it causes a change in the measured concent ration. Only in such case s would it be necessary to use the equation in section 10.2.

Comment 301 Don Shelly, Food and Environmental Technical Service : Does the homogenization protocol work with all matrices including motor oil? If an oil laden sample is passed through the device, is there residue left in the devices pathways and syringes? Could there be carryover? Questions regarding homogenization: a. Will the ultrasonic bath accommodate a full batch of samples plus QC? b. Is it really expected that the analyst can determine homogeneity by looking at the sample through a tinted glass bottle? c. How is homogeneity defined? d. Are there instructions for performing dilutions?23 The ASTM method requires the assumption of homogeneity and 1664 does not, as dilutions are neither allowed nor required

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA complian ce. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

Regarding the question on whether or not homogenization will work with motor oil, motor oil is mixture of compounds of various compositions. Therefore some of these compounds may be extracted more or less than when using n

- hexane. ASTM did not submit data on this method with motor oil, so EPA can not respond more directly to this question. Regarding the question on residue on the device pathways and syringes, the syringe and membrane are single use devices, so there would be no carryover. Regarding the question on the ultrasonic bath capacity, laboratories are free to choose any ultrasonic bath that meets the requirements of the method, and thus, they should choose the appropriate size or number of baths as needed. Regarding the question on the use of a tinted bottle disallowing determination of homogeneity, there is no requirement for the use of a tinted glass bottle. The F ederal R egister, at 40 CFR Part 136, Table II, only requires an unspecified type of glass bottle. Regarding the question of how homogeneity is defined and the assumption of homogeneity, as implied in Note 9 of the method, a sample is considered homogenous if there is no stratification in the sample. Regarding the question on whether or not there are instructions on how to perform dilutions, there are no such instructions in the method.

Comment 318 ASTM D19 SUBCOMMITTEE O N D7575 : Some commenters have discussed that the sample container is not specified in the method. Response: Sampling and sampling containers are discussed in the Referenced Documents (Section 2.2) of the method. Specifically EPA Method 1664 is referenced in which sampling containers are

addressed in Section 6.1.1. Here is the link to that document: http://water.epa.gov/scitech/methods/cwa/oil/upload/20070710methodsmethod oil 1664.pdf As well, sampling is discussed in the ASTM D7575 Standard Operating Procedure that was placed in the docket found here: http://www.regulations.gov/#!documentDetail;D=EPA

- HQ

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- 0219 Some commenters have discussed concerns over homogenization using techniques other

than non

- invasive. Response: The method states (Section 14.2) that it is up to the operator to ensure homogenization and suggests non

- invasive techniques that have been found suitable.

In the case that the non

- invasive techniques are insufficient

– the method (only then) suggests homogenization that might utilize contact. It should be understood that this method may not be suitable for all matrices. Homogenization is further discussed in the ASTM D7575 Standard Operating Procedure that was placed in the docket found here : http://www.regulations.gov/#!documentDetail;D=EPA

- HQ

- OW

- 2010

- 0192

- 021924 Data results compared to EPA 1664 demonstrate the success of homogenization for challengi ng real world samples. http://www.regulations.gov/#!documentDetail;D=EPA HQ

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Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

We agree with the commenters statement on sampling containers and homogenization. The method developer did not provide data on non

- invasive techniques and their effect on the method results, so EPA can not speak to this specific issue.

Comment 319 Patsy Root, IDEXX Laboratories : There are too many outstanding issues with the

D7575

- 1 0 method at this time and, therefore IDEXX advocates resolving those issues first before promulgating the OSS D7575

- 1 0 method. Certain steps in this method require clarification: What type of sample container must

be used to collect samples?

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that pe rmittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA refers the commenter to Table II in 40 CFR part 136.

Comment 321 Stephen Arms, Florida DOH Environmental Laboratory Certification Program : At Lem's direction, I am sending you my short comment on the referenced proposed

rule. The proposed method ASTM 7575

- 10 allows for subsampling from the sample container and does not provide for rinsing the sample container with solvent to remove any material that might have adhered to the interior. EPA, in method 1664A, and more emphatically so in 1664B, speaks to this issue as

critical to accurate measurements of Oil and Grease. These methods require using the entire sample

followed by rinsing the container with solvent, which is included in the volume analyzed. Use of the proposed method could compromise analytical accuracy and comparability with past results.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA disagrees. In the case of Method 1664, rinsing of the container is done to ensure that the entire sample has been extracted. For ASTM D7575, only an aliquot is necessary due to the nature of the determinative technique . T he critical requirement for this method is to ensure that the sample is sufficiently homogenized so that the aliquot is representative of the entire sample.

Comment 326 Debra Weber, Louisiana Government : The NODA does not show or present any new data for the EPA to consider the ASTM as an equivalent Oil and Grease method to25 EPA Method 1664A. It is the laboratory communities understanding that Oil and Grease is a Part 136 method defined analyte, to approve this method would require the EPA to redefine the definition of “Method Defined” analytes.

There is no way to make sure a sample is homogenous also since calibration devices are

used there is no data to show what kind of calibration can be established when calibrations are used as prescribed in EPA Method 1664A.

Response : S ee response to comment 247

.

As EPA is not promulgating this method in Part 136 and limited use ATPs are an appropriate vehicle for consideration of alternatives to method defined parameters , the comment about the definition of method defined parameters is outside the scope of this action.

B. 4. Matrix spike requirements

Comment 250 Anonymous : I have been running oil and grease sample for many years (almost back before the days of Freon), so I was very glad to hear that a new method might be available, to take us to the next level. Unfortunately, I do not see that this proposed ASTM 7575 method is

the ticket. I have read through the method completely and i picked out one part that I struggle with. Please note, that this is not the biggest problem in the method, just one of them, but unfortunately, there are many. Section 12.8.4 suggests that if the MS/MSD does not pass, that "all samples in the batch must be reanalyzed by a test method not affected by the matrix interference". As a lab manger, it does not make any practical sense for me to run all of my samples, only to find that I need to reanalyze them by another technique

- I guess LLE or SPE? As mentioned, this is only one issue I have with the proposed method, so when you total them all up, I do not see value in this method, and strongly urge the EPA not to approved it. My

life is diffic ult already. You will only add to it and get my local auditor annoyed as well. thanks for the chance to share my thoughts.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for

nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

The lan guage in this section is analogous to the language in Method 1664 (i.e., in section 9.3.4.2 it indicates that if the analytical system is out of control , the problem should be identified and corrected and the sample batch reanalyzed). ASTM D7575 specifies that if repeated attempts

fail , one of the three options available is to use a different test method. As the commenter suggests, LLE or SPE are appropria te choices.

Comment 251 Anonymous : Subject: ASTM 7575 Method Issue: Wider Acceptable Matrix Spike Recovery Windows In Table 2 of the ASTM method, the Matrix Spike % Recovery Window is 70% to 126%. I propose that these values be the same as the cur rent 1664 method - 83% to 101%.26 I interpret this need for a wider recovery window as a deficiency of the method, and now question its viability.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

E PA agrees that the matrix spike p ercent recovery is wider than for Method 1664. However, the correct range for Method 1664 is 78 to 114% (see section 17.0, Table 1). EPA acknowledges that for one of the acceptance criteria (matrix spike percent recovery), the ASTM method does not perform as well as the approved method. However the difference is not large, and thus the Agency concluded that this method is acceptable provided that side- by

- side comparability data shows that the method results are comparable to that of the approved method.

Comment 291 Anonymous : For so many years I was told that dilutions of my samples was strictly not allowed and now I find that you are thinking of including a method which actually promotes the dilution of the samples (section 12.8.1, 12.8.2)! To move forward with this method, EPA needs to reevaluate what is and isn't acceptable within the current metho d. My thought is that the ASTM method shouldn't be allowed because it contradicts what I've been being told for

years now.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for

nationwide use. Permittees should co ntinue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

The refer enced sections address the concentration of matrix spikes, not actual samples. However, in Note 10 of the ASTM method, dilutions are allowed during the extraction portion of the procedure if the sample clogs the extractor. EPA suggests that if the extract or becomes clogged, then EPA Method 1664 be used. EPA Method 1664 calls for using a smaller volume so that the background measure and the spike do not exceed the method range of 1000 mg/L (see Note in Section 9.3.2.1).

Comment 292 Anonymous : ASTM D7575-10 Section 12.8.4: "all samples in the batch must be reanalyzed by a test method not affected by the matrix interference" This is what my auditor will latch onto and I will be left with no choice but to comply. Shouldn't any new methods being allowed be robust enough to handle the majority of the samples that are run using it? This gives me severe reservations about this method.

Response : See response to comment 250.

Comment 293 Anonymous : Table 2 of the ASTM method D7575-10 has MS requirements that are broader than the current recovery limits in the oil and grease method. This is definately not holding to EPA's purpose to ensure that the public safe and is, in fact, taking a step backwards. Any change to the method should improve ALL points of the method and not sacrifice one point

for others.27 Response : See response to comment 251.

Comment 318 ASTM D19 SUBCOMMITTEE ON D7575 : A commenter was concerned about the case where and MS MSD fails and having to qualify or rerun the batch of samples. Response : As a specific point of consistency with EPA 1664, ASTM D7575 suggests the same.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

The ASTM method, in section 12.8.4, contains recommendations to address what to do if the matrix spike samples fail. EPA Method 1664, in section 9.3.4.1, contains similar instructions.

B. 5. M e thod detection limit ( MDL )

C omment 255 Anonymous : Quick comment on ASTM 7575. Table 1 of the method calls out an MDL value of 1.0 mg/L. Yet, in Table 3, the 7 replicate runs generated an MDL value of 1.29 mg/L. Reading this, it indicates this method cannot even achieve its own specified MDL values.

Looks like more work needs to be done.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

The commenter is correct that the calculated MDL in Table 3 is 1.29 mg/L. The ASTM method rounds the MDL down to 1.0 mg/L. The calculated MDL rounded down would be 1.0, so, the information in Table 3 does correspond with the method specifications. Further, t he MDL for Method 1664 is given as 1.4 mg/L so, in fact, the ASTM method produced a slightly lower MDL

than Method 1664 . Also , the recommended lower reporting limit for the ASTM method of 5 mg/L is comparable to Method 1664 (this number was rounded up from a calculated value of 4.1 mg/L).

Comment 295 Anonymous : The data illustrated in ASTM D75 75-10 does not even pass its own criteria! Table 1 states that the MDL must be 1.0 mg/L or less and Table 3 lists an MDL value of 1.29 mg/L. If the pioneers of this method cannot even pass their own criteria, how could it be expected that others could. This also says much to me about ASTM methods that they are not fully vetted before they are promoted. I would definately not recommend the inclusion of this technique as an alternative to my current techniques.

Response : See response to comment 255.

Comment 302 Anonymous : We believe that the MDL of method ASTM D7575-10 (5 to 200 mg/L) is not sufficient and not convincing in the mid- and longterm. The vision for oil- in

- water discharge stated by e.g. Statoil is "zero discharge"28 ( http://www.statoil.com/en/technologyinnovation/protectingtheenvironment/wastedisposal/pages /zerodischarge.aspx ). Many polluters (e.g. US oil companies) using internal guidelines have begun to set discharge limits <1 mg/L. Challenging goals for discharge reduction should not be hindered by analytical methods which are not able to measure low concentrations. Methods with minimum range 0.5 -200 mg/L should be promoted by the EPA.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA promulgates new or revised methods that are as good as or better than existing promulgated

methods w ith respect to minimum levels. The lowest concentration (i.e. reporting limit) stated in the method for the application of the promulgated methods and ASTM D7575 is 5 mg/L. Therefore, the commenter’s concern that ASTM D7575 does not measure to lower values is not

relevant to its consideration. A larger sample volume may be required to achieve lower limits.

Comment 312 Anonymous : I wanted to make it known that when we were round tabling this method in our department meeting we noticed that in table 3 of ASTM D7575- 10 lists a MDL value that does not even pass its own criteria. ASTM D7575-10 states it requires a MDL of 1mg/L or less to pass. Table 3 shows runs and a result of 1.29 mg/L, which fails their own criteria. If the parties involved promoting this ASTM method cannot generate a working MDL then how is anyone else going to? I hope the EPA does not consider this method.

Response : See response to comment 255.

B. 6. Method applicabil ity

C omment 223 Curt McCormick : Does EPA believe this method is only appropriate for POTW effluents (post treatment wastewaters)? POTWs will have to specify the appropriate method for their permitted users and others (e.g, restaurants, automotive servicing, etc.) based upon historical concentrations of oil and

grease since EPA believes this method is valid up to 200 mg/L.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

ASTM submitted this method to EPA for consideration on all effluents (i.e. nationwide us). For the reasons explained in the notice, EPA is not approving this method for nationwide use in Part 136. A POTW can not specify ASTM D7575 in its permits or contro l mechanisms and a permittee cannot conduct compliance monitoring using ASTM D7575 for the permit or control mechanism unless the Regional ATP coordinator has approved a limited use ATP for the specific application being permitted.29 Comment 238 Anonymous : I currently need to analyze for non- polar material in my Oil and Grease samples. In reviewing the ASTM D7575 Method for Oil and Grease testing, as I do not see any provision for handling and reporting non-polar material, I see no value in proposing this method for approval, and suggest the EPA not consider approval.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

ASTM and EPA agree that D7575 is not applicable for measurement of non- polar material. As such, it is not appropriate to consider it for measurements of non- polar materials for nationwide applications or limited use applications. Method 1664 is available for the measurement of nonpolar material.

Comment 239 Anonymous : My permit specifically needs a technique for the non- polar aspect of the 1664A method (SGT- HEM).

Response : See response to comment 238.

Comment 241 Anonymous : I disagree with the EPA considering the proposal and consideration of the ASTM 7575 method for the following reason. In section 6.3 of the method, it states that samples which contain a relatively large amount of particulate or biological material, processing the standard 10 mL amount of sample may not be possible. Note 2 further states that there m ay be samples wherein the solid matter is not sufficiently IR transmitting. This means that I have no guarantee of knowing if my sample will pass or fail, until it fails to report the correct value. Why would I ever consider using a poorly thought out procedure like this? I am disappointed that the EPA is wasting their time with garbage methods like this. Do not waste everyone's time with approving this method. Focus on better methods that solve problems - not create new ones!!!!

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

As the commenter states, in sections 6.3 and Note 2 of the method, there is a cautionary statement that for certain samples this method may not be appropriate and another measurement technique may be necessary. EPA asserts that this kind of cautionary statement is generally appropriate in many test methods that have potential interferences so that a permittee and/or laboratory are able to use judgment in the se lection of the most suitable method for a specific sample. This type of cautionary statement is not unique to ASTM D7575.

Permittees should consider these cautions if they wish to explore ASTM D7575 for a limited use application.30 Comment 243 Anonymous : Per the EPA's request, I am writing this comment about the proposed ASTM 7575 method for Oil and Grease. After a quick review of the method, one thing that caught my eye was the comment in Note 2, that if the sample contains a large concentration

of metal particulates, that a different measure technique may be used. What would this other technique be, and how would I know it was equivalent? My samples currently do contain high metal contents, so why would I use this method. I see no value in this method for my work, and suggest that the EPA do not consider approval, as it will only confuse my auditor even further, and make my life that much more difficult. Please EPA, add simplicity to my life

- don't make it

more difficult

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

Permittees should carefully consider the limitations and cautions in the method if they wish to explore ASTM D7575 for limited use applications.

Comment 263 Anonymous : For what is is worth, I have spent many years using IR for techniques, unrelated to the proposed Oil and Grease ASTM method. But as I reviewed the method, I see a major problem. For IR in general, the measured IR absorbance generally matches a previously determined weight for petroleum hydrocarbons, because of the CH group, and this technique has been used for many years, in the petroleum industry. However, if the sample contain a ny synthetic silicone based products, or perfluorinated oils, the carboxyl group is not detected 2920 cm, which will result in a lower value being reported. While reporting a lower value is the goal on any oil and grease permit holder, I do not

think this was the intent of the EPA.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

The commenter’s concern is addressed in a cautionary (Note 1) in the ASTM method. Likewise, similar cautionary language is in Method 1664 for some materials such as crude oils and heavy fuel oils that may not be soluble in n- hexane. Permittees should care fully consider the limitations and cautions in the method if they wish to explore ASTM D7575 for limited use applications.

Comment 294 Anonymous : The inclusion of this ASTM method D7575-10 should not happen as almost none of my samples sound like they would be sufficiently homogenized to be able to be run this way. Its not that they have high levels of O&G content, which would put them above the 200 mg/L limit of the ASTM method, but its the organic content of the samples. Even if I could get a sample to appear sufficiently homogenized, there is no guarantee that when I skim off 10 mL of the 1 Liter that is collected that it will representative of the entire sample. It is obvious to me that this method has not been tested with real samples and, instead, has only been31 tested in very controlled settings and I would request that this not be allowed as an option for anyone to be able to run.

Response : See response to comment 243.

Comment 297 Larry LaFluer, NCASI : We have reviewed the materials provided in the docket and agree that for the specific matrices that were evaluated with respect to comparability of results using EPA 1664A vs. ASTM D7575

- 10 the methods provided reasonably comparable but not necessarily ide ntical results. However, in our view, the range of matrices tested is far too narrow to consider approval for use across all SIC codes. Although ten matrices were tested, there was similarity in some (four were food processing operations and three were cle ar uses of petroleum products). We do not believe this is a sufficient test of the broader range of industrial wastewaters where other organic substance might be present. Furthermore, ten matrices would be the minimum required for a nationwide approval of an alternative test procedure for a specific target

substance where procedures exist to estimate and quantify accuracy and precision and

detection limits. These traditional analytical metrics and evaluation procedures cannot be applied to a method

- defined parameter. Thus, a much higher burden of proof must be met before an alternative test procedure should be approved for a method

- defined parameter.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method

for nationwide use.

Co mment 319 Patsy Root, IDEXX Laboratories : Revise or expand sample processing for those samples suspected to have high metal content. Add an EPA recommendation to the method for NPDES permit writers in states that require a technique that could be applicable or comparable to the non-polar aspects of 1664A. Revise or expand method procedure if a large amount of particulate or biological material is suspected to be present in the sample; this will help labs avoid

re -running samples.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

Regarding the comment on revising or expanding the sample processing, as the ASTM method suggests (see Note 2), this method may not be appropriate for samples with high metal content. Regarding the comment on the suggested addition to the method for non- polar aspects, EPA is

unclear as to what the commenter means. This method is not applicable to non- polar material but for total oil and grease measurement. See response to comment 238 under topic B.6.

Regarding the comment on expanding the procedure if particulate or biological material is suspected, EPA thanks the commenter for this suggestion. In Note 2 of the method, it states that for samples where IR transmission is impeded, "a different measurement technique may be necessary."

Permittees should carefully consider the limitations and c autions in the method if they wish to explore ASTM D7575 for limited use applications.32 B. 7. Infrared (IR) measurement

C omment 242 Anonymous : Maybe I am missing something here, and someone can enlighten me. As I look at this proposed ASTM 7575 method, it looks like once the sample has been forced through the membrane filter, that the filter is placed into the IR system, and only the dead center of the filter is hit with the IR beam. What happens with reading the entire surface of the membrane? Having do ne filtration work for most of my life, it is well known that the entire surface of any filter should be analyzed, not just a small portion. Plus, as most of the sample is forced through the center, I would guess that the IR readings would be biased high, as this is where most of the sample will reside. Why would I want to report a higher value than I need to?

I would ask the EPA not to consider this method - at least not until more valid and scientific work has been done. This approach looks half baked.

R esponse : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

Regarding the comment about the IR beam analysis and extractor spot size, b ased on the data in the record, the replicate sample result s demonstrated that the results are reproducible using the technique.

Comment 266 Anonymous : My lab currently runs EPA method 1664B for oil and grease samples. As this method requires a 4 place balance, I am required to make sure this balance is properly calibrated and traceable back to the NIST Weights and Measurement Division. I do not

see any s imilar requirement for the IR device. Why? If the IR unit is going to be used, than this device should also be required to be certified

and traceable.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

It is true that Method 1664 (see Section 9.1.2.2.5) requires that the analytical balance and weights are traceable back to NIST. However, when instruments are used for a measurement, EPA generally includes a statement that the analysts must follow instrument manufacturer recommendations. This is a prudent approach since laboratories may have instruments from

different manufacturers.

Comment 283 Joe Stefkovich, Xenosep Technologies, Boonton, NJ : Indirect Vs. Direct

Measurement of Oil a nd Grease. D7575 does not measure Oil and Grease weight directly. Instead, it primarily measures the infrared absorbance of CH 2 groups at the specified wavelength

of 2920 cm -1 . Using properly prepared working calibration standards, the observed infrared intensity can then be correlated back to the weight of the analyte(s) used to prepare the working calibration standards. For IR in general, the observed infrared absorbance ty pically correlates well with the observed weight for petroleum hydrocarbons (e.g. hexadecane) since they are33 comprised of various CH groups. For fatty acids (e.g. stearic acid), the observed weight is typically greater than the observed absorbance due to the carboxyl group that contributes to the weight but is not detected at 2920 cm -1 . As such, erroneous data can be expected for high grease containing samples as well as synthetic silicone -based or perfluorinated oils.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of

this metho d for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA agrees that the method acknowledges that synthetic silicone -based or perfluorinated oils may produce inc onsistent results as stated in N ote 1 of the method. N- Hexa ne has similar problems with crude oils and heavy fuel oils.

Permittees should carefully consider the limitations and cautions in the method if they wish to explore ASTM D7575 for limited use applications.

Comment 318 ASTM D19 S ubcommittee on D7575 : The ASTM D19 Subcommittee on ASTM

D7575: Standard Test Method for Solvent

- Free Membrane Recoverable Oil and Grease by Infrared

Determination would like to address some of the relevant comments specific to ASTM D7575 in this Notice of Data Availability.

Com menters were concerned about the IR beam analysis and spot size of the extractor. Response: These comments and concerns are not supported by the data. The extractor and optimized membrane therein has unique patent pending qualities that have been developed to ensure homogeneous distribution across the field of analysis. The data and QC results from the significant amount of testing would have shown this to be an issue if that was not the case.

It did not. A commenter was concerned about the analysi s of synthetic oils that may have no C

- H

bands at 2920. Response: This is addressed in Note 1 and Note 7 of the Method.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response. Regarding the comment about the IR beam analysis and extractor spot size, see response to
comment 242. Regarding the comment on synthetic oils analyses, EPA is in agreement with the response.

Comment 326 Debra Weber, Louisiana Government : The use of IR is prohibited in EPA 1664A so therefore to consider a method where IR is used violates the only approved Oil and

Grease method in CFR Part 136.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.34 EPA is in agreement with the statement that Method 1664 disallows the use of IR for the method. However, this prohibition does not apply to the use of IR in other methods such as

ASTM D75 75. Nor does it prohibit a permittee for requesting an alternative method that uses IR using existing authorities under 136.5.

B. 8. Working range of method

Comment 223 Curt McCormick : Does EPA believe this method is only appropriate when the

actual concentration of oil and grease never exceeds 200 mg/L.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use

of this me thod for a limited use through existing authorities in 136.5, EPA is providing a

response.

As specified in the method, t he method range of ASTM is 5

- 200 mg/L and thus the method is limited to this range. As with any method, if the actual concentration of the parameter being

measured can exceed this range of the method and other methods exist with wider ranges

, the

alternative method should be chosen

. In this case, Method 1664 has a range of 5

- 1,000 mg/L.

Comment 240 Anonymous : I frequently have samples which are outside the working range of the ASTM method specified (>200 mg/L). This will not work for my laboratory.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA recognizes that the ASTM method range is 5 -200 mg/L. Method 1664 provides a wider range and it is available for samples with concentrations >200 mg/L.

Comment 271 Debra Waller, NJDEP : ASTM D7575

- 11 as an acceptable choice? Comment: Aside from the potential interference from water in the extraction/membrane analysis, the comparability data presented in the docket appeared to be acceptable as compared to recoveries from samples tested with the hexane based method. NJDEP would like to see

stro nger language related to the fact that the ASTM method can only go up to 200 mg/L

without dilutions. EPA Method 1664 extends that range up to 1000mg/L. When sample concentrations are greater than 200 mg/L, a hexane extraction will be more effective and stronger language should be in the 40CFR regarding this matter. Data should have also included sample sites where the concentration of the sample was determined to be closer to the top end of the working range than towards the lower end. For example a chicken rendering facility in NJ would

have oil and grease concentrations closer to 200 or higher and this method would most likely not be appropriate for that type of sample. Also some really strong language about how this method is not for use when reporting total petroleum hydrocarbons is imperative.35 Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA agrees with the commenter on both the concentration range limitation and the inapplicability to total petroleum hydrocarbons.

Comment 300 Anonymous : My current Oil and Grease samples typically have a reporting value of 450 to 700 mg/L, but it looks like the proposed ASTM 7575 method can only handle samples between a range of 5 to 200 mg/L. Therefore, I do not see how this method can help me. Plus, allow two so totally different methods (1664 with a range of 5 - 1000 mg/L and ASTM 7575

with a range of 5 - 200 mg/L) would create so much confusion for end users and the State Auditors, that I strongly recommend that this method not be approved. We have bigger and more pressing issues to deal with in the lab. The last thing we need is more confusion. Thank you.

Response : See response to comment 240.

Comment 310 Anonymous : My laboratory is concerned with this proposed ASTM method D7575-10. We couldn't find anywhere in this method that states its able to extract non-polar (SGT

- HEM) as part of the procedure. We currently use automated SPE and we are able to extract samples with a much wider concentration range and this method is only limited to 200mg/L at the most. I would only hope the EPA will not accept this method.

Response : See response to comment 239 regarding non- polar material. See response to comment

240 regarding the concentration range.

Comment 318 ASTM D19 SUBCOMMITTEE ON D7575 : Commenters have asked about the performance of ASTM D7575 in matrices that include metal particulates. Response: ASTM D7575 specifically looked into these types of matrices during development. Comparative evaluation to EPA Method 1664 was performed in: Aluminum Can Manufacturer, Machine Shop, Auto Garage, Auto Salvage, Gunsmith, and Bilge samples. Please re fer to slides in

the docket file here: http://www.regulations.gov/#!documentDetail;D=EPA

- HQ

- OW

- 2010

- 0192

- 0218

Commenters have asked: “Can ASTM D7575 can do TPH?” a. Response: No. ASTM D7575 is currently for total oil and grease measurement. Commenters have discussed how to handle samples outside of range (e.g. > 200 mg/L). Response: The method discusses the option of process volume reduction and dilution in

Section 14.3.3 Note 10 and the qualification thereof. Section 16 addresses reporting.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promu lgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.36 Regarding the method performance in matrices that in clude metal particulates, EPA is in agreement with this statement, the method measures oil & grease, not total petroleum hydrocarbons (TPH).

Regarding the comment on whether or not the method can assay for TPH, EPA thanks the commenter. In addition, pl ease see Note 2 in the method regarding how to address samples containing a large concentration of metal particulates.

Regarding the comment on how to handle samples outside the method range, see response to comment 240. See Table 1 for the reporting range limits of the method.

Comment 319 Patsy Root, IDEXX Laboratories : The method limit for D7575-10 is 5–200 mg/L. What if results are historically higher than this limit? Can dilutions of the original sample be made using D7575- 10? The additional data on D7575

- 10 says that dilutions are not recommended and another method should be used. If that is the case, labs would have to be certified for both methods, which increases burden on the lab.

Response : See response to comment 223.

Regarding the need for certification on both methods should a second method be required, under the Clean Water Act, certification is not required. However, some States or permitting

authorities m ay require certification for each method used in the laboratory.

B. 9. C alibration

C omment 237 Department of Defense : This letter provides the Department of Defense's comments on the Guidelines for Establishing Test Procedures for the Analysis of Pollutants. These were prepared by the Clean Water Act Services Steering Committee (CWA SSC) which represents the Departments of the Navy, Air Force, and Army as well as several DoD components and agencies. These comments were developed in consultation with the DoD Environmental Data Quality Workgroup. DoD supports EPA's consideration of new and revised test methods. However, DoD

wants to ensure use of the most current methods, consistency in preservation requirements, and alignment of calibration methods with EPA methodologies. Enclosed are our detailed comments

and recommendations. DoD appreciates the opportunity to provide comments. If you have any questions concerning these comments, please contact the CWA SSC chair, Ms. Lindsay Nehm at 703-695-

5179 or via email at lindsay.nehm@navy.mil

. [EPA Note: the following comments are from the attachment.] Specific comments: Calibration criteria of ASTM D7575 are inconsistent with requirements

of EPA methods. Proposed Requirement/ Section Addressed: ASTM D7575

- 11, Section 12.2.4 (ASTM

D7575

- 10, Section 12.2.4).

Comment: ASTM D7575 has a c alibration curve coefficient of determination criteria (r 2 > 0.95 for linear and > 0.97 for quadratic). The ASTM method also allows for calibration points37 within the calibration curve (i.e., not the lowest or highest points) to be reanalyzed or eliminated completely from the calibration curve calculations. Discussion: The elimination of calibration points within the calibration curve is not permitted for most methods and should not be allowed. The coefficient of determination criteria in

ASTM D7575-11 is wider than most methods allow. Recommendation: Recommend modifying the requirements for the calibration to be more in line with EPA methodologies.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for

nationwide u se. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA does not currently have a requirement for specific calibration curve coefficient of determination criteria for every method. However, generally, such criteria should be stated

and be > 0.95



### .

Comment 248 Anonymous : I am sending this comment on ASTM 7575, as my local auditor asked for my help. His comment pertained to section 12.2.4 and 12.2.5. In this section, it is stated that the coefficient of determination should be >0.95 for linearity and >0.97 for quadratics. For most of the existing EPA methods, the coefficient of determination is required to be >=0.99. His recommendation is to hold the ASTM method to the same 0.99 value, as currently approved, and

used EPA methods.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA does not currently have a universal requirement for the coefficient of determination

. However, EPA agrees that metal methods that employ linear regression specify a criterion for correlation coefficient (coefficient of determination) of 0.995 ( Solutions to Analytical Chemistry

Problems with Clean Water Act Methods

, EPA 821 -R-07-002 ).

Comment 283 Joe Stefkovich, Xenosep Technologies, Boonton, NJ : In strument Calibration

Standards Vs. Method Calibration Standards. D7575 utilizes a set of Calibration Standard Devices to ensure the instrument is within calibration. They are also used as the working calibration standards for development of the method calibration curve. However, their use in this fashion assumes the lab technician has perfected the technique for drying the infrared

- amenable membrane using the ill defined period of time specified in the method which will vary from sample to sample, instrument to instrument and operator to operator. No data was found in any study to demonstrate the competence of a lab technician to successfully generate an acceptable calibration curve using the method as written with fresh, laboratory- prepar ed standards of known weight. This competence must be demonstrated as part of a new Tier III study to assure satisfactory technique for analyzing both known and unknown samples.38 Calibration and Standardization Traceable to Independent Reference. The an alytical balance employed in EPA 1664A is calibrated at 2mg and 1000mg using class “S” weights which are traceable to commonly accepted criteria of the National Institute of Standards and Technology, Weights and Measures Division. There is no data to suggest that Method D7575 Calibration Standard devices are traceable to any independent, reference standard.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

Regarding the point abou t membrane dryness, see response to comment 2 53 (in Section B.10 membrane drying) below . Regarding the point about calibration curves, EPA does not require NTTAA methods developers to provide methods development data, which would include data for the gener ation of an acceptable calibration curve. EPA only requires methods validation data. The calibration is simple and easy to check with freshly prepared standards. Regarding the third point about a Tier III study, see response to comment 283 (in Section B.14 method validation) below. Regarding the point about reference traceability, b ecause this is a new technology, the calibration standard devices are not traceable to an independent reference standard. However, the method contains procedural steps (see section 12) to ensure that analytical values obtained using the method are valid and accurate within the confidence limits of the test.

Comment 289 Anonymous : In regards to ASTM method D7575-10: Sections 12.2.4 and 12.2.5 require that the coefficients of determination for l inearity and quadratics be greater than 0.95 and 0.97 respectively. For this method to be included in the EPA method all equipment should be held to the same high analytical requirements as each other, namely that the coefficient of determination be >= 0.99 as in most GC work. A lower coefficient

will result in lower confidence in the final result.

Response : See response to comment 248.

B. 10. Membrane drying

C omment 253 Anonymous : This is my first time for sending a comment to the EPA, so if there is an established protocol to follow, I apologize that I do not know it. However, it was suggested that I look at the proposed membrane IR method and, as I have years of experience using SPE for my oil and grease samples, that I respond if I see something that could create new problems. While I am encouraged, and support, the E PA in looking at new technologies, I see many issues with this proposed method. Here is one of the biggest issues I see. Per the current 1664 method when using SPE, one requirement is to remove as much residual water as possible from the SPE material, be fore introducing the hexane layer. If too much water is present, than the hexane will not efficiently extract the oil and grease off. While conventional wisdom would say to simply increase the amount of the air dry time, it is a well

known fact that too mu ch air will also volatilize the lighter end of the sample. This is easily39 demonstrated when running a DI water spike, as the hexadecane will be lost, if longer than 5 minute air dry times are used. This new method also states that any residual water should be removed prior to using the IR (see Section 14.4.1 and Note 11), as too much water will cause an interference with the spectra. In one example, the method showed an air dry time of 45 minutes. One, who wants to wait 45 minutes for this, and two, with 5 minutes, the hexadecane value will be adversely impacted. Based on the need to remove residual water from the membrane so the spectra can be read, it seems that there will be a significant loss of the light end with this procedure. Don't forget the original 418 method, which used IR had no evaporation step, nor was there an issue with residual water. That is one of the reason 418 was such a good method. The only down side was the use of Freon. I see more problems by approving this method, than problems that will be solved. Say no to 7575!

Response : Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

The ASTM procedure states that for most samples a short drying time may be sufficient and
suggests an iterative step of drying/measurement to verify that the sample is sufficiently dried. The dryness of the membrane is easy to check and does not require extensive training. This is analogous to the drying step in Method 1664 which requires drying, cooling, and weighing until the weight is less than 4% of the previous weight or less than 0.5 mg, whichever is less. In both cases, it is possible that some volatile materials may not be captured.

Comment 264 Anonymous : ASTM method 7575 clearly indicates that residual water left on the membrane will adversely impact the IR reading. The method then implies that if the residual has not been sufficiently removed, to dry the membrane longer. As samples, especially those filled with suspended material, will have different characteristics, the amount of drying time will need to vary for these types of samples. As soon as random drying times are used, random recovery values will be reported. The proposed method is implying that the end user should determine the amount of air dry time, which is counter to most other EPA methods. It has been well documented that when using SPE disk technology, that if too long of an air dry time is used, that the hexadecane standard will be volati lized off of the disk. Therefore, all dry times with SPE disk are made to be consistent, and any residual water is dealt with in another fashion, that does not involve an air dry step. This approach provides better accuracy and precision. My experience i ndicates that auditors are currently looking for a level of consistency in the environmental methods being used, so they are able to assess when a lab is generating correct and accurate data. I see the adoption of 7575 as a step backwards and will only cre ate more confusion in the environmental testing lab community. I feel 7575 should not be approved at this

time.

Response : See response to comment 253.40 Comment 265 Anonymous : Several comments have already been made about the use of air to dry the IR membrane, i.e. the adverse impact of losing the more volatile light end of the sample. However, another issue to consider is the potential of introducing compressor pump oil when using a compressed air source. The better way around this issue is to require the use of dry nitrogen instead. This would solve any problem with compressor pump oil being introduced onto the membrane, but the amount of nitrogen purging would still be an issue and needs to be addressed before this method becomes approved.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

In regard to the use of air to dry the membrane, see response to comment 253. Based on the data in the record, the use of a pressurized dried air apparatus has not been found to cause any problems as the commenter suggests.

Comment 268 Anonymous : Key concern. The presence of water is such a huge interference to IR, that Method 7575 has its own appendix which states that it can "potentially infl uence the placement of the baseline points...leading to inaccurate analysis. This variation will only lead to mass confusion in the environmental community.

Response : See response to comment 253 . Air drying of the sample eliminates the water

interference.

Comment 269 Anonymous : The ASTM 7575 method mentions that anywhere from 5 to 20 minutes may be required to dry the membrane of residual water. Plus, in one PowerPoint presentation from OSS, an air dry time of 45 minutes was used. Studies have shown when using SPE disks, that air dry times longer than 10 minutes will adversely impact recoveries. This is due to the volatilization of the light end of the extract. I cannot see that passing air through the IR membrane would not contribute to the same lose. But if the membrane cannot be dried for longer than 10 minutes, than the residual water still left in

the membrane will cause random and inconsistent recoveries.

Response : See response to comment 253 . In most cases the drying time is less than 10 minutes.

Comment 271 Debra Waller, NJDEP :

Comment: Since water remains to be an interferent in this procedure, why not include a step to dry the sample with a filter with sodium sulfate? If sodium sulfate fines are a concern, a .45 micron filter could be used. How many laboratories processing samples will take the time to really determine if the samples are completely dry on a routine basis and not just when an auditor is present or when PT samples are being analyzed?

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request41 use of this method for a limited use through existing authorities in 136.5, EPA is providing a

response.

With respect to the dryness of the sample, this is a very simple step when using an FTIR instrument. If the sample is not completely dried, the disk can be dried for a longer period of time

and then re

- measured. This is analogous to section 14.4.4 of Method 1664, where the procedure calls for desiccating and weighing the sample until the weight loss is less than 4% of the previous weight or less than 0.5 mg, whichever is less. For the ASTM method, if the membrane is not completely dry, you would not be able to see an absorbance peak and thus you would not be able to quantify oil and grease. You would then nee d to re

- dry the membrane and redo the

measurement.

Comment 283 Joe Stefkovich, Xenosep Technologies, Boonton, NJ : Water is an Interfering

Substance. The presence of water in the final sample analysis can lead to inaccurate results. D7575 utilizes clean, dry compressed air to dry the infrared- amenable membrane for an ill defined period of time which will vary from sample to sample (See ASTM 7575 Note 11) although Appendix X1 contains some non-mandatory information for determining membrane dryness spectros copically. EPA 1664A utilizes 10g of sodium sulfate or other equivalent means

to remove water from the final n

- hexane extract. If water does happen to remain in the final 1664A extract, it is very visible as a known interference. If water remains in the D7575 extractor, it is not so visible and its presence may not be known. It will be extremely easy to report an erroneous value with D7575 as the first result possible will be used since the iterative drying/measurement step is not a core part of the met hod, e.g., similar to achievement of a stable gravimetric measurement in EPA 1664A.

R esponse : See response to comment 2 53.

Comment 311 Anonymous : I wanted to comment on this method. It has been noted in section

14.4.1 and as well in note 11 that how critical the removal of water is from the extraction membrane. In this proposed method they state it may need multiple air dry times to ensure no interferences within the spectra. In my experie nces with 1664 the longer you air dry the sample the lower the recovery in the samples. The compounds are the same and hexadecane is smaller molecular weight compound so I really am concerned with their statement of multiple air dry times may be needed. I find it counter productive and less efficient compared to my current SPE procedures.

Response : See response to comment 253.

Comment 313 Anonymous : ASTM D7575-10 is going to be more trouble than its worth with the possibility of too much water in that membrane. It will severely influence the placement of

the baseline on the IR and would lead to inaccurate results and additional or excessive air

- dry times that could impact the overall results of the sample since there will be smaller molecular weight compo unds in the samples. I am very concerned with this method and how inconstant it can be with the supporting data within the ATSM method D7575-10.

Response : See response to comment 253.42 Comment 318 ASTM D19 SUBCOMMITTEE ON D7575 : Some commenters discuss the sample

- dependent drying time of the method and the potential recovery loss. Response: These comments and concerns are not supported by the data. Drying time is discussed in the Method (Section 14), Note 11 provides guidance on this process, and the Appendix provides specific details. The Standard Operating Procedure provided in the docket http://www.regulations.gov/#!documentDetail;D=EPA

- HQ

- OW

- 2010

- 0192

- 0219 also provides detailed information on this topic. As can be seen in the quality of results compared to

EPA Method 1664 http://www.regulations.gov/#!documentDetail;D=EPA

- HQ

- OW

- 2010

- 0192

- 0202 All technicians that have used this method have had no issues with the drying process. Any significant loss of recovery would have demonstrated a bias and/o r significant reproducibility

issues between EPA 1664 and ASTM D7575 results. This was not the case. It should be noted that there is an iterative drying step in EPA Method 1664. A commenter expressed concerns with the compressor for drying, saying that a compressor would contaminate the sample with oil. Response : The method states that a drying system must be capable of drying sufficiently for IR analysis without affecting analyte retention. The compressors used are oil free, and the drying system includes in

- line dessicant and filtration, the

results of which are reflected in the numerous blanks in the validation studies.

Response : EPA is in agreement with th is comment

.

Comment 319 Patsy Root, IDEXX Laboratories : Air drying times need to be standardized to avoid volatilization of the lighter end of the sample.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

This is similar to drying times for Method 1664 and, based on the data in the record, drying does not appear to be a problem.

B. 11. M ethod

- defined parameters and comparability

Comment 223 Curt McCormick : For Significant Industrial Users (SIUs) regulated under 40

CFR Part 403 that have to monitor oil and grease for a Categorical Standard, shouldn't comparison data be included with Method 1664 for these specific wastewaters? If this is an

alternate method under Part 136, this seems like a requirement. Without doing this could create havoc with permitting, compliance determinations and enforcement.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. A significant industrial user (and all dischargers to POTWs) must monitor for oil and grease using a promulgated Method in Part 136 unless the Regional ATP coordinator has approved a limited use ATP for the specific application being permitted.

Comment 261 Anonymous : General question and concern for the group. "Oil and Grease" is a method defined analyte, but the definition of O&G is different as defined by Method 1664 and the proposed ASTM method, as the procedure and equipment is different. There was a report43 issued by a consultant (Ed Askew) which demonstrated that when comparing certain matrix types, that the results were so different, that the two methods (1664 and 7575) were not equivalent. It is my understanding that the only definition suitable for compliance monitoring is

HEM and SGT

- HEM. It would seem that introducing a new definition (call it MEM) without a clearly thought out regulatory plan would simply create confusion within the environmental lab industry, and would create many new issues for the EPA. Look at confusion that was caused by simply trying to remove the use of a co-extracting solvent when using SPE. I suggest this proposed ASTM method be sent back, until it can be shown to be a direct equivalent to the current definition of O&G. The EPA has bigger and more pressing issues to deal with, than to get caught up trying to deal with the non-equivalent results of the ASTM method.

Response : EPA acknowledges that because the methods measure different things (weight versus IR absorbance), it is unlikely that they will produce the same results. As explained in the notice, EPA did not promulgate Method D7575 for nationwide use.

Comment 262 A nonymous : While in theory a method which does not use a solvent is a good idea, the bottom line is that the proposed method is not "equivalent" to the current 1664procedure. 1664 uses hexane (replacing Freon) which was a good choice, as hexane being nonp olar, will do an excellent job extracting oil and grease from a water sample. Therefore, by the approved 1664 method, anything soluble in hexane, is by definition, Oil and Grease. There is plenty of supporting data on the web, which clearly shows that trapping oil and grease on a membrane is not "equivalent" to extracting the oil and grease in a solvent. Making the assumption that they are equivalent would be believing that one could also take an SPE disk, after the sample has been filtered, and pass an IR beam through the disk to get a reading. The problem with this approach is the amount of residual water still present, and all of the particulate matter which would be present on the surface of the disk. If the 7575 method were to be changed to make more like the original 418 IR method, which sent the IR beam through the solvent, than 1664 and 7575 might(?) be more equivalent. As a side note, many years ago the EPA was thinking about Method 1665 which was to be an IR method, that would complement method to 1664. Based on the confusion i see reading the other comments, i suggest the EPA not approve this 7575 method. I also suggest that the EPA remain the driving force behind develo ping and proposing methods, and not allow the general public develop methods that are self serving.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for

nationwide use.

Comment 281 Anonymous : Pertaining to the proposed ASTM 7575 method, and that this method appears counter to every standard of excellence that the EPA tries to develop their methods to, I struggle to understand how and why the EPA would do such an about face, and even consider this method for approval. This is further reinforced when you look at the recent change from 1664A to 1664B,

wherein a co

- eluting solvent was no permitted to be collected. The EPA was holding firm that only hexane should be collected in the vial with the final extract, and this EPA requirement caused considerable confusion and frustration in the lab community.44 Now it seems that the EPA is adopting an anything goes attitude, and willing to consider any method that randomly comes along. What happened to scientific integrity and holding firm when you know something is right?

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for

nationwide use.

Comment 283 Joe Stefkovich, Xenosep Technologies, Boonton, NJ : "Oil and Grease” is a Method Defined Analyte. The “definition” of Oil and Grease by D7575 and 1664A are different as these definitions are dependent on the procedure and equipment used to make the determination. The Ed Askew report demonstrated results across certain matrix t ypes were so different that the two methods were not “equivalent”. Currently the only definition suitable for compliance monitoring is HEM and SGT-HEM and introduction of a new definition (MEM) without a clear and complete regulatory plan for it would create confusion within the analytical community and would be a major uncontrollable distraction for the EPA in years to come. No Solvent Extraction/IR Vs. n-hexane Extraction/Gravimetry. D7575 does not employ a solvent to extract the oil and grease analytes from the water sample or from the infrared

amenable membrane before determination by IR. 1664A uses n-hexane (85% minimum purity,

99.0% minimum saturated C 6 isomers, residue < 1mg/mL) to extract the oil and grease analytes from the water sample or in the case of a modified 1664A SPE method, from the SPE filter prior to gravimetric determination. The presence of a solvent is particularly important for grease containing samples as these are usually solid/semi -solids at room temperature and do not homogeniz e well

– especially in 1L bottles which are typically filled to the top in order to meet current EPA sample volume requirements.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a

response.

EPA acknowledges that ASM D7575 may not be the appropriate choice for certain matrices that do not homogenize well (see Note 2 in the method).

Comment 297 Larry LaFluer, NCASI : The National Council for Air and Stream Improvement, Inc. (NCASI) is an independent, non profit membership organization that provides technical support to the forest products industry on environmental issues. An important part of our mission is to ensure that regulatory decision making is based on sound science. Therefore, NCASI is pleased to provide the following comments on EPA’s consideration of the possible approval of an alternative test procedure for oil and grease that was posed by the United States Environmental Protection Agency (EPA) on December 14, 2011 ( Fed. Reg. Vol .76, No. 240,

77742

- 77747). 1. Whether EPA should reconsider promulgating this additional method for oil and grease based on diffe rent extractants and determinative techniques than EPA Method 1 664A. We believe that EPA has correctly identified “oil and grease” as a method

- defined parameter, the45 method being EPA Method 1 664A. We also agree that a method

- defined parameter is correct ly described as “the measurements obtained by the method are a specific artifact of the method and defined solely by the elements (solvent, determinative technique) used to measure the analyte.” Because the method EPA is considering adding to 40 CFR Part 136.3 (ASTM D7575

- 1 0) uses a proprietary membrane to isolate oil and grease, we cannot know how or if it will isolate the exact same materials that Method 1664A would isolate by n

- hexane extraction. Thus, we cannot be assured that for any given matrix the methods would measure the same parameter. For this reason, we recommend that EPA not add ASTM D7575

- 10 as an alternative test procedure for oil and grease.

2. EPA's current view, based on the data it has reviewed to date, that ASTM D7575

- 10 is an acceptable choice for the determination of oil and grease for the range (5 to 200 mg/L)

evaluated. We recommend that EPA consider the requirements and protocols for demonstrating

the acceptability of a method

- defined parameter and that it publish those procedures in the Federal Register fo r comments just as it did for the alternative test procedures for specific target analyte

methods.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for

nationwide use. EPA is considering identifying protocols for demonstrating the acceptability of method defined parameters.

Comment 303 Anonymous : We believe that EPA's current conclusion that permit limit adjustment based on side- by -side comparisons is not appropriate seems not to be a good position. The two methods will show strongly different values for oil and grease for certain types of oil, e.g. in the case of low boiling crude oils (condensates). Following EPAs current conclusion will

lead to the situation that differe nt values for one sample may be reported. There is the danger, that pollutors will choose the method with the lower oil and grease value for reporting. This cannot be of interest for the EPA. Therefore it seems more applicable to set the

reference method as "golden standard" and establish a conversion factor by having the discharger perform a side

- by

- side comparison for a limited concentration range, a distinct sample stream (non-changing oil composition) and a distinct matrix. This concept was followed in Europe by setting gas chromatography as the reference method (ISO 9377 -2 mod.) and providing a guideline on criteria for alternative method acceptance (published by the OSPAR commission,

Ref. No. 2006- 6).

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for

nationwide use.

Comment 304 Anonymous : If EPA were to allow a side

- by

- side comparison with limit adjustment as necessary, EPA should adapt the approach used for n-hexane in place of Freon. We believe that it is more appropriate to define a reference method and provide guidelines for determining a conversion factor to be used with alternative methods (e.g. as established by the OSPAR commission, Ref. No. 2006- 6). Permitted alternative methods should fulfill the following requirements: - No underestimation. - Best available technology. - Suitabili ty for all kinds of oils and matrixes. Alternative methods may have drawbacks (e.g. calibration) but should have advantages as speed and ease of use.46 Method ASTM D7575-10 does not show the potential for replacing the reference method due to the loss of light ends (during the tedious drying procedure of the membrane) and the limited matrix properties, being a result of the membrane filtration principle. Samples with a high content of particles or organic material will block the membrane for spectroscopy; a prior removal of the particles would also remove the oil sticking on these particles. Suitable references methods could be gas chromatography methods (e.g. ISO 9377- 2) or

EPA 1664A. Other methods such as ASTM D7575- 10 should be acceptable as alternative methods with a conversion factor subject to acceptance criteria issued by the EPA.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for

nationwide use.

Comment 307 William Telliard, Consultant : [EPA Note: The following is from the attachment to the comment. It contains comments from Joe Stefkovich (see comment 283) (JS) followed by response from William Telliard (WT response)]. [JS] Method D7575 and most other Oil and Grease methods being cons idered for inclusion in Table IB are all not suitable for compliance monitoring of the method

- defined analyte Oil and Grease and as such are not required to be promulgated per the National Technology

Transfer and Advancement Act. If Method D7575 was included in Table IB and the other equally not suitable methods were not, almost certain legal consequence would result from the other method developers due to the appearance of impropriety and inconsistent treatment of their methods by the EPA. [WT response] Method D7575 has been proposed as an alternative to Method 1664A.

The current Administration and EPA Administrator have asked for environmentally friendly methods to augment existing toxic methods. JS's expressed concern about legal consequences

seems inan e; he is not an attorney, nor does he have experience in the enforcement field.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method

for nationwide use.

Comment 319 Patsy Root, IDEXX Laboratories : As stated in the NODA, oil and grease is a

method

- defined parameter. How will historical data using EPA 1664A be compared to data derived using D7575

- 10? The NODA does not clearly cover the statistical difference labs and data users will see when comparin g methods. For example, how do the two methods compare statistically in variety and quantity of components detected, percent difference between the two

methods.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method

for nationwide use. The notice also reminds permittees of existing authorities to request alternative methods for a specific use (Part 136.5). The notice additionally provide s guidance on how to demonstrate comparability for such requests.

B. 12. A nalysis cost

C omment 258 Anonymous : The driver for identifying an alternative oil and grease method is the need to move away from hexane as an extraction solvent. A solvent-less method sounds47 ideal, however the ASTM D7575-10 method proposed has distinct disadvantages over the existing EPA1664. ASTM D7575-10 requires the use of an expensive technically advanced FTIR analyser, large scale labware, on -site sampling system and filter consumables (I do not have sufficient information on the filter manufacturing process, re-use or disposability to comment but these issues should be considered). ASTM D7575- 10 also seems a step backwards from the current system in that it would be a difficult method for end users to implement on site (such as off shore platforms), thus prohibiting the fast analysis response times required to keep systems running as efficiently and environmentally sound as possible.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

As with any technology, environmental laboratories wishing to use this method may have an initial investment cost (FTIR analyzers have been available for other applications). With respect

to the method being difficult to implement on site, the current method is also a laboratory method, not a field method. The FTIR technology can be adapted for field use.

Comment 301 Don Shelly, Food and Environmental Technical Service : What is the cost of analyzing samples using ASTM D7575-10 vs. 1664?

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a

response.

After the initial investment in equipment (FTIR), we estimate that the cost will be comparable or slightly lower.

B. 13. Handling waste

C omment 259 Anonymous : This is mo re of a general comparison question between the proposed ASTM 7575 method, and the current SPE 1664 method i use. If I use the 7575 method, what am I expected to do with the left over sample? That is, I receive almost a liter of sample, but take only 10 mL out. Do I pour this down the drain? Do I

consider it hazardous waste? I am not sure. With 1664, I use the entire liquid sample, and as the sample has been filtered and is now much cleaner than when I started, this water is poured down the drain. I am left only with a dirty filter, which I dispose of properly, which I guess I would also do with the IR membrane. My concern and question is, am I generating more waste, which in turn will cost me money?

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part48 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

Although the ASTM method does not specifically address waste management, section 2.2 of the method does refer to EPA Method 1664. Please see the Waste Management section of EPA Method 1664 (15.0), which addresses how to dispose of waste from the method. In addition, ASTM has a method D4447, “Standard Guide for Disposal of Laboratory Chemical and Samples, ” that addresses this issue more fully.

Comment 319 Patsy Root, IDEXX Laboratories : Add guidance on disposal and hazardous waste designation of any remaining, unused sample

Response : See response to comment 259 and Section 1.5 of the method, where this issue is

addressed.

B. 14. Method v a lidation

C omment 223 Curt McCormick : The data found on the Internet indicate only one Publicly

Owned Treatment Works (POTW) wastewater (influent or effluent?) with a true oil and grease value of 10 mg/L was tested. Based upon this, EPA appears to be saying the Agency believes the method is equivalent to Method 1664. This assumption would appear to be unsupported based upon information found on the Internet from the company that developed the method: Oil and grease samples of POTW influent and effluent should be tested. These samples should

inc lude multiple oil and grease true concentrations in the 5 mg/L to 200 mg/L range. These sample should be sent to multiple independent wastewater laboratories. EPA seems to be indicating that based upon the data it reviewed (not provided in this Notice), th is method is approved for use under the Clean Water Act. EPA needs to do a more thorough public notice of the data it reviewed (provide the data) to make a decision that this method is equivalent to

Method 1664 for raw and final wastewaters approved under 40 CFR Part 136. Does EPA believe that this approach to method validation and the apparent lack of data on significant matrices (POTW influent wastewater, oil and grease from grease interceptors, etc) is appropriate to support approval of an alternate, enforceable method under the Clean Water Act?

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance.

Regarding the point on the validation studies conducted, the commenter seems to be confusing the validation study with the method comparability study. The method comparability study included

seven POTWs. The second phase of the ASTM study was the multi

- laboratory study in which one of the matrices used was a POTW. The purpose of these two studies is different. The multi

- laboratory study is done to define expected performance for the method (e.g., recovery , precision)

. Both the comparability data and the validation data were provided in the NODA docket for review and

comment

.49 Comment 267 Anonymous : From information that appears on various web sites, it appears that the evaluation of method 7575 was validated by the developers direct personnel, setting up the same equipment at various labs, and most likely running the samples. This means that the 7575 method does not meet the standard requirements for ASTM or the EPA Multi-Lab, Multi- Matrix study requiremen ts.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

The developers have stated that they provided equipment to the laboratories, trained the personnel prior to the validation study tests, and that the tests were conducted solely by laboratory personnel after the training session. Because this is a new technology, this is not an unreasonable process when introducing it to a laboratory.

Comment 280 Anonymous : It was mentioned in an earlier comment, and I agree, that the EPA should be very careful about approving the ASTM 7575 method, as there would most likely be lawsuits filed by those vested parties who have worked so hard to assist with the development of 1664. If the 7575 method were truly revolutionary and followed the guidelines established for other EPA methods, lawsuits would be less of an issue. But on close examination of 7575, there are too many inconsistencies, the data is suspect, smaller aliquots are taken from a larger container, contact mixing is suggested, a detection technique which has problems with water and particulate material, air dry times which are random, and it appears that a technical representative from OSS was present at each site which evaluated this approach, smacks of impropriety by those people who are promoting this method. The EPA could have a large and expensive lawsuit on its hand, if the EPA continues to

consider this 7575 method.

Response : See response to comment 283.

Regarding the general list of issues specific to D7575, please see the following sections wherein

similar comments have been addressed. Regarding the comment on “too many inconsistencies” more detail is needed. Regarding problems with water and particulate material, and air dry times, see responses in Section B.3, sampling requirements and preparation. Regarding the comment on the presence of an OSS technical representative, see Section B.14 method

validation.

Comment 283 Joe Stefkovich, Xenosep Technologies, Boonton, NJ : Thank you for the opportunity to review ASTM Method D7575 and related information for purposes of comparing it to EPA Method 1664A and rendering an independent opinion regarding possible inclusion of D7575 in the upcoming MUR, Ta ble IB. At this time we would strongly advise EPA to not include ASTM Method D7575 in the upcoming MUR, Table IB. Based on our review of the method, the Ed Askew report/rebuttal, comments from the various EPA Regions and other information:50 There appear to be serious technical issues or concerns with the method and submitted validation study so a successful EPA Tier III Multi-Lab, Multi- Matrix Validation study to address these issues should be performed prior to inclusion in Table IB as we believe it would be better for the EPA to push forward a known good method rather than pull back on a known bad

one in the future.

While a solvent- free Oil and Grease method is certainly appealing, it is highly unlikely that EPA or anyone else can say with certainty at this time that Method D7575 is acceptable for use and what could or should be done with a potentially new regulatory definition for Oil and

Grease. As Oil and Grease is the 2 nd most enforced against parameter (pH is 1 st ), we would strongly advise EPA to not include Method D7575 in the upcoming MUR, Table IB until the method is proven reliable with a new EPA Tier III study and EPA has a clear directive to replace the current Oil and Grease regulatory definition of HEM and SGT- HEM with MEM. As I’m

sure you can appreciate, once EPA enables additional confusion on D7575, it will be like opening Pandora’s Box with the net result being much self-inflicted pain, distraction and embarrassment on the part of the EPA. Incomplete ASTM and EPA Multi-Lab, Multi- Matri x Study Requirements. EPA 1664A was validated by independent work of at least 9 laboratories analyzing at least 9 different matrix types with at least 3 sets of Youden pairs per matrix. D7575 was validated by the dependent work of method developer personn el setting up the same equipment at 12 local laboratories and who were probably present when the study tests were performed. In addition only 3 matrix types were tested with only 1 set of Youden pairs per matrix. The D7575 validation study did not meet the standard requirements for ASTM or EPA Multi-Lab, Multi-Matrix study requirements and could really be considered an EPA Tier I study performed by 12 analysts.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

Under the National Technology Transfer and Advancement Act (NTTAA), EPA is required to consider methods validated by consensus standard organization, e.g., ASTM, which have validation requirements that are different from EPA's ATP requirements. EPA asked for and

received the underlying data from the validation studies conducted by ASTM and provided it for public review and comment. Consensus standard organizations are not required to follow thesame procedures as EPA and may choose not to conduct an EPA Tier III Multi-Lab, MultiMatrix Validation study. EPA does not favor one approach over the other with respect to validation. That is, a vendor or method developer is free to go through EPA’s process or may choose to go through a voluntary consensus organization process. The key is that they must choose only one approach. Neither process guarant ees that EPA will approve the proposed

method. With r egard to the point on incomplete multi- lab, multi

- matrix study requirements, ASTM has confirmed that ASTM guidelines for method validation were followed. The assertion that the developer personnel were present during the study tests has been denied by the method developer. The method developer acknowledged that equipment and training was provided to the participating laboratories prior to when the study data was collected. However, this is not unusual when new technology is introduced that is not standard for environmental analyses.51 Comment 301 Don Shelly, Food and Environmental Technical Service. Comments regarding Proposed Rule for ASTM D7575- 10 (Oil & Grease) EPA

- HQ -2010-0192. It is my opinion that many concerns remain unaddressed. Were the standards used in comparison studies between methods 1664 and ASTM D7575-10 certified and independent?

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

The standards were prepared as described in the methods. Neither method states that the standards must be certified and independent, but rather they give specifications on purity and preparation. In addition, standards are not required to be certified or independent in va lidation studies. Only for certification/accreditation purposes may independent standards be required.

Comment 307 William Telliard, Consultant : As a member of the D19 Committee of ASTM, I strongly support and recommend its new ASTM Method D7575. As the author of record for EPA Method 1664 and 1 664A, I feel it is my responsibility to submit some clarifying comments on a document submitted to the docket by Mr. Joseph Stefkovich (JS) to Lemuel Walker, EPA Office of Water: Office of Science and Techn ology. For your convenience, JS's letter and review (with my clarifying notes) are included at the end of this comment. My comments and opinion are the result of over thirty

- four years of experience at the Agency. While at EPA, I served in the Office of Wa ter, the Permits Division, Office of Water Enforcement, and the Office of Science and Technology. Approximately a hundred analytical methods were developed and promulgated under my direction. Numerous industrial guidelines and regulations for the energy an d mining industries were also developed under my aegis. The author, JS, asserts that he is providing an independent opinion on D7575. A difficult notion to support since he is employed by a direct, industrial competitor of this new green technology. JS and others were also supplied information on comments from the EPA Regions (as noted in his attached letter) and from other Agency "inside information." This information was not made available to ASTM D19 or the developer of the method (OSS, Inc.), nor included in any correspondence with ASTM. To my recollection, inter -Agency correspondence and work products are to be kept confidential or within the Agency's purview. I question why this data

was circulated to outside entities. Based on the this, can his review be considered "independent"? Also, I question his experience to express an opinion on permit, legal, and

enforcement issues. [EPA Note: The following is from the attachment to the comment . It contains comments from

Joe Stefkovich (see comment 283) [ JS ] followed by the response from William Telliard [ WT response]] [JS]: Thank you for the opportunity to review ASTM Method D7575 and related information for purposes of comparing it to EPA Method 1 664A and rendering an independent opinion regarding possible inclusion of D7575 in the upcoming MUR, Table IB. At this time we would strongly advise EPA to not include ASTM Method D7575 in the upcoming MUR, Table IB. Based on our review of the method, the Ed Askew report/rebuttal,

comments from the various EPA Regions and other information:52 There appear to be serious technical issues or concerns with the method and submitted validation study so a successful EPA Tier III Multi

- Lab, Multi

- Matrix Validation study

to address these issues should be performed prior to inclusion in Table IB as we believe it would be better for the EPA to push forward a known good method rather than pull back on a known

bad one in the future. [WT response]: ASTM has already exceeded the requirements of a Tier III M ulti

- Lab study. See the information below which is a NODA

- updated version of the same chart provided in a previously submitted EPA docket document found here: http://www.regulations.gov/#!documentDetail;D=EPA

- HQ

- OW

- 2010

- 0192

- 0218 see slide

12.

[JS] Attached with this report is a product data sheet the D7575 method developer has been distributing for the past 12 months which strongly implies the D7575 method/product is suitable for NPDES regulatory compliance testing and is a replacement for EPA 1664. While this implication is not true, inclusion in Table IB would make it “more be lievable” and as such, EPA would directly enable increased confusion regarding D7575 and as a result will have to deal with an unnecessary major distraction out of their control for years to come.

While a solvent- free Oil and Grease method is certainly ap pealing, it is highly unlikely that EPA or anyone else can say with certainty at this time that Method D7575 is acceptable for use and what could or should be done with a potentially new regulatory definition for Oil and

Grease. As Oil and Grease is the 2n d most enforced against parameter (pH is 1st), we would strongly advise EPA to not include Method D7575 in the upcoming MUR, Table IB until the method is proven reliable with a new EPA Tier III study and EPA has a clear directive to replace

the current Oil and Grease regulatory definition of HEM and SGT

- HEM with MEM. As I’m sure you can appreciate, once EPA enables additional confusion on D7575, it will be like opening Pandora’s Box with the net result being much self

- inflicted pain, distraction and

embarra ssment on the part of the EPA. [WT response] Note: A data sheet for D7575 was not attached to this report. D7575 has not been proposed as a REPLACEMENT FOR D1664A, BUT AS AN ALTERNATIVE. Thus, competitors could continue to market their out dated products. The method makes absolutely no change in the definition of oil and grease, as JS infers. The author apparently53 believes that the laboratory industry and the regulatory community are incompetent when dealing with a table in a Federal Registe r notice. (They do read and write.) I believe his final, closing sentence of this letter expresses his opinion of the US technical community.

Response 

### : EPA agrees with this commenter that EPA’s consideration of D7575 was as an

alternative to Method 1664A and not a replacement.

Comment 314 Scott C Hoatson, Oregon Department of Environmental Quality : I think I would like to see more side by side data in more matrices before this method is added to the MUR. Most samples were quite comparable but there were some that were different by a fair

amount. If there is a potential for a bias in certain matrices, we would have a concern regarding a carte blanche acceptance of the method. Additionally, though I have not sc r utinized all of the supporting validation information, I reviewed some of the raw data in the attached file that was part of the supporting doc umentation

and have some concerns. If this is an example of the supporting documentation, I cannot support adding the method to the MUR at this time. There are several of the MDL studies where a point was dropped for no apparent reason (It was not a statistical outlier); MDLs would be higher if the values were included. T here are a lot of hand corrections in the raw data without explanation and the corrected values are the ones

used in the spreadsheet (see notebook pages

– though it is not that unusual but it is obviously frowned upon practice). There are sample analyses that were rerun again after additional drying (sample numbers do not correlate with sample numbers on spreadsheet but raw values do). I suspect that these issues are likely innocent, but I don’t think it should be used to support any decision unless it is corrected.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method p romulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response that may be relevant to such considerations.

EPA agrees with the commenter with respect to the potential bias in certain matrices.

Comment 318 ASTM D19 SUBCOMMITTEE ON D7575 : A commenter suggested that ASTM D7575 did not meet EPA Tier III guidance for nationwide approval. Response : P rior to the NODA study, ASTM D7575 had already exceeded the guidance of an EPA Tier III MultiLab study for nationwide approval of a method. The informational chart below presents and even stronger case. It is a NODA

- updated version of the same chart provided in a previously

submitted EPA docket document found here: http://www.regulations.gov/#!documentDetail;D=EPA

- HQ

- OW

- 2010

- 0192

- 0218 see slide 12. EPA personnel were involved in all study plans.54 Some commenters have asked about equivalence of ASTM D7575 and EPA

Method 1664. Response: Statistical equivalence has been documented, see: http://www.regulations.gov/#!documentDetail;D=EPA

- HQ

- OW

- 2010

- 0192

- 0163 and http://www.regulations.gov/#!documentDetail;D=EPA

- HQ

- OW

- 2010

- 0192

- 0202 Commenters have suggested that the development of ASTM D7575 did not include independent autonomous testing. Response: Not true. See the scans of the laboratory

notebooks from the 12 different operators from 12 different certified laboratories that participated in the ASTM D7575 multilab study and autonomously performed the testing

here: http://www.regulations.gov/#!documentDetail;D=EPA

- HQ

- OW

- 2010

- 0192

- 0201

Response : See response to comment 283.

C omment 319 Patsy Root, IDEXX Laboratories : Data Collection Process: It is disconcerting that the generation and review of data was performed by OSS personnel. Documents in this docket indicate that the same OSS personnel and consultant (retired EPA official) set up the same equipment at each site and were at least present at each site, and pre

screening samples. This does not give the appearance of being the type of ‘hands

- off’ testing typically required by EPA. For example, in a typical ATP, the laboratory personnel themselves actually perform the testing, although training prior to testing is acceptable. Would EPA please comment on why, in this case, OSS personnel were allowed to participate in the testing process?

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.55 EPA disagrees. See response to comment 267. The comparability and validation data were collected by independent laboratories and not by OSS. ASTM and EPA staff independently

reviewed the data.

Comment 322 Joe Stefkovich : As a follow up to my February 10 note, I was disappointed to learn that there is no raw data in either the MUR or NODA dockets for any of the D7575 multi

lab validation reports. I was and have been under the impression that for a new method to be

considere d for compliance monitoring, all aspects of it must first be vetted via public disclosure. In the proposed MUR docket, I could not find any raw data to tie back to the summary

data and see if the method really does “work as advertised.” This observation however is not that surprising as the original EPA position was to not propose the method for the MUR so it was probably thought by the EPA that this data probably wasn’t necessary since the method wasn’t being proposed in the MUR. However, now that the method is being considered, the public review of raw data is now more important than ever. Unfortunately it seems that the cart is before the horse when it comes to D7575 as the public is being asked to comment on how the method could be employed without establishing the method works “as advertised” and is worth employing in the first place. At a minimum I would suggest the EPA might want to consider issuing a new NODA containing all the D7575 raw data and other pertinent information before taking

action on D75 75 as due to the apparent “special treatment” this method has received, there is a growing negative perception within the industry regarding EPA and this

D7575 method. Thanks.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA provided all the data ASTM submitted on method performance in the NODA docket, whether from the comparability study or from the validation studies for vetting and public disclosure. Contrary to this commenter’s assertion, EPA included raw data for the studies conducted for this ASTM method. In fact, EPA has gone beyond what is normally requ ested for methods from voluntary consensus standard bodies (VCSBs) when submitting adopted

methods for consideration . Methods and the underlying data from VCSBs are p eer

- reviewed and adopted by these organizations based on their peer

- review policies. EPA reviews these

methods to ensure that such methods meet EPA’s needs and places the submitted information in the docket for public review and comment prior to making a f inal determination . We typically do not request or review the ra w data from such organizations. Such a blanket
request would be a change in practice and may be considered in the future but is not a requirement . In this and prior regulatory actions, all met hods are indeed vetted through the public notice and comment.56 Therefore, contrary to this commenter’s assertion, the data available on D7575 is more extensive than typical and has been properly provided to the public for consideration

. Also

see response to comment 283.

B .15 Unfunde d mandate

C omment 277 Anonymous : Heads up to EPA. In the early days of developing Method 1664, one of the problems the EPA ran into was that the EPA had not conducted an Unfunded Mandate Study to understand the potential financial impact to the EPA, if certain sectors of the oil and grease permit holders were to put out of compliance by using this method. If these people were to file a lawsuit against the EPA, where would the money come from. As no study had been done, the method development group decided to fore go the study and released the method a LLE procedure, with the ability to use SPE as an alternative extraction technique. I do not see any indication that such a financial impact study has been done for 7575. Therefore, the EPA could find itself with a lawsuit from the current method developers w ho are being unfairly treated, as the 7575 developers are being given preferential treatment.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance.

The commenter misunderstands the unfunded mandate Reform Act . Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), 2 U.S.C. 1531-1538, requires federal agencies, unless otherwise prohibited by law, to assess the effects of their regulatory actions on State, local, and tribal governments and the private sector. In particular, UMRA focuses on rules that contain a federal mandate that may result in expenditures of $100 million or more for State, local, and tribal governments, in the aggregate, or the private sector in any one year. If EPA had adopted

ASTM D -7575, it would not have required the use of this method . Rather , rather it would have

added this method to the list of approved methods for oil and grease. Thus, the unfunded mandate requirements do not apply.

B .16 Method version (ASTM versions and EPA Method 1664 versions )

C omment 237 Department of Defense : Current Version of ASTM D7575 is not correct. Proposed Requirement/ Section Addressed: 76 FR 240, A.1, Proposes to allow ASTM

D7575- 10.

Comment: ASTM D7575 -10 is not the current active version of this method. The method

was revised and reissued on 1 November 2011 as ASTM D7575-11. Discussion: When ASTM updates a method, the older versions are no longer active. Recommendation: Recommend allowing the use of ASTM D7575-11 instead of ASTM

D7575-10.

Response : For the reasons specified in the notice, EPA has decided not to adopt this m ethod for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to57 request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

The two versions are nearly identical. D7575- 11 contains some editorial clarifications that EPA requested.

Comment 271 Debra Waller, NJDEP : Should EPS reconsider promulgating this additional

method for oil and grease based on different extractants and determinative techniques than EPA

1664A? C omment: The US EPA is withdrawing Method 1664A from 40CFR Part 136.3 and replacing Revision A with Revision B. Everything I read about the method refers to its comparability to Revision A and not Revision B. If the EPA is removing Revision A from the 40CFR why are there references to Revision A in the docket?

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a

response.

EPA added version B of Method 1664 in the recent Methods Update Rule. EPA did not remove

Method 1664 version A. The documents in the docket refer to documents that ASTM followed in their approach when they compared their method to EPA Method 1664 version A.

Comment 274 Anonymous : ASTM method D7575-10 is not the current method sold by ASTM. D7575-10 is listed as an historical method and D7575-11 is the current method. (1) what is the difference between the two technically that required an ASTM re -balloting and (2) can EPA promulgate an historical method?

Response : See response to comment 237. Note that both versions are in the record and were available for public review and comment.

Comment 299 Ed Askew : 1. The comments on the Notice of Data Availability (NODA) will not focus on original method submitted to the EPA for the current Method Update Rule (MUR)

which was ASTM D7575

- 10, but instead will focus on how the NODA concerns:

a. A final ASTM meth od that is not the same as the original ASTM method

submitted for inclusion into the MUR.

b. That the method listed in the NODA is not the final method to be considered by EPA.

c. That EPA staff was aware that the current ASTM D7575

- 11 has significant changes from the original ASTM method in the NODA. 2. From the NODA, Federal Register /Vol. 76, No. 240 /Wednesday, December 14, 2011: a. Based on the new information and EPA's analysis of this information as described in this Notice, EPA is reconsidering whether to promulgate ASTM D75 75

- 10 in 40 CFR Part 136 as an alternative method for oil and grease. 3. The docket contains information on a meeting (August 3, 2011) with EPA, Orono Spectral Solutions (OSS) staff and other interested 3 rd parties that indicate that EPA staff required major method procedural changes before the ASTM method D7575

- 10 would pass muster as an acceptable regulatory analytical method.58 a. Summary: Attendees discussed the analysis of additional matrices to compare

Methods 1 664B and ASTM 075 75. ASTM agreed to prepare a study plan for EPA review prior to testing additional matrices. In addition, EPA discussed the need for some changes to the ASTM method, as follows: 4. By ASTM rules whenever a method is technically modified it must be balloted within the consensus organization as a new method, not a modification of the older method. Thus, the current ASTM method which contains the new validation data, procedural chang es and Quality Control IS NOT D7575

- 10, but D7575

- 1 1. The changes to D7575 were not editorial in nature, but significant (See c below) (As per ASTM rules http://www.astm.org/COMMIT/Regs.pdf )

a. Reapproval of Standards

— If approved by a motion passed by the subcommittee, or by authorization of the subcommittee chairman, reapprovals shall be issued to main committee ballot and Society Review

b. Revisions to Standards

— Revisions can be proposed at any time and shall be considered by the responsible subcommittee.

c. Editorial Changes

— Editorial changes may be made at any time without a requirement for ballot. Editorial changes are of two types: (1) those which introduce no change in technical content, but correct typographical errors, modify editorial style, change non

- technical information, or reduce ambiguity, and (2) those which correct typographical errors in substance (essential information that could be misused). In the latter case, the year designation of the standard is changed.

5. EPA in communication with me confirmed that the method D7575

- 10 did have method procedural changes (See attached email from Dr. Michael Shapiro). a. In addition to submitting additional data, ASTM also agreed to revise some of the

language in the method to clarify the scope and applicability and to add additional information to the sample pretreatment section. ASTM adopted these

revisions in Novembe r 2011. So, the following can be said about the ASTM D7575 and the EPA NODA:

> The ASTM method being considered for inclusion into the MUR is the ASTM method that contains all of the additional EPA requirements which is D7575

- 11, not

D7575

- 10.

> The EPA has not clearly identified the ASTM approved method that contains all of their required changes in the NODA.

> ASTM did not edit D7575

- 10 method and reissue it as D7575

- 10, as the changes to the

method were not editorial in nature. But instead the se changes met the requirements for a

new ASTM consensus ballot and reissuance of the method with a new date, ASTM

D7575

- 11.

> Therefore, the NODA is flawed as it seeks approval an older outdated ASTM method,

D7575

- 10, instead of the ASTM method that EPA wants D 7575

- 11. Therefore, the EPA has not provided accurate and correct information in the NODA and it does not meet the requirements of federal public notice as it did not provide accurate and clear information so the public can comment.

> Therefore, the NODA should be withdrawn. An IG investigation may be need to identify EPA staff that drafted the inaccuracies in the NODA and any other 3 rd parties that would profit from it.59 [ EPA Note: The l etter to Mike Shapiro attachment is not shown here .]

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA consulted ASTM with respect to the requested changes/clarifications and ASTM indicated (and EPA agrees) that the changes are editorial in nature, serve to provide clarification, and do not affect method performance. A copy of both versions of the method was placed in the NODA docket for comment and page 77745 discussed the changes requested by EPA and incorporated in the revised version of the method. The

- 10 versus

- 11 indicates that there are differences (editorial) between the two versions. It would be confusing to make any changes (e.g., clarification on scope and applicability) and keep the same method identifying numbe r. The Mike Shapiro letter does not imply that there were procedural changes, but merely that additional procedural details were added (as per the SOP that validation participating laboratories followed). In addition, it is not uncommon for editorial chan ges to be

made to methods between the proposal and final approval ruling. Also see response to comment

319.

Comment 318 ASTM D19 SUBCOMMITTEE ON D7575 : Commenters have discussed

that the current version ASTM D7575

- 11 be the one considered. a. Response: We agree. Explanation of the confusion: During the recent NODA study, EPA has provided some (non

- technical) language changes to ASTM D7575

- 10. These changes were constructive and added some clarification to the method. The changes were voted on and accepted by ASTM and resulted in an updated version ASTM D7575

- 11.

Response : EPA agrees the version of ASTM D -7575 it ultimately considered for promulgation in Part 136 was ASTM D7575

- 11

.

Comment 319 Patsy Root, IDEXX Laboratories : B. NODA

- specific comments: 1. This notice of data availability is for an historical ASTM method, D7575 -10. ASTM lists the valid version as: D7575-11. Could EPA explain which method it intends to promulgate?

Response : EPA discussed both methods. In the NODA, EPA specified what changes were

made to D7575

- 10 in response to EPA comments. The revised version (D7575

- 11) was added to the NODA docket to give the public the opportunity to comment on the method and the changes. ASTM D7575

- 11 is the current version of the method.

B.17 Green chemistry

C omment 283 Joe Stefkovich, Xenosep Technologies, Boonton, NJ : The driving force regarding the 1.1 million liters in n

- hexane savings/green chemistry is probably overstated by a

factor of 10 -20 times based on the method developer’s assumptions regarding the number of EPA 1664A tests performed per year.60 Response : For the reasons explained in the notice, EPA did not promulgate ASTM D7575 in Part 136 for nationwide use. Also, EPA notes that this commenter did not provide any data to support its statement.

Comment 307 William Telliard, Consultant : [EPA Note: The following is from the attachment to the comment. It contains comments from Joe Stefkovich (see comment 283) (JS) follow ed by response from William Telliard (WT response)] [JS] The driving force regarding the 1.1 million liters in n-hexane savings/green chemistry is probably overstated by a factor of 10-20 times based on the method developer’s assumptions regarding the number of EPA 1 664A tests performed per year. [WT response]: The volume of hexane saved is based on state

- by

- state evaluation of permits, both for direct

- and indirect

- discharges. A significant number of analyses are required in the pretreatment program. Perhaps JS is not familiar with the permitting process.

Response : See response to 283.

Comment 318 ASTM D19 SUBCOMMITTEE ON D7575 : Some commenters discuss the green aspects of ASTM D7575 as compared the EPA Method 1664 which uses the

neurotoxin n

- Hexane (a regulated

- against chemical in the Clean Water and Clean Air Acts). Response : Here is a table that demonstrates the green aspects of ASTM D7575 versus the principles of green chemistry

– this chart was developed in conjunction with USEPA Office of Green Chemistry personnel:

Here is a report that was submitted previously to the docket that provides great detail on the health and occupational hazards of Hexane used in EPA Method 1664. See the report and61 comment here: http://www.regulations.gov/#!documentDetail;D=EPA

- HQOW

- 2010

- 0192

- 0148

Response : EPA agrees with the green aspects of the method.

B .18 National Technology Transfer and Advancement Act (NTTAA)

C omment 283 Joe Stefkovich, Xenosep Technologies, Boonton, NJ : Method D7575 and most other Oil and Grease methods being considered for inclusion in Table IB are all not suitable for compliance monitoring of the method- defined analyte Oil and Grease and as such are not required to be promulgated per the National Technology Transfer and Advancement Act. If Method D7575 was included in Table IB and the other equally not suitable methods were not,

almost certain legal consequence would result from the other method developers due to the appearance of impropriety and inconsistent treatment of their methods by the EPA.

Response : For the reasons explained in the notice, EPA has decided not to adopt ASTM D -7575

in Part 136 for nationwide use.

EPA agrees that it is not required to approve methods adopted by voluntary consensus standard organizations under NTTAA in Part 136. Rather, Section 12(d) of the National Technology Transfer and Advancement Act (NTTAA) of 1995, (Public Law 104-113; 15 U.S.C. 272 note) directs EPA to use voluntary consensus standards in its regulatory activities unless to do so

would be inc onsistent with applicable law or is otherwise impractical. ASTM requested that EPA consider their D7575 method for promulgation and in accordance with NTTAA, EPA did so. Just as it did for other oil and grease methods in its proposed MUR. EPA re- considered ASTM D

7575 because commenters including ASTM asked us to do so and submitted additional data to support their request. EPA did not receive such requests and additional data for the other oil and grease methods that it discussed but did not propose in the 2010 proposed MUR. As such, EPA’s handling of this method was lawful.

B .19 Accuracy of v endor information

C omment 283 Joe Stefkovich, Xenosep Technologies, Boonton, NJ : A ttached with this report is a product data sheet the D7575 method developer has been distributing for the past 12 months which strongly implies the D7575 method/product is suitable for NPDES regulatory compliance testing and is a replacement for EPA 1664. While this implication is not true, inclusion in Table IB would make it “more believable” and as such, EPA would directly enable increased confusion regarding D7575 and as a result will have to deal with an unnecessary major distraction out of their control for years to come.

R esponse : EPA is not responsible for the accuracy of vendor materials.

B .20 Number of oil and grease analyses per year

C omment 283 Joe Stefkovich, Xenosep Technologies, Boonton, NJ : Developer Assumption

of 5.9 Million Oil and Grease Analyses per Year. There are approximately 20,000 NPDES Oil62 and Grease permits so some simple math would indicate that each NPDES permittee (including shopping center parking lots) would need to have their discharge points tested 295 times per year on average (5,900,000/20,000=295). Clearly this could not be the case as the typical testing frequency for most major dischargers is approximately once per month. Further analysis indicates the following approximate assumptions:

2,500 x 12/yr = 30,000 NPDES Major Discharger Tests per Year 7,500 x 4/yr = 30,000 NPDES Minor Discharger Tests per Year 10,000 x 1/yr = 10,000 NPDES Minor (Parking Lots, Schools, etc) 20,000 x 3.5/yr= 70,000 NPDES Major and Minor Tests per Year

I t is obvious that there is a huge gap between the 70,000 Oil and Grease tests easily verifiable as being required for NPDES and the developer assumption of 5,900,000 tests as being performed per year for the same NPDES permit base. Considering Conoco Phillips, the main producer of the 85% minimum purity n -hexane originally specified in the method notified the EPA in 2004 that they were discontinuing this grade of n-hexane, the true testing volume (and subsequent hexane savings of 1.1 Million Liters per Year) is most likely overs tated by a factor of

10- 20 times. This value would also most likely include all of the “unregulated” testing as well which was omitted in the Developer’s original “conservative” estimate. A much clearer picture

of the true n- hexane requirements for EPA 1 664A should be developed by EPA before proposing D7575 as this could present an extreme amount of risk to the EPA without the promised reward based on clearly questionable assumptions.

Response : EPA did not propose to withdraw Method 1664 and replace it with ASTM D7575. If EPA chose to approve the ASTM method, it would be to provide another choice of method.

Further, including permits and control mechanisms for discharges to POTWs, EPA estimates that hundreds of thousands of permits include oil and grea se limits and/or measurement requirements.

EPA does not know the exact number and the exact number is not determinative. Solventless

methods do reduce the use of n- hexane.

B .21 NPDES permit limit adjustment

C omment 297 Larry LaFluer, NCASI : In addition, as discussed below in our comments on EPA’s question 3, the whole concept of the potential need for a permit limit adjustment factor supports the conclusion that the two methods are, indeed, not comparable and do not produce equivalent results. Thus the ASTM method should not be promulgated as an alternative test procedure for oil and grease . EPA's current conclusion that permit limit adjustment based on side

- by

- side comparison s of EPA Method 1664A and ASTM D75 75

- 10 is not appropriate. EPA is particularly interested in obtaining comments from permitting authorities on this issue and estimates of the burden associated with reviewing such requests.

We believe that the fact that the methods produce sufficiently different results to

warrant an adjustment factor is essentially evidence that the methods are not equivalent. Furthermore, without knowing the specifics of why the methods produce different results,

one could not determine how representative a single evaluation of the adjustment factor would be over the long term. If the differences in results produced by the two methods were63 attributable to a specific substance, one would have to know the variability in the level of that

substance to know how to establish an appropriate adjustment factor. Alternatively, the evaluation of the adjustment factor could be performed multiple times, but we believe that the level of effort needed to develop the required insight and review those data would not be a productive use of resources.

NCASI has not examined the side

- by

- side comparison procedure in detail and therefore

offers no comments on EPA’s question number 4.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA notes that Part 136.5 does not allow for use of an adjustment factor for alternative

methods.

B.22 Replacement of EPA Method 1664 with ASTM D7575

C omment 318 ASTM D19 SUBCOMMITTEE ON D7579 : Some commenters seem to be confused in thinking that ASTM D7575 would replace EPA Method 1664. Response : ASTM D7575 has been proposed as a green alternative to EPA Method 1664. Comments have suggested that promulgating D7575 will create confusion for permit

holders and auditors since it will replace EPA Method 1664. Response : As pointed out in the NODA, the promulgation of D7575 will not replace 1664, but rather will provide an alternative method which may offer benefits to certain permit holders (for example, eliminating your
exposure to n

- hexane, which is required for 1664 and has been shown to cause neurological disorders when regularly inhaled ( http://www.regulations.gov/#!documentDetail;D=EPA

- HQ

OW

- 2010

- 0192

- 0148)

. The intent is not to force end users into one method over the other, but is

instead attempt ing to provide additional flexibility to permit holders in analyzing for oil and

grease.

Response : EPA is in agreement with the se response s

. EPA agrees that its consideration of ASTM D7575 was as an alternative to existing promulgated methods and not a re placement

.

B .23 Method portability

C omment 318 ASTM D19 SUBCOMMITTEE ON D7575 : Commenters have suggested that ASTM D7575 technology is not field

- portable. Response: Not true. ASTM D7575 has been designed specifically for and has demonstrated its field portability on several occasions

– most importantly during the Gulf of Mexico Deep Water Horizon Disaster. Please refer to slides 43, and 73 through 79 of the docket file here: http://www.regulations.gov/#!documentDetail;D=EPA

- HQ OW

- 2010

- 0192

- 0218

Response : EPA agrees with the commenter that the method is portable.64 B.24 Time required to perform test

Comment 301 Don Shelly, Food and Environmental Technical Service : Observations of Concern. 1. The ASTM method extractor can only handle one channel at a time in the event of heavy particulate loading 2. Compared to 1664, the ASTM looks like it is very time consuming

a. 20 + minutes for homogenization b. Time to manually load the extractor c. Up to 2 hours to dry membrane The ASTM method realistically will require several hours per sample. 1664 can easily extract 24 samples in 1.5 hours (using the SPE option)

Response : It is unclear what the significance of these comments is . EPA disagrees with the concerns about the time required to perform this test. See method video at http://ossmaine.com/commercial.php

.

B .25 Use of chromatography in ASTM D7575 method

C omment 301 Don Shelly, Food and Environmental Technical Service : Chromatograp hy requires manual integrations. The ASTM method requires the skills of an experiences chromatographer. 1664 only requires a trained technician

Response : Th e ASTM method does not use chromatography.

B.26 The blank must be lower than the MDL of 1.0 mg/L

C omment 290 Anonymous : The fact that the blank must be lower than the MDL of 1.0 mg/L as stated in section 12.7.1 means that many more samples will have levels reported to my customers which are not normally (the current method's blank is 5 mg/L). This will cause a general

con fusion among the public who receives these test results which will not be favorable. The public has proven throughout the years to react negatively to changes such as these.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authoriti es in 136.5, EPA is providing a response.

Vendor methods may be more restrictive than EPA methods, such as in this case. The complete sentence in the ASTM method is "The concentration of oil and grease found in the blank must be below the MDL determined in Section 12.4 [i.e., 1.0 mg/L] or less than 10% of the known concentration of the associated test samples.” Thus the blank level can be higher than 1.0 mg/L

.65 

### C. Other comments

C .1. Using the same side- by

- side comparisons when switching from Freon to N- hexane for N-hexane to infrared analysis

C omment 315 Camille Turcotte, Wisconsin Department of Natural Resources : Issue 4. Yes

same as n

- hexane because it is a defined process. [EPA Note: Th i s comment is in reference to the 4 NODA request for comment issues. For issue 4, the commenter recommends the same approach to side by side comparisons as used when switching from Freon to n

- hexane. ]

Response: EPA thanks the commenter for her comment.

C. 2

. Document availability

C omment 223 Curt McCormick : Provide a link on EPA's website to the method and allow for

download of the method at no cost for review before approving. Provide a link to all of the data referenced in the Federal Register notice (see end of F R notice).

Response : EPA cannot post methods on its website from voluntary consensus organizations such as ASTM on its website, as these are proprietary. The method was available for viewing at EPA’s

docket office. The data referenced in the Federal Register notice were available in the rulemaking docket as supporting documents are available for viewing there

.

Comment 276 Magdi Ibrahim, North Carolina Department of Environment and Natural Resources (NCDENR) : Please, provide a link to the method for download and all of the data referenced in the Federal Register notice.

Response : The docket contains all of the referenced documents. See response to comment 223.

Comment 318 ASTM D19 SUBCOMMITTEE ON D7575 : Commenters have asked for links to the method and for supporting documents. Response: The ASTM D7575 method

can be found here: http://www.astm.org/Standards/D7575.htm and the supporting materials

th at were placed in the docket 12/14/2011 can be found in the docket here: http://www.regulations.gov/#!docketDetail;dct=SR;rpp=50;so=DESC;sb=docId;po=0;D =E

PA

- HQ

- OW

- 2010

- 0192 by looking at docket ID items 196 through 220. Other previously provided supporting materials may be found here: http://www.regulations.gov/#!docketDetail;dct=SR;rpp=50;so=DESC;sb=docId;po=0;D=E

PA

- HQ

- OW

- 2010

- 0192 in docket ID items 41,55,128,135

- 148,159,163, and 170.

Response : EPA thanks the commenter

.

Comment 326 Debra Weber, Louisiana Government : In the 2010 Methods Update Rule, the EPA placed in the docket a document titled to OSS 2009, ASTM D7575 “Inter

- Laboratory Study

to Establish Precision Statements for ASTM WK23240

— Standard Test Method for Solvent

- Free66 Membrane Recoverable Oil and Grease by Infrared Determination” Since Oil and Grease is a

Method Defined Part 136.6 Method Defined Parameter:

1 The EPA should show all raw lab data that clearly demonstrated how the OSS

method compared to EPA method 1664A since the method procedural steps are extremely

different. Unlike 1664A, D7575 does not use hexane as a solvent, does not wash the sample

collection containers, in which oil and grease can adhere to, does not involve heating as 1664A..

2 The EPA should show all the matrices tested with raw data from the participating labs.

3 The EPA should show the entire interlaboratory data used to determine that this

method can achieve similar results in various matrices tested in different l aboratories. Due to

number of limited matrices and the number of laboratories used in the original OSS interlaboratory study, there is no concrete data to support the conclusion that the method even

works.

4 The EPA should make available all raw data; inte rnal and external reports associated

studies and various versions of the ASTM

- OSS method. The EPA should provide a copy of

all the supported ASTM reports used to approve the ASTM D7575 method. There was very

little time elapsed between the various ASTM D7575 versions to perform adequate lab studies.

What did the EPA used to determine that D7575 is equivalent and properly multi

- lab validated?

Response : EPA does not understand the commenter's concern, since all of these materials were

included in the docket. EPA does not normally include the raw data from NTTAA methods, but did so for this method for clarification purposes. Also see response to comment 322 in B.14.

C.3 Requests for approval of IDEXX method

C omment 260 M atthew J. Sica, Principal Scientist, Matthew Sica Consulting : Please accept the following comment of behalf of Matthew Sica Consulting: We kindly request EPA add the IDEXX Colilert-18/Quanti-Tray method (ATP Case No.

N09 -0004) at 40 CFR 136.3 either by addition to this Notice of Data Avail ability or by Supplemental Notice of Rulemaking . The ATP Case No. N09-0004 method received EPA notification on June 28, 2010 and, according to the letter, met all EPA requirements for testing at 40 CFR 136.3 at that time. By adding this method to 40 CFR 136.3 for compliance testing, EPA would remove the current regulatory barrier and make it easier for our lab, and others, to adopt this method in a more straight forward manner. Being able to adopt the Colilert-18/Quanti- Tray method will

reduce labor co sts and facilitate adhering to sample processing times for facility laboratories. Waiting for the next Method Update Rule seems an unreasonable barrier since Agency has already deemed the method fit for the intended use. Given allowances made by EPA for other methods (such as ASTM D7575-10/D7575- 11) it makes sense to include the Colilert

18/Quanti- Tray method for compliance at this time in the final NODA, another NODA specific to this method or by a Supplemental Notice of Rulemaking. Thank you for consi dering my comment. Respectfully submitted, Matthew J Sica Prinicipal Scientist Matthew Sica Consulting 29 Roger Road Vassalboro, ME 04989 207-624-1532 matthew.j.sica@gmail.com

Response : Unlike ASTMD7575, EPA did not discuss the IDEXX method in its 2010 proposed

MUR and therefore does not have the same standing as ASTM D -7575. As required by the Clean Water Act and the Administrative Procedure Act, EPA may amend its regulations in 4067 C.F.R. Part 136 to include additional methods only after notice and co mment rulemaking. EPA agrees it has been positively reviewed for nationwide use through EPA’s nationwide ATP program and will propose this method in the next Methods Update Rule.

Comment 298 Kevin Cesar, Laboratory Supervisor, City of Millbrae WPCP, CA : Please accept the following comment on behalf of City of Millbrae WPCP, Laboratory. We kindly request EPA add the IDEXX Colilert-18/Quanti-Tray method (ATP Case No.

N09 -0004) at 40 CFR 136.3 either by addition to this Notice of Data Availability or by Sup plemental Notice of Rulemaking. The ATP Case No. N09-0004 method received EPA notification on June 28, 2010 and, according to the letter, met all EPA requirements for testing at 40 CFR 136.3 at that time. By adding this method to 40 CFR 136.3 for compliance testing, EPA would remove the current regulatory barrier and make it easier for other labs to adopt this method in a more straight forward manner. The City of Millbrae has gone through the ATP procedure and ELAP and isapproved to use colilert-18 for fecal coliform but only for our own WPCP samples. The Colilert18/Quanti-Tray method has reduced our costs and has allowed us to respond much quicker operationally to problems in the plant when fecal coliform exceed our limits. Yet, other treatment plants and commercial labs cannot or will not adopt this method until it is promulgated in 40 CFR 136.3. Having other labs use this method is beneficial to us. If our sealer or incubator fails we could then sub out our samples to these labs and still get the results within 24 hours. Thank you for considering my comment.

Response : See response to comment 260.

Comment 319 Patsy Root, IDEXX Laboratories : In addition, and based on points made under A 1 above, IDEXX requests that EPA opens up a venue at this time, which would allow the

Colilert

- 1 8 for fecal coliform testing method to listed at 40 CFR Part 136.3.

Response : See response to comment 260.

Comment 327 Thomas Granato, Metropolitan Water Reclamation District of Greater Chicago : Please accept the following comment on behalf of the Monitoring and Research Depart

ment of the Metropolitan Water Reclamation District of Greater Chicago (District). We kindly request that the United States Environmental Protection Agency (USEPA) a dd

the IDEXX Colilert

- 18/Quanti

- Tray method for fecal coliform density quantification (ATP Case

No. N09

- 0004) to the lists of approved methods in the USEPA 40 Code of Federal Regulations (CFR) Part 136 for measurement of fecal coliform. It is recommended that the USEPA

include in the 40 CFR Part 136.3 the option of utilizing the commercially available IDEXX

Colilert 18/Quanti

- Tray, which is a convenient, reproducible method for determining fecal

coliform den sity in wastewater. The attached documents support t he use of this method for measuring fecal coliform in wastewater. The District may employ the IDEXX Colilert

- 18/Quant

- Tray method in special circums

tances to supplement the USEPA

- approved SM9222D, membrane filtration method for the mea

surement of fecal coliform bacteria. Adding this method to 40 CFR 136.3 for compliance testing will simplify performance of fecal coliform analyses. The Colilert

- 18/Quanti

- Tray method will reduce labor costs and facilitate adherence to sample processing times for special wet weather68 analyses in our laboratory. If you have any questions concerning this' comment, please contact Dr. Geeta Rij al at 708

- 588

- 4224. [EPA Note: The "Summary of ATP Report for Colilert* -18, Detection and Enumeration of Fecal

Coliforms in US Wastewater Samples" and "IDEXX Summary" attachments are not included here.]

Response : See response to comment 260.

C .4 Preservation

C omment 237 Department of Defense : P reservation is not verified in ASTM D7575

- 11. Proposed Requirement /Section Addressed: ASTM D7575

- 11, Section 14.2 (ASTM

D7575- 10, Section 14.2) versus Method 1664A, Section 11.2.1. Comment: ASTM D7575 does not require the pH of the sample to be checked and modified, if needed, prior to analysis as Method 1664A does. Discussion: Preservation should be verified as correct prior to analysis for both methods. Recommendation: Recommend preservation verification requirements be identified as the

same for both methods.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

EPA agrees with the commenter . In addition, the preservation and holding time requirements in

Table II of 40 CFR part 136 would be applicable.

C .5 Comment period extension

Comment 306 Jessica Skerritt, TRSA : This letter formally requests an extension for comment until June 30, 2012

, for Docket ID No. EPA

- HQ

- OW

- 2010 0192, Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act; Analysis and Sampling Procedures; Notice of Data Availability. The testing protocol for D7575 has yet to be verified applicable to the industrial laund ry sector. The primary results do not adequately reflect the measurement across all industry sectors, and with only one test there is not yet enough data for our industry for statistical validation. Industrial laundries are in the process of applying the protocol to the specific demands of the industry and are awaiting a more detailed, comprehensive study on the impacts of the protocol on the industrial laundry ind ustry. TRSA would be better able to comment after this further testing is

done. Again, to reduce the chance of unintended negative consequences, I ask that the comment period be extended until June 30, 2012 when further tests are accomplished and analyzed. TRSA represents a $16

- billion industry employing nearly 200,000 people at more than 1,500 facilities nationwide. These independent and national companies provide laundered, reusable textiles and other products and services that help businesses project a clean and attractive public image. The industry reaches every major business and industrial region and municipality in the country. Most Americans benefit at least once a week from the cleanliness and69 safety provided by the industry— through its laundering and delivery of reusable linens, uniforms, towels, floor mats and other products for the healthcare, hospitality and industrial/manufacturing sectors. TRSA member companies' services minimize environmental impacts on air, water and solid waste disposal wh ile reducing costs for millions of customers.

Response : EPA is not extending the comment period for the NODA. EPA notes that if it had promulgated ASTM D7575 in Part 136, it would have been an alternative to the existing promulgated methods rather than a requirement.

C.6 Transparency

Comment 283 Joe Stefkovich, Xenosep Technologies, Boonton, NJ : Inconsistent Treatment by EPA Regarding Various Oil and Grease Methods. EPA 1664A measures the method defined parameter commonly known as Oil and Grease. EPA has already informed the appropriate Voluntary Consensus Body and Vendor method developers of SM 5520G, ASTM D7066-04 and the Horizon Methanol Rinse-Collection that their methods would not be proposed in the upcoming MUR, Table IB due to the method-defined dif ferences of these methods with 1664A and the potential confusion they may cause within the analytical community. If EPA were to propose D7575 in the upcoming MUR, Table IB, this could be perceived as unfair and inconsistent treatment by the EPA towards th e various method developers and would almost certainly result in potential litigation due to the appearance of impropriety towards the D7575 developers.

Response : As is the case with any proposed rulemaking, based on new information or in response to comments, EPA may choose not to adopt a method it has proposed, to adopt or, where it has decided not to propose a method for adoption, may change its mind and choose to adopt something it has announced in a proposal its preliminary intention not to adopt. Often, when EPA obtains new data and information following proposal where it may take a different approach than proposed, EPA may choose to issue a notice of data ava ilability (NODA) affording the public an additional opportunity to provide comment. EPA then takes into account any additional information received in comment on the NODA prior to making a final

determination. This is the approach EPA has been followed w ith ASTM D -7575.

EPA did not receive similar comments and new data on the other oil and grease methods it discussed but did not propose. As such, the approach EPA has followed here for ASTM D7575 was not applicable to these other oil and grease methods.

Comment 319 Patsy Root, IDEXX Laboratories : A. General comments relating to procedures, transparency and equal treatment for method developers.

1

. Timeline / Transparency: The deadline for inclusion in the current MUR was July 17, 2009 as indicated by Dr Richard Reding in a letter dated July 17, 2009 ..”we are drafting the proposed rule with the methods and suggestions collected so far.”

Timeline for OSS method D7575

- 10: It is obvious from the docket that the request for

inclusion of D7575

- 10 was submitted September 2010 (EPA

- HW

- OW

- 0192

- 0209). In fact, the collection of data to satisfy EPA requirements and various meetings to that effect continued through November 2011. This resulted in EPA publishing a NODA for the OSS method on December 14, 2011.70 Timeline for IDEXX method Colilert

- 18 for fecal coliform testing: In June 2010, EPA issued a letter of positive disposition for this method indicating “.. will recommend that this method be included in future regulatory actions in which EPA periodically adds to the list of approved methods at 40 CFR Part 136.3”. Even though the IDEXX method satisfied all the requirements by June 2010 to be

included in the current MUR, we were tol d that it was too late. According to the document EPA

HW

- OW

- 0192

- 0209, Mr. Jack Hall formally requested EPA include D7575

- 10 in the current MUR in September 2010. The MUR was then published September 23, 2010 and included the

D7575

- 10 method but not the IDEXX method. This shows preferential treatment in terms of having a transparent EPA timeline for all method developers. 2. Equal Treatment of method developers: Of equal concern is the apparent ownership EPA has taken in the approval path for this method. A follow- up e

- mail from OSS to EPA (document EPA

- HQ

- OW

- 2010

- 0192

- 0145) reviews an on

- site meeting between OSS and Agency representatives in which EPA provided guidance on two options OSS could follow to get D7575-10 into the current Method Update Rule. In contrast, IDEXX had requested similar meetings to better understand EPA processes and

review our options but the Agency declined all such interactions. An explanation is in order to better understand why the Agency was so personally

involved in coach ing and recommending an approval pathway to this particular method developer.

Response : Timeline: EPA treated ASTM method D7575 in the same way it would have treated any other method at a similar stage of review that it might have been received at that time. It appears the commenter misunderstood the intent in Dr. Reding’s letter. Before EPA will inclu de a new or revised CWA method in a proposed rulemaking, the method must either have been positively reviewed by EPA as indicated by a letter to that effect) under the ATP program or have been adopted by a voluntary standards organization. It may take a significant amount of time from receipt of an ATP application to EPA to receipt of a letter from EPA indicating our positive review. Similarly, from the time a voluntary standards organization begins discussions on a new or revised method to adoption also takes significant time. Dr. Reding’s letter simply communicates that it was highly unlikely that a method that had not already begun review under the ATP program or had not already begun development by a consensus standards organization would be completed in time to include in the 2010 proposed MUR.

The above is different from a “cut

- off” date in which an ATP must have completed review or a consensus standard organization must have adopted and submitted to EPA. The cut- off date

reflects the level of inter nal and external review that EPA proposals must undergo before EPA signs a notice of proposal for publication in the Federal Register. In contrast to your method, all of the methods cited above were completed at least seven months prior to the August 2010 proposed publication date for the MUR. EPA plans to propose the IDEXX method in the next Methods Update Rule. EPA also disagrees with the statement that EPA shows preferential treatment but realizes from these comments that greater clarify and transparency are necessary in the future to avoid confusion regarding the inclusion of methods in a Methods Update Rule.

Equal Treatment: See response to comment 283. When EPA discusses a method in a proposal and it receives public comment that it needs to addres s, EPA often works with the developer (if it71 went through the ATP process) or the voluntary standards organization to respond to such

comments . T he e

- mail you cited by the commenter was dated 10/5/10- clearly after ASTM D

7575 was adopted by ASTM and clear ly after ASTM D -7575 was already discussed in the proposed MUR. As such, these interactions fall into the above category. Finally, EPA notes that it has met with IDEXX concerning their method.

Comment 325 Janet Eastep, Fairway Laboratories : Please accept the following comment on behalf of Fairway Laboratories. We kindly request EPA add the IDEXX Colilert

- 18/Quanti

- Tray method (ATP Case

No. N09

- 0004) at 40 CFR 136.3 either by addition to this Notice of Data Availability or by Supplemental Notice of Rulemak ing .

The ATP Case No. N09

- 0004 method received EPA notification on June 28, 2010 and, according to the letter, met all EPA requirements for testing at 40 CFR 136.3 at that

time. By adding this method to 40 CFR 136.3 for compliance testing, EPA would remo ve the current regulatory barrier and make it easier for our lab, and others, to adopt this method in a more straight forward manner. Being able to adopt the Colilert

- 18/Quanti

Tray method will reduce labor costs, facilitate adhering to sample processing times, and overall will help the Micro. Dept. run more smoothly on the busier days. Waiting for the next Method Update Rule seems an unreasonable barrier since Agency has already deemed the method fit for the intended use. Given allowances made by

EPA for other methods (such as ASTM D7575

- 10/D7575

- 11) it makes sense to include the

Colilert

- 18/Quanti

- Tray method for compliance at this time in the final NODA, another NODA specific to this method or by a Supplemental Notice of Rulemaking. Thank you for consid ering my comment.

Response : See response to comment 319 and comment 260 in C.3.

C.7 Duplicate samples

C omment 319 Patsy Root, IDEXX Laboratories : Requiring duplicate samples in every run

should be recommended to avoid contamination if re

- sampling from the original container presents a contamination issue.

Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part

136 for CWA compliance. Because EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response.

Also, EPA notes that the promulgated oil and grease method does not require duplicate samples.

C.8 Appropriateness of paint shaker in a certified laboratory

C omment 319 Patsy Root, IDEXX Laboratories : The use of a paint shaker doesn’t seem like appropriate equipment for a certified laboratory; suggest OSS provide an alternative process or equipment.72 Response : For the reasons specified in the notice, EPA has decided not to adopt this method for nationwide use. Permittees should continue to use an oil and grease method promulgated in Part 136 for CWA compliance. Becau se EPA recognizes that permittees may wish to request use of this method for a limited use through existing authorities in 136.5, EPA is providing a response. EPA requested that ASTM add information on the homogenization apparatus as OSS had included in SOPs they prepared for laboratories that use the method. In response to EPA’s request, this information was added to D7575-11.

C .9 EPA is purposely delaying a final ruling to allow a single method to "catch up"

Comment 319 Patsy Root, IDEXX Laboratories : Procedural : The extended delay in finalizing the current MUR in order to accommodate one method is highly unusual and not in line with prior practices. It is not fair to delay the promulgation of several other methods in order to allow one method to ‘catch up’ with work required to demonstrate qualification.

Response : EPA disagrees. The Agency did not delay promulgation of the MUR due to ASTM D7575 as demonstrated by the fact that it promulgated the final MUR in May, 2011 without a

determination on D7575 an d that it is issuing its determination through this notice after that date.