Waste Management System; Testing and Monitoring Activities; Update V of SW-846, 63185-63193 [2013-24852]

Download as PDF Federal Register / Vol. 78, No. 205 / Wednesday, October 23, 2013 / Notices 63. Because Virginia incorporated 40 CFR Part 63 by reference, Virginia should also no longer allow sources to use the former SSM exemption from the General Provisions of 40 CFR Part 63 due to the Court’s ruling in Sierra Club vs. EPA. EPA appreciates Virginia’s continuing NESHAP and NSPS enforcement efforts, and also Virginia’s decision to take automatic delegation of additional and more recent NESHAP and NSPS by adopting them by reference. Sincerely, Diana Esher, Director, Air Protection Division. This notice acknowledges the update of Virginia’s delegation of authority to implement and enforce NESHAP and NSPS. Dated: September 18, 2013. Diana Esher, Director, Air Protection Division, Region III. [FR Doc. 2013–24880 Filed 10–22–13; 8:45 am] BILLING CODE 6560–50–P ENVIRONMENTAL PROTECTION AGENCY [FRL–9901–74–Region 5] Public Hearing and Request for Comments on Proposed Revisions to Michigan’s Clean Water Act (CWA) Program Environmental Protection Agency (EPA). ACTION: Notice of proposed revisions to Michigan’s CWA Section 404 program, public hearing and request for comments. AGENCY: EPA requests comments on proposed revisions to Michigan’s CWA Section 404 permitting program resulting from the recent enactment of Michigan Public Act 98 (PA 98). EPA will hold a public hearing in Lansing, Michigan, on December 11, 2013, to take comments on the proposed program revisions. Under Section 404 of the CWA, permits are required for activities involving discharges of dredged or fill material to waters of the United States, including wetlands, lakes and streams. In 1984, Michigan assumed Section 404 permitting authority for its inland waters and wetlands. PA 98 amended the wetlands and the inland lakes and streams provisions of the Michigan’s Natural Resources and Environmental Protection Act to address areas, as identified by EPA in a 2008 program review, where the state’s Section 404 program did not comply with CWA requirements. In addition to changes to address issues identified in EPA’s program review, PA 98 included: (1) Changes to the definition of contiguous emcdonald on DSK67QTVN1PROD with NOTICES SUMMARY: VerDate Mar<15>2010 18:13 Oct 22, 2013 Jkt 232001 wetlands regulated by Michigan’s Section 404 program; (2) the addition of new exemptions from permitting; and (3) changes to the requirements for mitigating the effects of filling wetlands and other waters of the United States. Under federal regulations, substantial changes to state CWA Section 404 programs do not become effective until program revisions are approved by EPA. Information about PA 98, the resulting proposed revisions to Michigan’s Section 404 program, the public hearing, and procedures for submitting comments is available at: www.regulations.gov/ (insert: EPA–HQ– OW–2013–0710 in the search field). On December 11, 2013, at 7:00 p.m. EST, EPA will hold a public hearing to take oral and written comments at the Crowne Plaza Lansing West (formerly known as the Lexington Lansing Hotel), 925 South Creyts Road, Lansing, Michigan 48917. The formal hearing will be preceded by an informational session at 6:00 p.m. EST. Written comments will also be accepted until December 18, 2013. DATES AND LOCATION: Submit comments, referencing Docket ID No. EPA–HQ– OW–2013–0710, online using www.regulations.gov (the preferred method); by email to owdocket@epa.gov; or by mail to: EPA Docket Center, Environmental Protection Agency, Mail Code 28221T, 1200 Pennsylvania Ave. NW., Washington, DC 20460. All comments received will be included in the public docket without change, including any personal information provided, unless the comment includes profanity, threats, information claimed to be Confidential Business Information, or other information whose disclosure is restricted by statute. ADDRESSES: For further information, call toll-free, 800– 621–8431, weekdays, 8:30 a.m. to 4:30 p.m., central time, or contact Sue Elston, at the EPA Docket Center address noted above. FOR FURTHER INFORMATION CONTACT: Dated: September 27, 2013. Timothy C. Henry, Acting Director, Water Division, EPA Region 5. [FR Doc. 2013–24841 Filed 10–22–13; 8:45 am] BILLING CODE 6560–50–P PO 00000 Frm 00028 Fmt 4703 Sfmt 4703 63185 ENVIRONMENTAL PROTECTION AGENCY [EPA–HQ–RCRA–2012–0072; FRL–9901–86– OSWER] Waste Management System; Testing and Monitoring Activities; Update V of SW–846 Environmental Protection Agency (EPA). ACTION: Notice. AGENCY: The Environmental Protection Agency (EPA or the Agency) is providing notice of the availability of ‘‘Update V’’ to the Third Edition of EPA publication SW–846, ‘‘Test Methods for Evaluating Solid Waste, Physical/ Chemical Methods.’’ Update V contains 23 new and revised analytical methods that the Agency has evaluated, and determined to be appropriate and which may be used for monitoring or complying with the Resource Conservation and Recovery Act (RCRA) hazardous and non-hazardous waste regulations. Because the analytical methods contained in Update V are not required by the RCRA hazardous waste regulations, EPA is issuing this update as guidance. In addition, the Agency is also taking comment on revisions to Chapters One through Five of EPA publication SW–846, an ORCR Policy Statement, and other guidance. The Agency is seeking public comment on Update V, and after consideration of the public comments, will place these new and revised methods, guidance, and chapters in the SW–846 methods compendium. SUMMARY: Comments must be received on or before January 21, 2014. ADDRESSES: Submit your comments, identified by Docket ID No. EPA–HQ– RCRA–2012–0072, by one of the following methods: • www.regulations.gov: Follow the on-line instructions for submitting comments. • Email: RCRA-docket@epa.gov, Attention Docket ID No. EPA–HQ– RCRA–2012–0072. • Fax: Fax comments to: 202–566– 9744, Attention Docket ID No. EPA– HQ–RCRA–2012–0072. • Mail: Send comments to: OSWER Docket, EPA Docket Center, Mail Code 28221T, Environmental Protection Agency, 1200 Pennsylvania Avenue NW., Washington, DC 20460, Attention Docket ID No. EPA–HQ–RCRA–2012– 0072. Please include two copies of your comments. • Hand Delivery: Deliver two copies of your comments to: Environmental Protection Agency, EPA Docket Center, DATES: E:\FR\FM\23OCN1.SGM 23OCN1 emcdonald on DSK67QTVN1PROD with NOTICES 63186 Federal Register / Vol. 78, No. 205 / Wednesday, October 23, 2013 / Notices Room 3334, 1301 Constitution Avenue NW., Washington DC, Attention Docket ID No. EPA–HQ–RCRA–2012–0072. Such deliveries are only accepted during the docket’s normal hours of operation and special arrangements should be made for deliveries of boxed information. Instructions: Direct your comments to EPA–HQ–RCRA–2012–0072. EPA’s policy is that all comments received will be included in the public docket without change and may be made available online at www.regulations.gov, including any personal information provided, unless the comment includes information claimed to be Confidential Business Information (CBI) or other information whose disclosure is restricted by statute. Do not submit information that you consider to be CBI or otherwise protected through www.regulations.gov or email. The www.regulations.gov Web site is an ‘‘anonymous access’’ system, which means EPA will not know your identity or contact information unless you provide it in the body of your comment. If you send an email comment directly to EPA without going through www.regulations.gov, your email address will be automatically captured and included as part of the comment that is placed in the public docket and made available on the Internet. If you submit an electronic comment, EPA recommends that you include your name and other contact information in the body of your comment and with any disk or CD–ROM you submit. If EPA cannot read your comment due to technical difficulties and cannot contact you for clarification, EPA may not be able to consider your comment. Electronic files should avoid the use of special characters, any form of encryption, and be free of any defects or viruses. For additional information about EPA’s public docket, visit the EPA Docket Center homepage at https:// www.epa.gov/epahome/dockets.htm. Docket: All documents in the docket are listed in the www.regulations.gov index. Although listed in the index, some information is not publicly available, e.g., CBI or other information whose disclosure is restricted by statute. Certain other material, such as copyrighted material, will be publicly available only in hard copy. Publicly available docket materials are available either electronically in www.regulations.gov or in hard copy at the OSWER Docket, EPA/DC, EPA West, Room 3334, 1301 Constitution Ave. NW., Washington, DC. The Public Reading Room is open from 8:30 a.m. to 4:30 p.m., Monday through Friday, excluding legal holidays. The telephone VerDate Mar<15>2010 18:13 Oct 22, 2013 Jkt 232001 number for the Public Reading Room is (202) 566–1744, and the telephone number for the OSWER Docket is (202) 566–0270. FOR FURTHER INFORMATION CONTACT: Kim Kirkland, Materials Recovery and Waste Management Division, Office of Resource Conservation and Recovery, Office of Solid Waste and Emergency Response (5304P), Environmental Protection Agency, 1200 Pennsylvania Ave. NW., Washington, DC 20460; telephone number: 703–308–8855; fax number: 703–308–0522; email address: kirkland.kim@epa.gov. SUPPLEMENTARY INFORMATION: I. General Information A. Does this action apply to me? This notice is directed to the public in general. It may, however, be of particular interest to you if you conduct waste sampling and analysis for RCRArelated activities. This might include any entity that generates, treats, stores, or disposes of hazardous or nonhazardous solid waste and is subject to RCRA subtitle C or D sampling and analysis requirements, and might also include any laboratory that conducts waste sampling and analyses for such entities. B. What should I consider as I prepare my comments for EPA? 1. Submitting CBI. Do not submit this information to EPA through www.regulations.gov or email. Clearly mark the part or all of the information that you claim to be CBI. For CBI information on a disk or CD ROM that you mail to EPA, mark the outside of the disk or CD ROM as CBI and then identify electronically within the disk or CD ROM the specific information that is claimed as CBI. In addition to one complete version of the comment that includes information claimed as CBI, a copy of the comment that does not contain the information claimed as CBI must be submitted for inclusion in the public docket. Information so marked will not be disclosed except in accordance with the procedures set forth in 40 CFR part 2. 2. Tips for Preparing Your Comments. When submitting comments, remember to: • Identify the rulemaking by docket number and other identifying information (subject heading, Federal Register date and page number). • Follow directions—The agency may ask you to respond to specific questions or organize comments by referencing a Code of Federal Regulations (CFR) part or section number. PO 00000 Frm 00029 Fmt 4703 Sfmt 4703 • Explain why you agree or disagree; suggest alternatives and substitute language for your requested changes. • Describe any assumptions and provide any technical information and/ or data that you used. • If you estimate potential costs or burdens, explain how you arrived at your estimate in sufficient detail to allow for it to be reproduced. • Provide specific examples to illustrate your concerns, and suggest alternatives. • Explain your views as clearly as possible, avoiding the use of profanity or personal threats. • Make sure to submit your comments by the comment period deadline identified. C. How can I get copies of Update V and the Third Edition of SW–846 as amended by its Final Updates? Update V is available in the RCRA docket and the final version will be available on-line after all comments have been addressed. The Third Edition of SW–846, as amended by Final Updates I, II, IIA, IIB, III, IIIA, IIIB, IVA, and IVB, is available in portable document format (PDF) on EPA’s Office of Resource Conservation and Recovery (ORCR) Web page at: https:// www.epa.gov/SW-846. D. How is the rest of this notice organized? The rest of this Notice includes the following sections: II. What is the subject and purpose of this notice? III. Why is the Agency releasing Update V to SW–846? IV. What does Update V contain? A. OSWER/ORCR Policy Statement B. Changes to QA/QC Guidance V. Summary II. What is the subject and purpose of this notice? The Agency is announcing the availability of and inviting public comment on Update V to ‘‘Test Methods for Evaluating Solid Waste, Physical/ Chemical Methods’’, EPA Publication SW–846. Update V of SW–846 contains analytical methods that the Agency has evaluated, and/or revised and determined to be appropriate and may be used for monitoring or complying with the RCRA hazardous waste regulations. Because the analytical methods contained in Update V are not required by the RCRA hazardous waste regulations, EPA is issuing this update as guidance. This guidance does not add or change the RCRA regulations, and does not have any impact on existing rulemakings associated with the RCRA E:\FR\FM\23OCN1.SGM 23OCN1 Federal Register / Vol. 78, No. 205 / Wednesday, October 23, 2013 / Notices program. To date, the Agency has finalized Updates I, II, IIA, IIB, III, IIIA, IIIB, IVA, and IVB to the SW–846 manual, which can be found on the EPA’s ORCR Web page at: https:// www.epa.gov/SW-846. emcdonald on DSK67QTVN1PROD with NOTICES III. Why is the Agency releasing Update V to SW–846? The Agency revises the content of SW–846 over time as new information and data become available. We continually review advances in analytical instrumentation and techniques and periodically incorporate such advances into SW–846 as method updates by adding new methods to the manual, and replacing existing methods with revised versions of the same method. These updates improve analytical method performance and cost effectiveness. Since the publication of the Methods Innovation Rule (MIR) (70 FR 34537, June 14, 2005), the Agency no longer needs to use a rulemaking process for publication of an update to SW–846, as long as the update does not contain a method required by the RCRA regulations (e.g., Method-Defined Parameter (MDP), such as the Toxicity Characteristic Leaching Procedure (TCLP) (Method 1311)), see 40 CFR 260.11. The Agency instead can make an SW–846 update available to the public more efficiently through a Federal Register notice announcing its availability and inviting public comment on the update. In addition, the MIR allows flexibility in method selection and use for meeting the analytical needs of the RCRA program, with the exception of those methods specifically required by the RCRA regulations. This approach is consistent with the Agency’s commitment to fully implement a performance-based measurement system (PBMS), whereby the analytical focus is on measurement objectives and performance rather than specific measurement technologies. Furthermore, the Agency’s PBMS approach has evolved resulting in the Agency adopting the new ‘‘Flexible Approaches to Environmental Measurement—The Evolution of the Performance Approach’’ as developed by the Forum on Environmental Measurements (FEM) at the direction of EPA’s Science Policy Council (i.e., now the Science and Technology Policy Council (STPC)). One of the main goals of the Performance Approach is to increase flexibility in choosing sampling and analytical approaches to meet regulatory requirements for measurements. For more information on VerDate Mar<15>2010 18:13 Oct 22, 2013 Jkt 232001 the Performance Approach, see: https:// www.epa.gov/fem/approach.htm. In using the SW–846 methods, the regulated entity need only demonstrate that an analytical method generates data that meet the project-specific data quality objectives (DQOs) and performance acceptance criteria. The Agency finds this flexible approach to be particularly useful, and sufficient in most cases, during the characterization of the complex matrices of RCRArelated wastes. Thus, a method user can modify an SW–846 method (provided it is not one specifically required by regulation, e.g., 40 CFR 260.11), in order to best meet a waste matrix-specific analytical need, as long as the modifications meet the project-specific DQOs and performance acceptance criteria. The public should note that in some cases the method established certain requirements (e.g., conducting a calibration curve, using specific reagents, analyzing a Quality Control (QC) check sample to demonstrate precision and accuracy). While these standard principles are not regulatory requirements, they are necessary to yield data of acceptable quality as intended and are called for by sound science. (The public can obtain more information about the MIR and PBMS at the Agency’s Web site dedicated to SW– 846 and the testing of RCRA-regulated wastes: https://www.epa.gov/SW-846.) The subject of today’s notice, Update V to SW–846, contains 23 new and revised analytical methods and revises Chapters One through Five of SW–846. After the comment period, and based on the Agency’s evaluation of the comments received, the new and revised methods and revised chapters will be formally included in the SW– 846 methods compendium. Most of the Update V methods previously resided under the heading ‘‘New Methods’’ at EPA’s SW–846 Web site as either revised versions of existing SW–846 methods or as new methods that the Agency planned to add to SW–846. Although these methods were not yet part of an official update to any edition of the SW–846 manual at the time of their posting on the Web site, the Agency wanted to make these Agencyevaluated methods available for use and comment as soon as possible. The Agency believed that public access to these new and revised methods, for guidance purposes, would assure that reliable and innovative methods are provided to the regulated community in a timely and cost-effective manner. Therefore, these methods could be used for any RCRA applications, other than one specifically required by regulation, for which their performance could be PO 00000 Frm 00030 Fmt 4703 Sfmt 4703 63187 demonstrated to be appropriate and meet project-specific DQOs, and thus be consistent with implementation and promotion of a flexible and performance-based approach to RCRArelated analyses. The Agency is also responding to concerns expressed by the Environmental Laboratory Advisory Board (ELAB), a Federal Advisory Committee Act (FACA) committee that advises the Agency on measurement, monitoring, and laboratory science issues, who contacted EPA’s FEM with several issues regarding the use of SW– 846. The ELAB specifically contacted EPA regarding which version of a revised method is recommended. Historically, as noted above, the Agency has posted new and revised methods on the SW–846 Web site under the ‘‘New Test Methods Online’’ (at: https:// www.epa.gov/epawaste/hazard/ testmethods/sw846/new_meth.htm), for use by the laboratory community, the States, and the regulated community pending publication of these methods in the Federal Register. The Agency was subsequently contacted by the ELAB, who identified several concerns regarding the process for updating and posting updates on the ‘‘New Test Methods Online’’ link on the SW–846 Web site. ELAB requested that EPA clarify those issues that caused some confusion with some entities of the user community. Specifically, confusion existed when a method had multiple versions available on the web. For example, Method 8000C, on the ’’New Test Methods Online’’ link has quality control (QC) guidelines that differ from Method 8000B (the official version) in the SW–846 compendium. The public was confused by the difference in QC guidelines in the two available versions of the method. The Agency subsequently decided that the revisions to Method 8000C were more significant than those previously posted, and has decided to replace Method 8000C with Method 8000D, and is issuing Method 8000D as part of Update V. In response to ELAB’s concerns, ORCR prepared a Policy Statement that identifies the status of methods (e.g., validated methods, final methods, etc.), and provides the rationale for identifying when changes to methods are significant, through a letter designation and by noting the date the method was revised by ORCR. For more information on the ORCR Policy Statement, see section IV of this Notice. Finally, the Agency is requesting public comment on the Update V methods and the other relevant updated materials presented in this Notice for E:\FR\FM\23OCN1.SGM 23OCN1 63188 Federal Register / Vol. 78, No. 205 / Wednesday, October 23, 2013 / Notices emcdonald on DSK67QTVN1PROD with NOTICES inclusion in the SW–846 manual (i.e., Table of Contents and Chapters One through Five). See the ADDRESSES section of this notice for the procedure for submitting comments. The Agency will consider public comments submitted on or before the comment period deadline and subsequently finalize Update V as an official part of SW–846. In addition, the EPA SW–846 Web site contains an updated version of the ‘‘Method Status Table for SW–846,’’ which identifies the update history for each document in SW–846. The Agency strongly recommends the use of the latest version of an SW–846 method, especially for new analyte monitoring situations. The Agency, however, is not imposing restrictions on the use of earlier versions of nonrequired SW–846 methods or precluding the use of previous guidance, if such use is appropriate. For example, earlier versions of an SW–846 method may be more appropriate for regulatory purposes (e.g., for compliance with an existing permit or consent decree), or when new method versions may be more costly than necessary for meeting project-specific objectives. In the future, the Agency plans to make electronic copies of earlier versions of SW–846 methods available through a separate hyperlink from the SW–846 Web site. The Agency hopes that the posting of this information on the Web site for immediate public access will mitigate any remaining confusion regarding the use of SW–846 methods. In addition, the public can also access the Methods Information Communication Exchange (MICE) for answers to their questions or concerns regarding SW–846 methods. MICE can be accessed by phone at (703) 818–3238, by fax at (703) 818–8813, or by email at mice@techlawinc.com. IV. What does Update V contain? Update V contains 23 new and revised analytical methods, revised versions of Chapters One through Five of EPA publication SW–846, the ORCR Policy Statement, and other guidance (e.g., quality assurance/quality control (QA/QC) guidance on lower limit of quantitation (LLOQ), relative standard error (RSE), initial demonstration of proficiency (IDP), etc.), each dated October 2012 and identified as ‘‘Update V’’ in the document footer. For the convenience of the reader, EPA has identified key areas of interest in the sections below, but all the methods and other information for which the Agency is seeking comments are contained in the docket for this Notice. Table 1 (included at the end of this Notice) provides a listing of the five revised VerDate Mar<15>2010 18:13 Oct 22, 2013 Jkt 232001 chapters and twenty-three methods (eight new and fifteen revised methods) in Update V. After consideration of comments received from publication of this Notice, Update V, including the revised versions of Chapters One through Five, will be incorporated into the SW–846 methods compendium. A. OSWER/ORCR Policy Statement In 2008, ELAB requested that ORCR describe their plan for releasing Updates to SW–846, as well as clarify the status of deleted, obsolete, previous versions or revised methods, and a statement regarding the status of previous versions of methods. In addition, ELAB raised the following additional concerns and suggestions: • Clarification is needed regarding which method is the final version in SW–846. • Many states are not adopting the final version of new methods. • States may not have the resources to certify multiple versions of final methods. • Some of the regulated community doesn’t know how the method revision varied. EPA has engaged in several face-toface meetings with the ELAB at national conferences to address their requests and resolve their concerns and suggestions. As a result of those meetings, ORCR developed a policy statement intended to clarify the basic terminology used in SW–846 regarding the status of methods and how the SW– 846 Methods program develops and releases methods to the public. That policy statement, entitled ‘‘USEPA Office of Resource Conservation and Recovery Policy on the Use of Test Methods for Evaluating Solid Waste, Physical/Chemical Methods (SW–846)’’ provides background on SW–846, general guidance on the procedures for adopting methods into SW–846, and defines key terms used to identify the status of methods in SW–846. Below is the ORCR Policy Statement, a copy of which has also been placed in the docket associated with this Federal Register Notice: USEPA Office of Solid Waste and Emergency Response/Office of Resource Conservation and Recovery Policy on the Use of ‘‘Test Methods for Evaluating Solid Waste, Physical/Chemical Methods’’ (SW–846) The United States Environmental Protection Agency’s (EPA) Office of Resource Conservation and Recovery (ORCR) provides analytical and sampling methods to assist the regulated and regulatory community and others in implementing the Resource PO 00000 Frm 00031 Fmt 4703 Sfmt 4703 Conservation and Recovery Act (RCRA). These methods are published in the Test Methods for Evaluating Solid Waste, Physical/Chemical Methods (SW–846) and are available on the ORCR Web site (www.epa.gov./epawaste/hazard/ testmethods/index.htm). With the exception of those particular methods which are promulgated in the regulations to implement RCRA (see 40 CFR 260.11), the remaining methods are considered guidance, and users may select any scientifically appropriate method when conducting analyses to comply with the RCRA regulatory program. The Methods Innovation Rule (MIR) published on June 14, 2005 (70 FR 34538), reemphasized the flexible approach in method selection, when appropriate, when testing for compliance, under RCRA. Since the publication of this rule, ORCR no longer uses a formal rulemaking process for publication of method updates to SW– 846. EPA informs the regulated and regulatory community of new methods and updates to SW–846 and solicits comments on them through a Notice of Availability published in the Federal Register. This approach is consistent with ORCR’s commitment to fully implement the Agency’s performancebased measurement system (PBMS) approach to regulation. A new effort was developed and approved to reinvigorate the goals of PBMS with the versatility of each of our program’s needs. It is called the Flexible Approaches to Environmental Measurements—The Evolution of the Performance Approach which the Science and Technology Policy Council (STPC) approved on February 15, 2008. In 2009, ORCR subsequently adopted the new ‘‘Performance Approach’’ as defined by the Forum on Environmental Measurements (FEM). The FEM is a standing committee of senior EPA Environmental Protection managers established to develop policies to guide the Agency’s measurement community in: validating and disseminating methods for sample collection and analysis; for ensuring that monitoring studies are scientifically rigorous, statistically sound, and yield representative measurements; and for employing a quality systems approach that ensures that the data gathered and used by the Agency are of known and documented quality. After shortening the name of the PBMS effort to the ‘‘Performance Approach,’’ the FEM’s Performance Approach Action Team took a look at the issues surrounding the lack of the program’s progress with the ultimate conclusion that the ‘‘one size fits all’’ E:\FR\FM\23OCN1.SGM 23OCN1 emcdonald on DSK67QTVN1PROD with NOTICES Federal Register / Vol. 78, No. 205 / Wednesday, October 23, 2013 / Notices approach does not work for the diversely different programs and authorities each of our major program offices (i.e., air, pesticides, waste, and water) has in carrying out their work. To avoid the proliferation of terminology, ORCR has adopted the ‘‘Flexible Approach’’ which is consistent with ORCR’s approach to environmental management, based on the goals and statutes of EPA program offices. Under the PBMS approach for RCRA, when labs conducted regulatory required monitoring, the regulated community had to either employ a scientifically appropriate method published in SW–846 or use any other scientifically appropriate method from another reliable source. This is still true under the Flexible Approach. However, when choosing a reliable alternative source, the focus should be on measurement objectives, rather than on measurement technologies. In all cases, the user must demonstrate the method selected generates data that are appropriate for the intended use. Although both approaches are applicable for RCRA, ORCR had dropped the term PBMS, and strongly supports the use of the new Flexible Approach to be consistent with the Agency’s new guidance that allows each program to determine program specific flexibility when addressing waste analysis issues. ORCR strongly recommends that persons use the latest version of a SW–846 method whenever possible, especially in new monitoring situations, since updated versions of the methods EPA publishes generally are in the Agency’s view less subject to misinterpretation, yield improved precision and/or bias, or provide for the use of newer and, often, more costeffective technologies. In situations where it may not be appropriate to use the latest method in SW–846, earlier versions may be used. These situations may include, but are not limited to, those where an earlier version of a method is required for existing permits, consent decrees, waste analysis plans or sampling analysis plans. In addition, laboratories, especially small laboratories, may find a previous version of a SW–846 method appropriate if it is more cost-effective in meeting the project-specific objectives. The Agency is not imposing restrictions on the use of earlier versions of nonrequired methods contained in SW–846 or precluding the use of previous guidance. Nonetheless, the adoption of the latest method version is recommended and should be accomplished as soon as possible, as appropriate. When methods are VerDate Mar<15>2010 18:13 Oct 22, 2013 Jkt 232001 employed, it is the responsibility of the user to ensure that the method yields data of a quality appropriate for the particular application for which it is being used. EPA views the methods in the SW–846 compendium as tools for the user to employ in developing individual standard operating procedures to meet the goals and objectives of specific projects. This approach enables the user to optimize and modify methods for effective performance on unique projects. The SW–846 methods are for most applications considered as guidance with the exception of those methods required by the RCRA regulations (i.e., Method-Defined Parameters (MDPs), see 40 CFR 260.11). In situations where the user is not certain whether the selected method or method modification is appropriate, EPA recommends regulated entities contact and seek approval as needed from the appropriate regulatory agency (e.g., Federal or State/local government) before applying any method on a specific project, including situations where the method is used verbatim. EPA may publish new methods, revise existing methods, or withdraw methods from the SW–846 compendium whenever it deems it appropriate. For example, methods may be updated in order to reflect new advancements in technology, to reflect the addition of new performance data, or to clarify areas of the procedure that experience indicates may be misunderstood. Methods may also be revised to reflect new EPA policy regarding the use of certain chemicals and reagents. In other cases, methods are removed if the technology is no longer available or applicable. ORCR has developed specific procedures for releasing updates, revisions, or withdrawing methods, which are designed to minimize disruption to regulatory processes. Specific definitions for the terms associated with a method’s status, which support the change procedures, have been developed and provided below. The Agency will only post the most recent version of a final SW–846 method on the ORCR Web page as part of the SW–846 methods compendium (www.epa.gov./epawaste/hazard/ testmethods/index.htm). Prior versions of methods formerly contained in SW–846 and still considered appropriate for use will be available through a separate hyperlink in the future. EPA’s objective is to identify and make available on the Agency’s SW–846 Web site the latest information regarding the methodologies that generate effective data at minimum PO 00000 Frm 00032 Fmt 4703 Sfmt 4703 63189 costs in response to new technological or scientific advancements, while, at the same time, making available earlier versions for those situations where such methods may be needed or appropriate (e.g., to determine how a particular analysis had been performed, to determine how to comply with a specific permit requirement, etc.). SW–846 Methods Status Definitions Analytical methods are officially made a part of the SW–846 manual through a rigorous process of technical evaluation both within the Agency and through external review. Methods are also revised as needed after a formal evaluation process by analytical experts (e.g., SW–846 work and focus groups) and an announcement of method availability and request for public comment in the Federal Register as a Notice of Availability. During the method development/evaluation process, the methods go through various stages of review and revision. The methods are officially included as part of an update to the most current edition of SW–846 at the conclusion of this process. ORCR employs a specific naming convention (i.e., method number and letter suffix) when publishing methods. The naming convention is intended to minimize confusion within the user community regarding a method’s developmental status. The method number designates the underlying technology (e.g., 8000 series methods designate determinative procedures for organic compounds). A revision to a method where the underlying technology does not change is indicated by continued use of the same method number and letter, but with a new issuance date. If the revision retains the underlying technology, but does not affect the precision and/or accuracy of the data, the revision is considered to be minor or nonsignificant and the method number and letter is not changed or sequenced. If, on the other hand, the revision retains the underlying technology, but changes the precision and/or accuracy of the data, the change is considered to be significant and is indicated by a subsequent letter suffix (e.g., changes from 8270C to 8270D) and a new issuance date. For example, if the quality control recommendations are changed in a manner that improves the bias or precision of the method, but does not change the underlying technology (e.g., a tightening of the calibration acceptance criteria), the method number stays the same, but the letter suffix is sequenced to the next letter. The differences between the E:\FR\FM\23OCN1.SGM 23OCN1 emcdonald on DSK67QTVN1PROD with NOTICES 63190 Federal Register / Vol. 78, No. 205 / Wednesday, October 23, 2013 / Notices earlier and later versions of a method are detailed in the method summary section of the revised version regardless of the type of change. Examples of changes that may be considered minor or nonsignificant include, but are not limited to: Language added to a method to provide increased clarity or guidance; expansion of lists of acceptable instrumentation, applicability of the method to a matrix not previously referenced, adding new compounds to the list of applicable compounds, or changes to instrument specifications which do not result in an existing acceptable instrument being rendered unacceptable; or formatting and editorial changes that are designed to improve readability or correct spelling or grammatical errors. ORCR has defined a ‘‘significant change’’ as a change that results in improved analytical results (e.g., changes that result in reducing analytical bias or improving data precision). Examples of significant changes may include, but are not limited to: a change in the operating parameter which reduces analytical flexibility; a change in instrumentation specification which minimizes interference and/or optimizes instrument performance (if the use of such interference reduction technique or performance enhancement is required); a change in calibration guidance which results in more restrictive recommendations; a change that institutes tighter QC recommendations; or a change in the reagents that are required by the method. ORCR understands revisions are sometimes necessary to either enhance the performance of the method or to allow flexibilities due to the complexity of sample matrices. In situations where the user is not certain whether the selected method, method modification or modification to their plan is appropriate, EPA recommends the regulated community seek approval from the appropriate regulatory agency (e.g., Federal or State/local government, client) before their use of a revised method; amend their plan (e.g., Project Plan, Quality Assurance Project Plan (QAPP), Sampling and Analysis Plan (SAP), Standard Operating Procedure (SOP)); and properly document the change when reporting analytical results. The following method status definitions reflect the current method development process and have been developed to add clarity for the method users. ORCR uses these definitions and the terms may vary for other program offices. VerDate Mar<15>2010 18:13 Oct 22, 2013 Jkt 232001 Final Method—A method that has been formally adopted into the most recent version of the SW–846 compendium. Before a method becomes final, the validated version would have been made available for public review and comment in a Notice of Availability (NOA) or a proposed rulemaking, as appropriate. Validated Method—A method that has undergone development and technical review by EPA, but has not been formally adopted into the SW–846 method compendium and published through a Federal Register Notice. Since this review includes technical work group approval and/or inter-laboratory validation, validated methods are included on the Agency Web site for evaluation and use by the public and as a means of soliciting comment from the broader scientific community. The public may use a validated method prior to its inclusion in the SW–846 compendium, provided that the users demonstrate that it generates data that are appropriate for the intended use. Revised Method—A method included in SW–846 that has been updated to reflect changes that may be editorial in nature and do not impact data or performance comparability, that broaden the method to introduce new technologies that may increase productivity, but do not change the fundamental technology, or that change the quality control requirements to increase bias or precision. The number of a method that has been revised does not change, but the method may receive a subsequent letter suffix. If the revision is a significant one (as defined above) then both the letter suffix and the issuance date are updated. If, on the other hand, the revision is editorial in nature, or consists of the addition of new performance data, then only the issuance date is changed. Previous versions are not precluded from being used provided that the users demonstrate that it generates data that are appropriate for the intended use. Draft Method—A new method that is being evaluated for possible inclusion into SW–846. It represents the latest innovative technological advancements in scientific methodology, but has not completed technical review by EPA nor been subject to notice and comment in the Federal Register. Superseded Method—A superseded method is an earlier version of an SW– 846 method or other guidance that is no longer included in the SW–846 compendium and has been replaced by a newer version. Revised versions of Superseded methods should be viewed as the preferred method. Methods in PO 00000 Frm 00033 Fmt 4703 Sfmt 4703 this category are removed from the compendium, but remain available on line and are not precluded for use where required for existing projects or where an adequate justification for use exists. The term ‘‘Superseded’’ is documented in the method title as listed on the EPA Web site for prior versions of final methods followed by the date it was superseded. Withdrawn Method—A method or other guidance that EPA strongly recommends not be used, (e.g., cyanide and sulfide reactivity guidance withdrawn, June 14, 2005). EPA has determined that such procedures or methods, for the use or technical objectives for which they were originally published, are technically inadequate and/or no longer meet such use or technical objectives. This does not mean, however, that there would be no situations under which the procedures or methods may be appropriate. In any situation in which a person may believe that the withdrawn method is appropriate, we strongly encourage consultation with applicable regulatory agencies at the state or federal level. The prospective user of the method will need to demonstrate the old method is, indeed, appropriate. Any use of these methods, without any such consultation and demonstration, will be done at the user’s risk. The Agency understands that earlier versions of the SW–846 methods that aren’t required may still be in use to meet project specific criteria (e.g., permits, sampling plans, Consent Decrees, etc.). Permits and other plans formally approved by regulatory authorities that specify the use of particular methods for required analysis continue in effect unless they are changed. However, the Agency encourages the regulated community to use the latest version of SW–846, when applicable. EPA will continue to update the Methods Status Table to inform the public as to the status of methods in SW–846 and the Policy Statement will be added to the SW–846 methods compendium when the Update V package is finalized. [end of policy statement] B. Changes to Chapters One Through Five and QA/QC Guidance (Chapter One and Individual Methods) in SW–846 In general, EPA’s revisions to Chapters One through Five to EPA publication SW–846 reflects the new method style guide format and added all the Update V methods and new letters/ version to the appropriate related method sections. Specifically: E:\FR\FM\23OCN1.SGM 23OCN1 emcdonald on DSK67QTVN1PROD with NOTICES Federal Register / Vol. 78, No. 205 / Wednesday, October 23, 2013 / Notices • Chapter One of SW–846 was revised to make it more user friendly and to be more consistent with the Agency’s official guidance on QA/QC implementation and procedures (e.g., Quality Assurance Project Plans (QAPPS), Data Quality Objectives (DQOs), and the Flexible Approach to Environmental Measurement). • Chapter Two now includes a Table of Contents to make finding the information easier. In addition, a typographical error was found for bis(2chloroisopropyl) ether and was corrected to bis(2-chloro-1-methylethyl) ether in Tables 2–1, 2–4, 2–15, 2–22, and 2–34. Furthermore, Table 2–40(A) was revised to reflect the current sample preservation guidance for styrene and vinyl chloride in aqueous samples (i.e., deletion of previously recommended practice of collecting a second set of samples without acid preservatives and analyze immediately, if styrene and vinyl chloride are analytes of interest) and Table 2–40(B) was revised to include Mercury Speciation hold times in addition to totals. • Chapter Three was revised so that the definition for instrument detection limit (IDL) is consistent with the revised methods 6010D and 6020B. In addition, the term ‘‘accuracy’’ was replaced by ‘‘bias’’ where appropriate; the definition for linear range was revised to be consistent with methods 6010D and 6020B; the definition of interference check sample (ICS) was replaced with the spectral interference check (SIC) solution to be consistent with methods 6010D and 6020B; and the definition of ‘‘laboratory control sample’’ was revised to recommend the use of a spiking solution from the same source as the calibration standards. Also, the collision/reaction cell technology was added to Sections 3.6 and 3.7 as an effective method for removing isobaric interferences when analyzing by ICP– MS and a minimum collection mass of 100 g was added to Table 3–2 for solid samples collected for sulfide analysis. • Chapter Four (see Table 4–1) was reformatted and updated by removing the recommendation to collect a second set of samples without adding an acid preservative and analyze in a shorter time frame if vinyl chloride and styrene are analytes of concern for aqueous samples. • Chapter 5 had no significant changes outside of general ones specified above (e.g., updated format changes and method reference to chapters). In addition, EPA is incorporating three new and revised QC features in Chapter One and the Update V methods, where appropriate, for RCRA VerDate Mar<15>2010 18:13 Oct 22, 2013 Jkt 232001 compliance monitoring which warrant further discussion here. A summary of changes to chapters in SW–846 are provided in Appendix A of each chapter. The new and revised features that have been added to Chapter One (Quality Control) and individual methods (where appropriate) are: • Lower Limit of Quantitation (LLOQ)—References to the Method Detection Limit (MDL) have been replaced with the LLOQ. It is recommended to establish the LLOQ as the lowest point of quantitation, which, in most cases, is the concentration of the lowest calibration standard in the calibration curve that has been adjusted for the preparation mass and/or volume. The LLOQ value is a function of both the analytical method and the sample being evaluated. Why is MDL removed and replaced by LLOQ for SW–846? ORCR has removed references to the MDL procedure (i.e., 40 CFR 136, Appendix B) beginning with Update IV and from the revised and new Update V methods and has recommended establishing the LLOQ. We continue to refine the procedure for establishing the LLOQ. The refined procedure considers sample matrix effects; provides a provision to verify the reasonableness of the reported quantitation limit (QL); and recommends a frequency of LLOQ verification (found in Chapter One and each method) to be balanced between rigor and practicality. (Note: The agency understands that previous versions of methods published in SW–846 may contain the MDL reference. However, as methods are updated, EPA will remove the reference to the MDL, and will remove the reference in older methods that have not yet been updated, as time and resources allow. Therefore, ORCR recommends that LLOQ be used, as appropriate, for the methods that have not yet been updated. See the Section 9.8 in Method 6020B for inorganic analytes and Section 9.7 in Method 8000 for organic analytes on LLOQ for further information on implementation.) ORCR understands that other EPA programs may continue to use MDLs to meet their program use and needs (e.g., the National Pollutant Discharge Elimination System (NPDES) permit program). However, ORCR has found that the procedure in 40 CFR 136, Appendix B, for the determination of MDLs, developed for the Clean Water Act (CWA) program uses a clean matrix (e.g., reagent water for preparing ‘‘spiked’’ samples, or samples with known constituent concentrations). Analytical laboratories often have PO 00000 Frm 00034 Fmt 4703 Sfmt 4703 63191 difficulty demonstrating they can meet the MDL established using Part 136 when evaluating complex matrices, such as wastes. The procedure outlined in Part 136 is generally not suitable for RCRA wastes or materials because the MDL approach generally yields unrealistic and/or unachievable method detection limits for the complex matrices (e.g., soils, sludges, wipes, and spent materials) encountered under the RCRA program. The MDLs are normally calculated from analysis of a sample that does not cause matrix interferences (typically determined using spiked reagent water). However, most wastes evaluated for compliance with RCRA consist of complex matrices. The LLOQ considers the effect of sample matrix (e.g., components of a sample other than the analyte) by taking the sample through the entire analytical process, including sample preparation, clean up (to remove sample interferences), and determinative procedures. Also, if method users choose, the LLOQ sample can be included at the end of the run to see if it meets the established acceptance criteria. Lastly, results above the LLOQ are quantifiable within an acceptable precision and bias. Thus, the LLOQ approach better suits the needs of the RCRA program, because it provides reliable and defensible results, especially at the lower level of quantitation, and can be reported with a known level of confidence for the complex matrices being evaluated. SW–846 methods are being used by various programs in implementing various statutes, including RCRA, the Comprehensive Environmental Response, Compensation and Liability Act (CERCLA), the Toxic Substances Control Act (TSCA), and Homeland Security Presidential Directives, for waste and materials characterization, compliance testing, site/incident characterization and risk assessment for protection of human health and the environment, and better management and use of wastes and materials, for a wide range of difficult matrices. ORCR believes that the LLOQ approach is an important improvement, and supports the essential need to provide data that are verified to meet the precision and accuracy requirements of the Agency’s program needs. Establishing LLOQ for Inorganic analytes: When performing methods for inorganic analyses, the LLOQ should be verified by the analysis of at least seven replicate samples (prepared in a clean matrix or control material) and spiked at the LLOQ and processed through all preparation and analysis steps of the method. The mean recovery and relative standard deviation (RSD) of these E:\FR\FM\23OCN1.SGM 23OCN1 emcdonald on DSK67QTVN1PROD with NOTICES 63192 Federal Register / Vol. 78, No. 205 / Wednesday, October 23, 2013 / Notices samples provide an initial statement of precision and bias at the LLOQ. In most cases, the mean recovery should be ±35% of the true value and the RSD should be ≤20%. Ongoing LLOQ verification, at a minimum, is on a quarterly basis to validate quantitation capability at low analyte concentration levels. This verification may be accomplished either with clean control material (e.g., reagent water, method blanks, Ottawa sand, diatomaceous earth, etc.) or a representative sample matrix free of target compounds. Optimally, the LLOQ should be less than the desired regulatory action levels based on the stated project-specific requirements. For more information, please see the individual methods (e.g., Methods 6010 and 6020) and Chapter One of SW–846. Establishing LLOQ for organic analytes: When performing methods for organic analyses, the LLOQ should be verified using either a clean control material (e.g., reagent water, method blanks, Ottawa sand, diatomaceous earth, etc.) or a representative sample matrix free of target compounds. Optimally, the LLOQ should be less than the desired regulatory action levels based on the stated project-specific requirements. For organic analyses, the acceptable recovery ranges of target analytes will vary more than for other types of analyses, such as inorganics. The recovery of target analytes in the LLOQ check sample should be within established limits, or other such projectrequired acceptance limits, for precision and bias to verify the data reporting limits. Until the laboratory has sufficient data to determine acceptance limits statistically, a limit of 20% +/¥ the Laboratory Control Sample (LCS) criteria may be used for the LLOQ acceptance criteria. This approach acknowledges the poorer overall response at the low end of the calibration curve. Historically based LLOQ acceptance criteria should be determined as soon as practical once sufficient data points have been acquired. In-house limits for bias (e.g., % Recovery) and precision (e.g., Relative Percent Difference, %RPD) of the LLOQ for a particular sample matrix may be calculated when sufficient data points exist. The laboratory should have a documented procedure for establishing its in-house acceptance ranges. Sometimes the laboratory instrument and/or analyst performance vary or test samples cause problems with the detector (e.g., samples may have interferences; may clog the instruments VerDate Mar<15>2010 18:13 Oct 22, 2013 Jkt 232001 cells, wall or tube; may cause contamination; etc.). Therefore, the limits of acceptance (for precision and bias) are established by a lab with sufficient data to demonstrate that they can report down to the LLOQ with a certain level of confidence. The acceptance limits (for precision and bias) for LLOQ may be established by the laboratory or at the project level through the data quality objectives in a quality assurance project plan. The frequency of the LLOQ check is not specified for organic analytes. Note: The LLOQ check sample should be spiked with the analytes of interest at the predicted LLOQ concentration levels and carried through the same preparation and analysis procedures as environmental samples and other QC samples. For more information, please see individual methods (e.g., Method 8000) and Chapter One of SW– 846. How is LLOQ used? The RCRA program deals with complex wastes and materials that are managed or used in many different ways (e.g., landfilling, land application, incineration, recycling). The thresholds (e.g., action or remediation levels) for data users (e.g., engineers or risk assessors) to make their decisions, therefore, vary. Method users will need to properly plan their analytical strategy to ensure the LLOQs for targeted analytes are lower than the thresholds needed to generate data used to determine how waste or materials can be properly managed or used. • Initial Demonstration of Performance (IDP)—The laboratory must make an initial demonstration of ability to generate results with acceptable accuracy and precision for each preparation and determinative method they perform. This demonstration should be performed prior to independently analyzing real sample matrices by each analytical method and should be repeated if other changes occur (e.g., significant change in procedure, new staff are trained, etc.). Documentation of the IDP should be maintained by the Quality Assurance Manager. Each laboratory should have a training program documenting that a new analyst is capable of performing the method or portion of the method for which the analyst is responsible. This demonstration should document that the new analyst is capable of successfully following the standard operating procedure (SOP) based on the laboratory’s IDP policy. For Update V, changes to the IDP have been specified in the individual Update V methods where appropriate (e.g., PO 00000 Frm 00035 Fmt 4703 Sfmt 4703 screening method where there is not a quantitative reporting limit such as a bioassay method). The IDP changes allow laboratories to use their time and resources effectively, especially for the organic analyses. Key Changes in the IDP for the Determination of Organic Analytes: The IDP section was expanded to describe two situations: When a significant change to instrumentation or procedure occurs: Reliable performance of the methods is dependent on careful adherence to the instructions in the written method, and aspects of the method are mandatory to ensure that the method performs as intended. Therefore, if a major change to the sample preparation procedure is made (e.g., a change of solvent), the IDP must be repeated for that preparation procedure to demonstrate the laboratory technician’s continued ability to reliably perform the method. EPA considers conducting IDPs as part of good laboratory practice procedures and has already included these procedures in EPA’s laboratories practices. Alterations in instrumental procedures only (e.g., changing Gas Chromatograph (GC) temperature programs or High Performance Liquid Chromatography (HPLC) mobile phases or the detector interface), require a new calibration, but not a new IDP because the preparation procedure is unchanged. When new staff members are trained: A new analyst needs to be capable of performing the method, or portion of the method, for which the analyst is responsible. For example, when analysts are trained for a subset of analytes for an 8000 series method, the new sample preparation analyst should prepare reference samples for a representative set of analytes (e.g., the primary analyte mix for Method 8270, or a mix of Aroclor 1016 and 1260 for Method 8082) for each preparation method the analyst will be performing. The instrument analyst being trained will need to analyze prepared samples (e.g., semi-volatile extracts). • Relative Standard Error (RSE)— ORCR evaluated and included, as the analytical community recommended, RSE as an option (in addition to calculation of the % error) in SW–846 for the determination of the acceptability for a linear or non-linear calibration curve. RSE refits the calibration data back to the calibration model and evaluates the difference between the measured and the true amounts or concentrations used to create the model. E:\FR\FM\23OCN1.SGM 23OCN1 Federal Register / Vol. 78, No. 205 / Wednesday, October 23, 2013 / Notices Where: xi = True amount of analyte in calibration level i, in mass or concentration units. x´i = Measured amount of analyte in calibration level i, in mass or concentration units. p = Number of terms in the fitting equation (average = 1, linear = 2, quadratic = 3, cubic = 4). n = Number of calibration points. The RSE acceptance limit criterion for the calibration model is the same as the RSD limit in the determinative method. If the RSD limit is not defined in the determinative method, the RSE limit should be set at ≤20% for good performing compounds and ≤30% for poor performing compounds. V. Summary EPA believes that these changes in Update V will assist the method users to demonstrate method competency and generate better quality data. For the convenience of the analytical community, the Agency will revise the OSWER Methods’ Team homepage on 63193 EPA’s Web site with updated information to better communicate new policy and analytical procedures, and will include Update V and selected documents at that Web site after Update V is finalized. Please see the Web site: https:// www.epa.gov/epawaste/hazard/ testmethods/index.htm for more information. Table 1 provides a listing of the five chapters and twenty-three methods (eight new and fifteen revised methods) in Update V. TABLE 1—UPDATE V (METHODS, CHAPTERS AND GUIDANCE) Analytical method No. 1030 ............ 3200 * .......... 3511 * .......... 3572 * .......... 3620C .......... 4025 * .......... 4430 * .......... 4435 * .......... 5021A .......... 6010D .......... 6020B .......... 6800 ............ 8000D .......... 8021B .......... 8111 ............ 8270D .......... 8276 * .......... 8410 ............ 8430 ............ 9013A .......... 9014 ............ 9015 * .......... 9320 ............ Method or chapter title Table of Contents. Chapter One—Quality Control. Chapter Two—Choosing the Correct Procedure. Chapter Three—Inorganic Analytes. Chapter Four—Organic Analytes. Chapter Five—Miscellaneous Test Methods. Methods Status Table. Ignitability of Solids. Mercury Species Fractionation and Quantification by Microwave-Assisted Extraction, Selective Solvent Extraction and/or Solid Phase Extraction. Organic Compounds in Water by Microextraction. Extraction of Wipe Samples for Chemical Agents. Florisil Cleanup. Screening for Polychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans (PCDD/Fs) by Immunoassay. Screening for Polychlorinated Dibenzo-p-Dioxins and Furans (PCDD/Fs) by Aryl Hydrocarbon Receptor PCR Assay. Method for Toxic Equivalent (TEQS) Determination for Dioxin-Like Chemical Activity With the CALUX® Bioassay. Volatile Organic Compounds in Various Sample Matrices Using Equilibrium Headspace Analysis. Inductively Coupled Plasma-Atomic Emission Spectrometry. Inductively Coupled Plasma-Mass Spectrometry. Elemental and Speciated Isotope Dilution Mass Spectrometry. Determinative Chromatographic Separations. Aromatic and Halogenated Volatiles by Gas Chromatography Using Photoionization and/or Electrolytic Conductivity Detectors. Haloethers by Gas Chromatography. Semivolatile Organic Compounds by Gas Chromatography/Mass Spectrometry. Toxaphene and Toxaphene Congeners by Gas Chromatography/Negative Ion Chemical Ionization Mass Spectrometry (GC–NICI/ MS). Gas Chromatography/Fourier Transform Infrared Spectrometry for Semivolatile Organics: Capillary Column. Analysis of Bis (2-Chloroethyl) Ester and Hydrolysis Products by Direct Aqueous Injection. Cyanide Extraction Procedure for Solids and Oils. Titrimetric and Manual Spectrophotometric Determinative Methods for Cyanide. Metal Cyanide Complexes by Anion Exchange Chromatography and UV Detection. Radium 228. Dated: September 27, 2013. Barnes Johnson, Acting Director, Office of Resource Conservation and Recovery. FARM CREDIT ADMINISTRATION [FR Doc. 2013–24852 Filed 10–22–13; 8:45 am] AGENCY: BILLING CODE 6560–50–P VerDate Mar<15>2010 18:13 Oct 22, 2013 Jkt 232001 Farm Credit Administration Board; Sunshine Act; Regular Meeting Farm Credit Administration. SUMMARY: Notice is hereby given, pursuant to the Government in the PO 00000 Frm 00036 Fmt 4703 Sfmt 4703 Sunshine Act, of the regular meeting of the Farm Credit Administration Board (Board). The regular meeting of the Board will be held at the offices of the Farm Credit Administration in McLean, Virginia, on October 10, 2013, DATE AND TIME: E:\FR\FM\23OCN1.SGM 23OCN1 EN23OC13.003</GPH> emcdonald on DSK67QTVN1PROD with NOTICES * New Methods.

Agencies

[Federal Register Volume 78, Number 205 (Wednesday, October 23, 2013)]
[Notices]
[Pages 63185-63193]
From the Federal Register Online via the Government Printing Office [www.gpo.gov]
[FR Doc No: 2013-24852]


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ENVIRONMENTAL PROTECTION AGENCY

[EPA-HQ-RCRA-2012-0072; FRL-9901-86-OSWER]


Waste Management System; Testing and Monitoring Activities; 
Update V of SW-846

AGENCY: Environmental Protection Agency (EPA).

ACTION: Notice.

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SUMMARY: The Environmental Protection Agency (EPA or the Agency) is 
providing notice of the availability of ``Update V'' to the Third 
Edition of EPA publication SW-846, ``Test Methods for Evaluating Solid 
Waste, Physical/Chemical Methods.'' Update V contains 23 new and 
revised analytical methods that the Agency has evaluated, and 
determined to be appropriate and which may be used for monitoring or 
complying with the Resource Conservation and Recovery Act (RCRA) 
hazardous and non-hazardous waste regulations. Because the analytical 
methods contained in Update V are not required by the RCRA hazardous 
waste regulations, EPA is issuing this update as guidance. In addition, 
the Agency is also taking comment on revisions to Chapters One through 
Five of EPA publication SW-846, an ORCR Policy Statement, and other 
guidance. The Agency is seeking public comment on Update V, and after 
consideration of the public comments, will place these new and revised 
methods, guidance, and chapters in the SW-846 methods compendium.

DATES: Comments must be received on or before January 21, 2014.

ADDRESSES: Submit your comments, identified by Docket ID No. EPA-HQ-
RCRA-2012-0072, by one of the following methods:
     www.regulations.gov: Follow the on-line instructions for 
submitting comments.
     Email: RCRA-docket@epa.gov, Attention Docket ID No. EPA-
HQ-RCRA-2012-0072.
     Fax: Fax comments to: 202-566-9744, Attention Docket ID 
No. EPA-HQ-RCRA-2012-0072.
     Mail: Send comments to: OSWER Docket, EPA Docket Center, 
Mail Code 28221T, Environmental Protection Agency, 1200 Pennsylvania 
Avenue NW., Washington, DC 20460, Attention Docket ID No. EPA-HQ-RCRA-
2012-0072. Please include two copies of your comments.
     Hand Delivery: Deliver two copies of your comments to: 
Environmental Protection Agency, EPA Docket Center,

[[Page 63186]]

Room 3334, 1301 Constitution Avenue NW., Washington DC, Attention 
Docket ID No. EPA-HQ-RCRA-2012-0072. Such deliveries are only accepted 
during the docket's normal hours of operation and special arrangements 
should be made for deliveries of boxed information.
    Instructions: Direct your comments to EPA-HQ-RCRA-2012-0072. EPA's 
policy is that all comments received will be included in the public 
docket without change and may be made available online at 
www.regulations.gov, including any personal information provided, 
unless the comment includes information claimed to be Confidential 
Business Information (CBI) or other information whose disclosure is 
restricted by statute. Do not submit information that you consider to 
be CBI or otherwise protected through www.regulations.gov or email. The 
www.regulations.gov Web site is an ``anonymous access'' system, which 
means EPA will not know your identity or contact information unless you 
provide it in the body of your comment. If you send an email comment 
directly to EPA without going through www.regulations.gov, your email 
address will be automatically captured and included as part of the 
comment that is placed in the public docket and made available on the 
Internet. If you submit an electronic comment, EPA recommends that you 
include your name and other contact information in the body of your 
comment and with any disk or CD-ROM you submit. If EPA cannot read your 
comment due to technical difficulties and cannot contact you for 
clarification, EPA may not be able to consider your comment. Electronic 
files should avoid the use of special characters, any form of 
encryption, and be free of any defects or viruses. For additional 
information about EPA's public docket, visit the EPA Docket Center 
homepage at https://www.epa.gov/epahome/dockets.htm.
    Docket: All documents in the docket are listed in the 
www.regulations.gov index. Although listed in the index, some 
information is not publicly available, e.g., CBI or other information 
whose disclosure is restricted by statute. Certain other material, such 
as copyrighted material, will be publicly available only in hard copy. 
Publicly available docket materials are available either electronically 
in www.regulations.gov or in hard copy at the OSWER Docket, EPA/DC, EPA 
West, Room 3334, 1301 Constitution Ave. NW., Washington, DC. The Public 
Reading Room is open from 8:30 a.m. to 4:30 p.m., Monday through 
Friday, excluding legal holidays. The telephone number for the Public 
Reading Room is (202) 566-1744, and the telephone number for the OSWER 
Docket is (202) 566-0270.

FOR FURTHER INFORMATION CONTACT: Kim Kirkland, Materials Recovery and 
Waste Management Division, Office of Resource Conservation and 
Recovery, Office of Solid Waste and Emergency Response (5304P), 
Environmental Protection Agency, 1200 Pennsylvania Ave. NW., 
Washington, DC 20460; telephone number: 703-308-8855; fax number: 703-
308-0522; email address: kirkland.kim@epa.gov.

SUPPLEMENTARY INFORMATION: 

I. General Information

A. Does this action apply to me?

    This notice is directed to the public in general. It may, however, 
be of particular interest to you if you conduct waste sampling and 
analysis for RCRA-related activities. This might include any entity 
that generates, treats, stores, or disposes of hazardous or 
nonhazardous solid waste and is subject to RCRA subtitle C or D 
sampling and analysis requirements, and might also include any 
laboratory that conducts waste sampling and analyses for such entities.

B. What should I consider as I prepare my comments for EPA?

    1. Submitting CBI. Do not submit this information to EPA through 
www.regulations.gov or email. Clearly mark the part or all of the 
information that you claim to be CBI. For CBI information on a disk or 
CD ROM that you mail to EPA, mark the outside of the disk or CD ROM as 
CBI and then identify electronically within the disk or CD ROM the 
specific information that is claimed as CBI. In addition to one 
complete version of the comment that includes information claimed as 
CBI, a copy of the comment that does not contain the information 
claimed as CBI must be submitted for inclusion in the public docket. 
Information so marked will not be disclosed except in accordance with 
the procedures set forth in 40 CFR part 2.
    2. Tips for Preparing Your Comments. When submitting comments, 
remember to:
     Identify the rulemaking by docket number and other 
identifying information (subject heading, Federal Register date and 
page number).
     Follow directions--The agency may ask you to respond to 
specific questions or organize comments by referencing a Code of 
Federal Regulations (CFR) part or section number.
     Explain why you agree or disagree; suggest alternatives 
and substitute language for your requested changes.
     Describe any assumptions and provide any technical 
information and/or data that you used.
     If you estimate potential costs or burdens, explain how 
you arrived at your estimate in sufficient detail to allow for it to be 
reproduced.
     Provide specific examples to illustrate your concerns, and 
suggest alternatives.
     Explain your views as clearly as possible, avoiding the 
use of profanity or personal threats.
     Make sure to submit your comments by the comment period 
deadline identified.

C. How can I get copies of Update V and the Third Edition of SW-846 as 
amended by its Final Updates?

    Update V is available in the RCRA docket and the final version will 
be available on-line after all comments have been addressed. The Third 
Edition of SW-846, as amended by Final Updates I, II, IIA, IIB, III, 
IIIA, IIIB, IVA, and IVB, is available in portable document format 
(PDF) on EPA's Office of Resource Conservation and Recovery (ORCR) Web 
page at: https://www.epa.gov/SW-846.

D. How is the rest of this notice organized?

    The rest of this Notice includes the following sections:
    II. What is the subject and purpose of this notice?
    III. Why is the Agency releasing Update V to SW-846?
    IV. What does Update V contain?
    A. OSWER/ORCR Policy Statement
    B. Changes to QA/QC Guidance
    V. Summary

II. What is the subject and purpose of this notice?

    The Agency is announcing the availability of and inviting public 
comment on Update V to ``Test Methods for Evaluating Solid Waste, 
Physical/Chemical Methods'', EPA Publication SW-846. Update V of SW-846 
contains analytical methods that the Agency has evaluated, and/or 
revised and determined to be appropriate and may be used for monitoring 
or complying with the RCRA hazardous waste regulations. Because the 
analytical methods contained in Update V are not required by the RCRA 
hazardous waste regulations, EPA is issuing this update as guidance. 
This guidance does not add or change the RCRA regulations, and does not 
have any impact on existing rulemakings associated with the RCRA

[[Page 63187]]

program. To date, the Agency has finalized Updates I, II, IIA, IIB, 
III, IIIA, IIIB, IVA, and IVB to the SW-846 manual, which can be found 
on the EPA's ORCR Web page at: https://www.epa.gov/SW-846.

III. Why is the Agency releasing Update V to SW-846?

    The Agency revises the content of SW-846 over time as new 
information and data become available. We continually review advances 
in analytical instrumentation and techniques and periodically 
incorporate such advances into SW-846 as method updates by adding new 
methods to the manual, and replacing existing methods with revised 
versions of the same method. These updates improve analytical method 
performance and cost effectiveness. Since the publication of the 
Methods Innovation Rule (MIR) (70 FR 34537, June 14, 2005), the Agency 
no longer needs to use a rulemaking process for publication of an 
update to SW-846, as long as the update does not contain a method 
required by the RCRA regulations (e.g., Method-Defined Parameter (MDP), 
such as the Toxicity Characteristic Leaching Procedure (TCLP) (Method 
1311)), see 40 CFR 260.11. The Agency instead can make an SW-846 update 
available to the public more efficiently through a Federal Register 
notice announcing its availability and inviting public comment on the 
update.
    In addition, the MIR allows flexibility in method selection and use 
for meeting the analytical needs of the RCRA program, with the 
exception of those methods specifically required by the RCRA 
regulations. This approach is consistent with the Agency's commitment 
to fully implement a performance-based measurement system (PBMS), 
whereby the analytical focus is on measurement objectives and 
performance rather than specific measurement technologies. Furthermore, 
the Agency's PBMS approach has evolved resulting in the Agency adopting 
the new ``Flexible Approaches to Environmental Measurement--The 
Evolution of the Performance Approach'' as developed by the Forum on 
Environmental Measurements (FEM) at the direction of EPA's Science 
Policy Council (i.e., now the Science and Technology Policy Council 
(STPC)). One of the main goals of the Performance Approach is to 
increase flexibility in choosing sampling and analytical approaches to 
meet regulatory requirements for measurements. For more information on 
the Performance Approach, see: https://www.epa.gov/fem/approach.htm.
    In using the SW-846 methods, the regulated entity need only 
demonstrate that an analytical method generates data that meet the 
project-specific data quality objectives (DQOs) and performance 
acceptance criteria. The Agency finds this flexible approach to be 
particularly useful, and sufficient in most cases, during the 
characterization of the complex matrices of RCRA-related wastes. Thus, 
a method user can modify an SW-846 method (provided it is not one 
specifically required by regulation, e.g., 40 CFR 260.11), in order to 
best meet a waste matrix-specific analytical need, as long as the 
modifications meet the project-specific DQOs and performance acceptance 
criteria. The public should note that in some cases the method 
established certain requirements (e.g., conducting a calibration curve, 
using specific reagents, analyzing a Quality Control (QC) check sample 
to demonstrate precision and accuracy). While these standard principles 
are not regulatory requirements, they are necessary to yield data of 
acceptable quality as intended and are called for by sound science. 
(The public can obtain more information about the MIR and PBMS at the 
Agency's Web site dedicated to SW-846 and the testing of RCRA-regulated 
wastes: https://www.epa.gov/SW-846.)
    The subject of today's notice, Update V to SW-846, contains 23 new 
and revised analytical methods and revises Chapters One through Five of 
SW-846. After the comment period, and based on the Agency's evaluation 
of the comments received, the new and revised methods and revised 
chapters will be formally included in the SW-846 methods compendium. 
Most of the Update V methods previously resided under the heading ``New 
Methods'' at EPA's SW-846 Web site as either revised versions of 
existing SW-846 methods or as new methods that the Agency planned to 
add to SW-846. Although these methods were not yet part of an official 
update to any edition of the SW-846 manual at the time of their posting 
on the Web site, the Agency wanted to make these Agency-evaluated 
methods available for use and comment as soon as possible. The Agency 
believed that public access to these new and revised methods, for 
guidance purposes, would assure that reliable and innovative methods 
are provided to the regulated community in a timely and cost-effective 
manner. Therefore, these methods could be used for any RCRA 
applications, other than one specifically required by regulation, for 
which their performance could be demonstrated to be appropriate and 
meet project-specific DQOs, and thus be consistent with implementation 
and promotion of a flexible and performance-based approach to RCRA-
related analyses.
    The Agency is also responding to concerns expressed by the 
Environmental Laboratory Advisory Board (ELAB), a Federal Advisory 
Committee Act (FACA) committee that advises the Agency on measurement, 
monitoring, and laboratory science issues, who contacted EPA's FEM with 
several issues regarding the use of SW-846. The ELAB specifically 
contacted EPA regarding which version of a revised method is 
recommended. Historically, as noted above, the Agency has posted new 
and revised methods on the SW-846 Web site under the ``New Test Methods 
Online'' (at: https://www.epa.gov/epawaste/hazard/testmethods/sw846/new_meth.htm), for use by the laboratory community, the States, and 
the regulated community pending publication of these methods in the 
Federal Register. The Agency was subsequently contacted by the ELAB, 
who identified several concerns regarding the process for updating and 
posting updates on the ``New Test Methods Online'' link on the SW-846 
Web site.
    ELAB requested that EPA clarify those issues that caused some 
confusion with some entities of the user community. Specifically, 
confusion existed when a method had multiple versions available on the 
web. For example, Method 8000C, on the ''New Test Methods Online'' link 
has quality control (QC) guidelines that differ from Method 8000B (the 
official version) in the SW-846 compendium. The public was confused by 
the difference in QC guidelines in the two available versions of the 
method. The Agency subsequently decided that the revisions to Method 
8000C were more significant than those previously posted, and has 
decided to replace Method 8000C with Method 8000D, and is issuing 
Method 8000D as part of Update V.
    In response to ELAB's concerns, ORCR prepared a Policy Statement 
that identifies the status of methods (e.g., validated methods, final 
methods, etc.), and provides the rationale for identifying when changes 
to methods are significant, through a letter designation and by noting 
the date the method was revised by ORCR. For more information on the 
ORCR Policy Statement, see section IV of this Notice.
    Finally, the Agency is requesting public comment on the Update V 
methods and the other relevant updated materials presented in this 
Notice for

[[Page 63188]]

inclusion in the SW-846 manual (i.e., Table of Contents and Chapters 
One through Five). See the ADDRESSES section of this notice for the 
procedure for submitting comments. The Agency will consider public 
comments submitted on or before the comment period deadline and 
subsequently finalize Update V as an official part of SW-846. In 
addition, the EPA SW-846 Web site contains an updated version of the 
``Method Status Table for SW-846,'' which identifies the update history 
for each document in SW-846.
    The Agency strongly recommends the use of the latest version of an 
SW-846 method, especially for new analyte monitoring situations. The 
Agency, however, is not imposing restrictions on the use of earlier 
versions of non-required SW-846 methods or precluding the use of 
previous guidance, if such use is appropriate. For example, earlier 
versions of an SW-846 method may be more appropriate for regulatory 
purposes (e.g., for compliance with an existing permit or consent 
decree), or when new method versions may be more costly than necessary 
for meeting project-specific objectives. In the future, the Agency 
plans to make electronic copies of earlier versions of SW-846 methods 
available through a separate hyperlink from the SW-846 Web site.
    The Agency hopes that the posting of this information on the Web 
site for immediate public access will mitigate any remaining confusion 
regarding the use of SW-846 methods. In addition, the public can also 
access the Methods Information Communication Exchange (MICE) for 
answers to their questions or concerns regarding SW-846 methods. MICE 
can be accessed by phone at (703) 818-3238, by fax at (703) 818-8813, 
or by email at mice@techlawinc.com.

IV. What does Update V contain?

    Update V contains 23 new and revised analytical methods, revised 
versions of Chapters One through Five of EPA publication SW-846, the 
ORCR Policy Statement, and other guidance (e.g., quality assurance/
quality control (QA/QC) guidance on lower limit of quantitation (LLOQ), 
relative standard error (RSE), initial demonstration of proficiency 
(IDP), etc.), each dated October 2012 and identified as ``Update V'' in 
the document footer. For the convenience of the reader, EPA has 
identified key areas of interest in the sections below, but all the 
methods and other information for which the Agency is seeking comments 
are contained in the docket for this Notice. Table 1 (included at the 
end of this Notice) provides a listing of the five revised chapters and 
twenty-three methods (eight new and fifteen revised methods) in Update 
V. After consideration of comments received from publication of this 
Notice, Update V, including the revised versions of Chapters One 
through Five, will be incorporated into the SW-846 methods compendium.

A. OSWER/ORCR Policy Statement

    In 2008, ELAB requested that ORCR describe their plan for releasing 
Updates to SW-846, as well as clarify the status of deleted, obsolete, 
previous versions or revised methods, and a statement regarding the 
status of previous versions of methods. In addition, ELAB raised the 
following additional concerns and suggestions:
     Clarification is needed regarding which method is the 
final version in SW-846.
     Many states are not adopting the final version of new 
methods.
     States may not have the resources to certify multiple 
versions of final methods.
     Some of the regulated community doesn't know how the 
method revision varied.
    EPA has engaged in several face-to-face meetings with the ELAB at 
national conferences to address their requests and resolve their 
concerns and suggestions. As a result of those meetings, ORCR developed 
a policy statement intended to clarify the basic terminology used in 
SW-846 regarding the status of methods and how the SW-846 Methods 
program develops and releases methods to the public. That policy 
statement, entitled ``USEPA Office of Resource Conservation and 
Recovery Policy on the Use of Test Methods for Evaluating Solid Waste, 
Physical/Chemical Methods (SW-846)'' provides background on SW-846, 
general guidance on the procedures for adopting methods into SW-846, 
and defines key terms used to identify the status of methods in SW-846. 
Below is the ORCR Policy Statement, a copy of which has also been 
placed in the docket associated with this Federal Register Notice:
USEPA Office of Solid Waste and Emergency Response/Office of Resource 
Conservation and Recovery Policy on the Use of ``Test Methods for 
Evaluating Solid Waste, Physical/Chemical Methods'' (SW-846)
    The United States Environmental Protection Agency's (EPA) Office of 
Resource Conservation and Recovery (ORCR) provides analytical and 
sampling methods to assist the regulated and regulatory community and 
others in implementing the Resource Conservation and Recovery Act 
(RCRA). These methods are published in the Test Methods for Evaluating 
Solid Waste, Physical/Chemical Methods (SW-846) and are available on 
the ORCR Web site (www.epa.gov./epawaste/hazard/testmethods/index.htm). 
With the exception of those particular methods which are promulgated in 
the regulations to implement RCRA (see 40 CFR 260.11), the remaining 
methods are considered guidance, and users may select any 
scientifically appropriate method when conducting analyses to comply 
with the RCRA regulatory program.
    The Methods Innovation Rule (MIR) published on June 14, 2005 (70 FR 
34538), reemphasized the flexible approach in method selection, when 
appropriate, when testing for compliance, under RCRA. Since the 
publication of this rule, ORCR no longer uses a formal rulemaking 
process for publication of method updates to SW-846. EPA informs the 
regulated and regulatory community of new methods and updates to SW-846 
and solicits comments on them through a Notice of Availability 
published in the Federal Register. This approach is consistent with 
ORCR's commitment to fully implement the Agency's performance-based 
measurement system (PBMS) approach to regulation.
    A new effort was developed and approved to reinvigorate the goals 
of PBMS with the versatility of each of our program's needs. It is 
called the Flexible Approaches to Environmental Measurements--The 
Evolution of the Performance Approach which the Science and Technology 
Policy Council (STPC) approved on February 15, 2008. In 2009, ORCR 
subsequently adopted the new ``Performance Approach'' as defined by the 
Forum on Environmental Measurements (FEM). The FEM is a standing 
committee of senior EPA Environmental Protection managers established 
to develop policies to guide the Agency's measurement community in: 
validating and disseminating methods for sample collection and 
analysis; for ensuring that monitoring studies are scientifically 
rigorous, statistically sound, and yield representative measurements; 
and for employing a quality systems approach that ensures that the data 
gathered and used by the Agency are of known and documented quality.
    After shortening the name of the PBMS effort to the ``Performance 
Approach,'' the FEM's Performance Approach Action Team took a look at 
the issues surrounding the lack of the program's progress with the 
ultimate conclusion that the ``one size fits all''

[[Page 63189]]

approach does not work for the diversely different programs and 
authorities each of our major program offices (i.e., air, pesticides, 
waste, and water) has in carrying out their work. To avoid the 
proliferation of terminology, ORCR has adopted the ``Flexible 
Approach'' which is consistent with ORCR's approach to environmental 
management, based on the goals and statutes of EPA program offices.
    Under the PBMS approach for RCRA, when labs conducted regulatory 
required monitoring, the regulated community had to either employ a 
scientifically appropriate method published in SW-846 or use any other 
scientifically appropriate method from another reliable source. This is 
still true under the Flexible Approach. However, when choosing a 
reliable alternative source, the focus should be on measurement 
objectives, rather than on measurement technologies. In all cases, the 
user must demonstrate the method selected generates data that are 
appropriate for the intended use. Although both approaches are 
applicable for RCRA, ORCR had dropped the term PBMS, and strongly 
supports the use of the new Flexible Approach to be consistent with the 
Agency's new guidance that allows each program to determine program 
specific flexibility when addressing waste analysis issues.
    ORCR strongly recommends that persons use the latest version of a 
SW-846 method whenever possible, especially in new monitoring 
situations, since updated versions of the methods EPA publishes 
generally are in the Agency's view less subject to misinterpretation, 
yield improved precision and/or bias, or provide for the use of newer 
and, often, more cost-effective technologies. In situations where it 
may not be appropriate to use the latest method in SW-846, earlier 
versions may be used. These situations may include, but are not limited 
to, those where an earlier version of a method is required for existing 
permits, consent decrees, waste analysis plans or sampling analysis 
plans. In addition, laboratories, especially small laboratories, may 
find a previous version of a SW-846 method appropriate if it is more 
cost-effective in meeting the project-specific objectives. The Agency 
is not imposing restrictions on the use of earlier versions of non-
required methods contained in SW-846 or precluding the use of previous 
guidance. Nonetheless, the adoption of the latest method version is 
recommended and should be accomplished as soon as possible, as 
appropriate. When methods are employed, it is the responsibility of the 
user to ensure that the method yields data of a quality appropriate for 
the particular application for which it is being used.
    EPA views the methods in the SW-846 compendium as tools for the 
user to employ in developing individual standard operating procedures 
to meet the goals and objectives of specific projects. This approach 
enables the user to optimize and modify methods for effective 
performance on unique projects. The SW-846 methods are for most 
applications considered as guidance with the exception of those methods 
required by the RCRA regulations (i.e., Method-Defined Parameters 
(MDPs), see 40 CFR 260.11).
    In situations where the user is not certain whether the selected 
method or method modification is appropriate, EPA recommends regulated 
entities contact and seek approval as needed from the appropriate 
regulatory agency (e.g., Federal or State/local government) before 
applying any method on a specific project, including situations where 
the method is used verbatim.
    EPA may publish new methods, revise existing methods, or withdraw 
methods from the SW-846 compendium whenever it deems it appropriate. 
For example, methods may be updated in order to reflect new 
advancements in technology, to reflect the addition of new performance 
data, or to clarify areas of the procedure that experience indicates 
may be misunderstood. Methods may also be revised to reflect new EPA 
policy regarding the use of certain chemicals and reagents. In other 
cases, methods are removed if the technology is no longer available or 
applicable. ORCR has developed specific procedures for releasing 
updates, revisions, or withdrawing methods, which are designed to 
minimize disruption to regulatory processes. Specific definitions for 
the terms associated with a method's status, which support the change 
procedures, have been developed and provided below.
    The Agency will only post the most recent version of a final SW-846 
method on the ORCR Web page as part of the SW-846 methods compendium 
(www.epa.gov./epawaste/hazard/testmethods/index.htm). Prior versions of 
methods formerly contained in SW-846 and still considered appropriate 
for use will be available through a separate hyperlink in the future. 
EPA's objective is to identify and make available on the Agency's SW-
846 Web site the latest information regarding the methodologies that 
generate effective data at minimum costs in response to new 
technological or scientific advancements, while, at the same time, 
making available earlier versions for those situations where such 
methods may be needed or appropriate (e.g., to determine how a 
particular analysis had been performed, to determine how to comply with 
a specific permit requirement, etc.).
SW-846 Methods Status Definitions
    Analytical methods are officially made a part of the SW-846 manual 
through a rigorous process of technical evaluation both within the 
Agency and through external review. Methods are also revised as needed 
after a formal evaluation process by analytical experts (e.g., SW-846 
work and focus groups) and an announcement of method availability and 
request for public comment in the Federal Register as a Notice of 
Availability. During the method development/evaluation process, the 
methods go through various stages of review and revision. The methods 
are officially included as part of an update to the most current 
edition of SW-846 at the conclusion of this process.
    ORCR employs a specific naming convention (i.e., method number and 
letter suffix) when publishing methods. The naming convention is 
intended to minimize confusion within the user community regarding a 
method's developmental status. The method number designates the 
underlying technology (e.g., 8000 series methods designate 
determinative procedures for organic compounds). A revision to a method 
where the underlying technology does not change is indicated by 
continued use of the same method number and letter, but with a new 
issuance date. If the revision retains the underlying technology, but 
does not affect the precision and/or accuracy of the data, the revision 
is considered to be minor or nonsignificant and the method number and 
letter is not changed or sequenced.
    If, on the other hand, the revision retains the underlying 
technology, but changes the precision and/or accuracy of the data, the 
change is considered to be significant and is indicated by a subsequent 
letter suffix (e.g., changes from 8270C to 8270D) and a new issuance 
date. For example, if the quality control recommendations are changed 
in a manner that improves the bias or precision of the method, but does 
not change the underlying technology (e.g., a tightening of the 
calibration acceptance criteria), the method number stays the same, but 
the letter suffix is sequenced to the next letter. The differences 
between the

[[Page 63190]]

earlier and later versions of a method are detailed in the method 
summary section of the revised version regardless of the type of 
change.
    Examples of changes that may be considered minor or nonsignificant 
include, but are not limited to: Language added to a method to provide 
increased clarity or guidance; expansion of lists of acceptable 
instrumentation, applicability of the method to a matrix not previously 
referenced, adding new compounds to the list of applicable compounds, 
or changes to instrument specifications which do not result in an 
existing acceptable instrument being rendered unacceptable; or 
formatting and editorial changes that are designed to improve 
readability or correct spelling or grammatical errors.
    ORCR has defined a ``significant change'' as a change that results 
in improved analytical results (e.g., changes that result in reducing 
analytical bias or improving data precision). Examples of significant 
changes may include, but are not limited to: a change in the operating 
parameter which reduces analytical flexibility; a change in 
instrumentation specification which minimizes interference and/or 
optimizes instrument performance (if the use of such interference 
reduction technique or performance enhancement is required); a change 
in calibration guidance which results in more restrictive 
recommendations; a change that institutes tighter QC recommendations; 
or a change in the reagents that are required by the method.
    ORCR understands revisions are sometimes necessary to either 
enhance the performance of the method or to allow flexibilities due to 
the complexity of sample matrices. In situations where the user is not 
certain whether the selected method, method modification or 
modification to their plan is appropriate, EPA recommends the regulated 
community seek approval from the appropriate regulatory agency (e.g., 
Federal or State/local government, client) before their use of a 
revised method; amend their plan (e.g., Project Plan, Quality Assurance 
Project Plan (QAPP), Sampling and Analysis Plan (SAP), Standard 
Operating Procedure (SOP)); and properly document the change when 
reporting analytical results.
    The following method status definitions reflect the current method 
development process and have been developed to add clarity for the 
method users. ORCR uses these definitions and the terms may vary for 
other program offices.
    Final Method--A method that has been formally adopted into the most 
recent version of the SW-846 compendium. Before a method becomes final, 
the validated version would have been made available for public review 
and comment in a Notice of Availability (NOA) or a proposed rulemaking, 
as appropriate.
    Validated Method--A method that has undergone development and 
technical review by EPA, but has not been formally adopted into the SW-
846 method compendium and published through a Federal Register Notice. 
Since this review includes technical work group approval and/or inter-
laboratory validation, validated methods are included on the Agency Web 
site for evaluation and use by the public and as a means of soliciting 
comment from the broader scientific community. The public may use a 
validated method prior to its inclusion in the SW-846 compendium, 
provided that the users demonstrate that it generates data that are 
appropriate for the intended use.
    Revised Method--A method included in SW-846 that has been updated 
to reflect changes that may be editorial in nature and do not impact 
data or performance comparability, that broaden the method to introduce 
new technologies that may increase productivity, but do not change the 
fundamental technology, or that change the quality control requirements 
to increase bias or precision.
    The number of a method that has been revised does not change, but 
the method may receive a subsequent letter suffix. If the revision is a 
significant one (as defined above) then both the letter suffix and the 
issuance date are updated. If, on the other hand, the revision is 
editorial in nature, or consists of the addition of new performance 
data, then only the issuance date is changed. Previous versions are not 
precluded from being used provided that the users demonstrate that it 
generates data that are appropriate for the intended use.
    Draft Method--A new method that is being evaluated for possible 
inclusion into SW-846. It represents the latest innovative 
technological advancements in scientific methodology, but has not 
completed technical review by EPA nor been subject to notice and 
comment in the Federal Register.
    Superseded Method--A superseded method is an earlier version of an 
SW-846 method or other guidance that is no longer included in the SW-
846 compendium and has been replaced by a newer version. Revised 
versions of Superseded methods should be viewed as the preferred 
method. Methods in this category are removed from the compendium, but 
remain available on line and are not precluded for use where required 
for existing projects or where an adequate justification for use 
exists. The term ``Superseded'' is documented in the method title as 
listed on the EPA Web site for prior versions of final methods followed 
by the date it was superseded.
    Withdrawn Method--A method or other guidance that EPA strongly 
recommends not be used, (e.g., cyanide and sulfide reactivity guidance 
withdrawn, June 14, 2005). EPA has determined that such procedures or 
methods, for the use or technical objectives for which they were 
originally published, are technically inadequate and/or no longer meet 
such use or technical objectives. This does not mean, however, that 
there would be no situations under which the procedures or methods may 
be appropriate. In any situation in which a person may believe that the 
withdrawn method is appropriate, we strongly encourage consultation 
with applicable regulatory agencies at the state or federal level. The 
prospective user of the method will need to demonstrate the old method 
is, indeed, appropriate. Any use of these methods, without any such 
consultation and demonstration, will be done at the user's risk.
    The Agency understands that earlier versions of the SW-846 methods 
that aren't required may still be in use to meet project specific 
criteria (e.g., permits, sampling plans, Consent Decrees, etc.). 
Permits and other plans formally approved by regulatory authorities 
that specify the use of particular methods for required analysis 
continue in effect unless they are changed. However, the Agency 
encourages the regulated community to use the latest version of SW-846, 
when applicable. EPA will continue to update the Methods Status Table 
to inform the public as to the status of methods in SW-846 and the 
Policy Statement will be added to the SW-846 methods compendium when 
the Update V package is finalized.
    [end of policy statement]

B. Changes to Chapters One Through Five and QA/QC Guidance (Chapter One 
and Individual Methods) in SW-846

    In general, EPA's revisions to Chapters One through Five to EPA 
publication SW-846 reflects the new method style guide format and added 
all the Update V methods and new letters/version to the appropriate 
related method sections. Specifically:

[[Page 63191]]

     Chapter One of SW-846 was revised to make it more user 
friendly and to be more consistent with the Agency's official guidance 
on QA/QC implementation and procedures (e.g., Quality Assurance Project 
Plans (QAPPS), Data Quality Objectives (DQOs), and the Flexible 
Approach to Environmental Measurement).
     Chapter Two now includes a Table of Contents to make 
finding the information easier. In addition, a typographical error was 
found for bis(2-chloroisopropyl) ether and was corrected to bis(2-
chloro-1-methylethyl) ether in Tables 2-1, 2-4, 2-15, 2-22, and 2-34. 
Furthermore, Table 2-40(A) was revised to reflect the current sample 
preservation guidance for styrene and vinyl chloride in aqueous samples 
(i.e., deletion of previously recommended practice of collecting a 
second set of samples without acid preservatives and analyze 
immediately, if styrene and vinyl chloride are analytes of interest) 
and Table 2-40(B) was revised to include Mercury Speciation hold times 
in addition to totals.
     Chapter Three was revised so that the definition for 
instrument detection limit (IDL) is consistent with the revised methods 
6010D and 6020B. In addition, the term ``accuracy'' was replaced by 
``bias'' where appropriate; the definition for linear range was revised 
to be consistent with methods 6010D and 6020B; the definition of 
interference check sample (ICS) was replaced with the spectral 
interference check (SIC) solution to be consistent with methods 6010D 
and 6020B; and the definition of ``laboratory control sample'' was 
revised to recommend the use of a spiking solution from the same source 
as the calibration standards. Also, the collision/reaction cell 
technology was added to Sections 3.6 and 3.7 as an effective method for 
removing isobaric interferences when analyzing by ICP-MS and a minimum 
collection mass of 100 g was added to Table 3-2 for solid samples 
collected for sulfide analysis.
     Chapter Four (see Table 4-1) was reformatted and updated 
by removing the recommendation to collect a second set of samples 
without adding an acid preservative and analyze in a shorter time frame 
if vinyl chloride and styrene are analytes of concern for aqueous 
samples.
     Chapter 5 had no significant changes outside of general 
ones specified above (e.g., updated format changes and method reference 
to chapters).
    In addition, EPA is incorporating three new and revised QC features 
in Chapter One and the Update V methods, where appropriate, for RCRA 
compliance monitoring which warrant further discussion here. A summary 
of changes to chapters in SW-846 are provided in Appendix A of each 
chapter.
    The new and revised features that have been added to Chapter One 
(Quality Control) and individual methods (where appropriate) are:
     Lower Limit of Quantitation (LLOQ)--References to the 
Method Detection Limit (MDL) have been replaced with the LLOQ. It is 
recommended to establish the LLOQ as the lowest point of quantitation, 
which, in most cases, is the concentration of the lowest calibration 
standard in the calibration curve that has been adjusted for the 
preparation mass and/or volume. The LLOQ value is a function of both 
the analytical method and the sample being evaluated.
Why is MDL removed and replaced by LLOQ for SW-846?
    ORCR has removed references to the MDL procedure (i.e., 40 CFR 136, 
Appendix B) beginning with Update IV and from the revised and new 
Update V methods and has recommended establishing the LLOQ. We continue 
to refine the procedure for establishing the LLOQ. The refined 
procedure considers sample matrix effects; provides a provision to 
verify the reasonableness of the reported quantitation limit (QL); and 
recommends a frequency of LLOQ verification (found in Chapter One and 
each method) to be balanced between rigor and practicality. (Note: The 
agency understands that previous versions of methods published in SW-
846 may contain the MDL reference. However, as methods are updated, EPA 
will remove the reference to the MDL, and will remove the reference in 
older methods that have not yet been updated, as time and resources 
allow. Therefore, ORCR recommends that LLOQ be used, as appropriate, 
for the methods that have not yet been updated. See the Section 9.8 in 
Method 6020B for inorganic analytes and Section 9.7 in Method 8000 for 
organic analytes on LLOQ for further information on implementation.)
    ORCR understands that other EPA programs may continue to use MDLs 
to meet their program use and needs (e.g., the National Pollutant 
Discharge Elimination System (NPDES) permit program). However, ORCR has 
found that the procedure in 40 CFR 136, Appendix B, for the 
determination of MDLs, developed for the Clean Water Act (CWA) program 
uses a clean matrix (e.g., reagent water for preparing ``spiked'' 
samples, or samples with known constituent concentrations). Analytical 
laboratories often have difficulty demonstrating they can meet the MDL 
established using Part 136 when evaluating complex matrices, such as 
wastes. The procedure outlined in Part 136 is generally not suitable 
for RCRA wastes or materials because the MDL approach generally yields 
unrealistic and/or unachievable method detection limits for the complex 
matrices (e.g., soils, sludges, wipes, and spent materials) encountered 
under the RCRA program. The MDLs are normally calculated from analysis 
of a sample that does not cause matrix interferences (typically 
determined using spiked reagent water). However, most wastes evaluated 
for compliance with RCRA consist of complex matrices. The LLOQ 
considers the effect of sample matrix (e.g., components of a sample 
other than the analyte) by taking the sample through the entire 
analytical process, including sample preparation, clean up (to remove 
sample interferences), and determinative procedures. Also, if method 
users choose, the LLOQ sample can be included at the end of the run to 
see if it meets the established acceptance criteria. Lastly, results 
above the LLOQ are quantifiable within an acceptable precision and 
bias. Thus, the LLOQ approach better suits the needs of the RCRA 
program, because it provides reliable and defensible results, 
especially at the lower level of quantitation, and can be reported with 
a known level of confidence for the complex matrices being evaluated.
    SW-846 methods are being used by various programs in implementing 
various statutes, including RCRA, the Comprehensive Environmental 
Response, Compensation and Liability Act (CERCLA), the Toxic Substances 
Control Act (TSCA), and Homeland Security Presidential Directives, for 
waste and materials characterization, compliance testing, site/incident 
characterization and risk assessment for protection of human health and 
the environment, and better management and use of wastes and materials, 
for a wide range of difficult matrices. ORCR believes that the LLOQ 
approach is an important improvement, and supports the essential need 
to provide data that are verified to meet the precision and accuracy 
requirements of the Agency's program needs.
    Establishing LLOQ for Inorganic analytes: When performing methods 
for inorganic analyses, the LLOQ should be verified by the analysis of 
at least seven replicate samples (prepared in a clean matrix or control 
material) and spiked at the LLOQ and processed through all preparation 
and analysis steps of the method. The mean recovery and relative 
standard deviation (RSD) of these

[[Page 63192]]

samples provide an initial statement of precision and bias at the LLOQ. 
In most cases, the mean recovery should be 35% of the true 
value and the RSD should be <=20%. Ongoing LLOQ verification, at a 
minimum, is on a quarterly basis to validate quantitation capability at 
low analyte concentration levels. This verification may be accomplished 
either with clean control material (e.g., reagent water, method blanks, 
Ottawa sand, diatomaceous earth, etc.) or a representative sample 
matrix free of target compounds. Optimally, the LLOQ should be less 
than the desired regulatory action levels based on the stated project-
specific requirements. For more information, please see the individual 
methods (e.g., Methods 6010 and 6020) and Chapter One of SW-846.
    Establishing LLOQ for organic analytes: When performing methods for 
organic analyses, the LLOQ should be verified using either a clean 
control material (e.g., reagent water, method blanks, Ottawa sand, 
diatomaceous earth, etc.) or a representative sample matrix free of 
target compounds. Optimally, the LLOQ should be less than the desired 
regulatory action levels based on the stated project-specific 
requirements.
    For organic analyses, the acceptable recovery ranges of target 
analytes will vary more than for other types of analyses, such as 
inorganics. The recovery of target analytes in the LLOQ check sample 
should be within established limits, or other such project-required 
acceptance limits, for precision and bias to verify the data reporting 
limits. Until the laboratory has sufficient data to determine 
acceptance limits statistically, a limit of 20% +/- the Laboratory 
Control Sample (LCS) criteria may be used for the LLOQ acceptance 
criteria. This approach acknowledges the poorer overall response at the 
low end of the calibration curve. Historically based LLOQ acceptance 
criteria should be determined as soon as practical once sufficient data 
points have been acquired.
    In-house limits for bias (e.g., % Recovery) and precision (e.g., 
Relative Percent Difference, %RPD) of the LLOQ for a particular sample 
matrix may be calculated when sufficient data points exist. The 
laboratory should have a documented procedure for establishing its in-
house acceptance ranges. Sometimes the laboratory instrument and/or 
analyst performance vary or test samples cause problems with the 
detector (e.g., samples may have interferences; may clog the 
instruments cells, wall or tube; may cause contamination; etc.). 
Therefore, the limits of acceptance (for precision and bias) are 
established by a lab with sufficient data to demonstrate that they can 
report down to the LLOQ with a certain level of confidence. The 
acceptance limits (for precision and bias) for LLOQ may be established 
by the laboratory or at the project level through the data quality 
objectives in a quality assurance project plan. The frequency of the 
LLOQ check is not specified for organic analytes.

    Note:  The LLOQ check sample should be spiked with the analytes 
of interest at the predicted LLOQ concentration levels and carried 
through the same preparation and analysis procedures as 
environmental samples and other QC samples. For more information, 
please see individual methods (e.g., Method 8000) and Chapter One of 
SW-846.

How is LLOQ used?
    The RCRA program deals with complex wastes and materials that are 
managed or used in many different ways (e.g., landfilling, land 
application, incineration, recycling). The thresholds (e.g., action or 
remediation levels) for data users (e.g., engineers or risk assessors) 
to make their decisions, therefore, vary. Method users will need to 
properly plan their analytical strategy to ensure the LLOQs for 
targeted analytes are lower than the thresholds needed to generate data 
used to determine how waste or materials can be properly managed or 
used.
     Initial Demonstration of Performance (IDP)--The laboratory 
must make an initial demonstration of ability to generate results with 
acceptable accuracy and precision for each preparation and 
determinative method they perform. This demonstration should be 
performed prior to independently analyzing real sample matrices by each 
analytical method and should be repeated if other changes occur (e.g., 
significant change in procedure, new staff are trained, etc.). 
Documentation of the IDP should be maintained by the Quality Assurance 
Manager. Each laboratory should have a training program documenting 
that a new analyst is capable of performing the method or portion of 
the method for which the analyst is responsible. This demonstration 
should document that the new analyst is capable of successfully 
following the standard operating procedure (SOP) based on the 
laboratory's IDP policy.
    For Update V, changes to the IDP have been specified in the 
individual Update V methods where appropriate (e.g., screening method 
where there is not a quantitative reporting limit such as a bioassay 
method). The IDP changes allow laboratories to use their time and 
resources effectively, especially for the organic analyses.
    Key Changes in the IDP for the Determination of Organic Analytes:
    The IDP section was expanded to describe two situations:
    When a significant change to instrumentation or procedure occurs: 
Reliable performance of the methods is dependent on careful adherence 
to the instructions in the written method, and aspects of the method 
are mandatory to ensure that the method performs as intended. 
Therefore, if a major change to the sample preparation procedure is 
made (e.g., a change of solvent), the IDP must be repeated for that 
preparation procedure to demonstrate the laboratory technician's 
continued ability to reliably perform the method. EPA considers 
conducting IDPs as part of good laboratory practice procedures and has 
already included these procedures in EPA's laboratories practices.
    Alterations in instrumental procedures only (e.g., changing Gas 
Chromatograph (GC) temperature programs or High Performance Liquid 
Chromatography (HPLC) mobile phases or the detector interface), require 
a new calibration, but not a new IDP because the preparation procedure 
is unchanged.
    When new staff members are trained: A new analyst needs to be 
capable of performing the method, or portion of the method, for which 
the analyst is responsible. For example, when analysts are trained for 
a subset of analytes for an 8000 series method, the new sample 
preparation analyst should prepare reference samples for a 
representative set of analytes (e.g., the primary analyte mix for 
Method 8270, or a mix of Aroclor 1016 and 1260 for Method 8082) for 
each preparation method the analyst will be performing. The instrument 
analyst being trained will need to analyze prepared samples (e.g., 
semi-volatile extracts).
     Relative Standard Error (RSE)--ORCR evaluated and 
included, as the analytical community recommended, RSE as an option (in 
addition to calculation of the % error) in SW-846 for the determination 
of the acceptability for a linear or non-linear calibration curve. RSE 
refits the calibration data back to the calibration model and evaluates 
the difference between the measured and the true amounts or 
concentrations used to create the model.

[[Page 63193]]

[GRAPHIC] [TIFF OMITTED] TN23OC13.003

Where:

xi = True amount of analyte in calibration level i, in 
mass or concentration units.
x[acute]i = Measured amount of analyte in calibration 
level i, in mass or concentration units.
p = Number of terms in the fitting equation (average = 1, linear = 
2, quadratic = 3, cubic = 4).
n = Number of calibration points.

    The RSE acceptance limit criterion for the calibration model is the 
same as the RSD limit in the determinative method. If the RSD limit is 
not defined in the determinative method, the RSE limit should be set at 
<=20% for good performing compounds and <=30% for poor performing 
compounds.

V. Summary

    EPA believes that these changes in Update V will assist the method 
users to demonstrate method competency and generate better quality 
data. For the convenience of the analytical community, the Agency will 
revise the OSWER Methods' Team homepage on EPA's Web site with updated 
information to better communicate new policy and analytical procedures, 
and will include Update V and selected documents at that Web site after 
Update V is finalized.
    Please see the Web site: https://www.epa.gov/epawaste/hazard/testmethods/index.htm for more information. Table 1 provides a listing 
of the five chapters and twenty-three methods (eight new and fifteen 
revised methods) in Update V.

           Table 1--Update V (Methods, Chapters and Guidance)
------------------------------------------------------------------------
    Analytical method No.               Method or chapter title
------------------------------------------------------------------------
                               Table of Contents.
                               Chapter One--Quality Control.
                               Chapter Two--Choosing the Correct
                                Procedure.
                               Chapter Three--Inorganic Analytes.
                               Chapter Four--Organic Analytes.
                               Chapter Five--Miscellaneous Test Methods.
                               Methods Status Table.
1030.........................  Ignitability of Solids.
3200 *.......................  Mercury Species Fractionation and
                                Quantification by Microwave-Assisted
                                Extraction, Selective Solvent Extraction
                                and/or Solid Phase Extraction.
3511 *.......................  Organic Compounds in Water by
                                Microextraction.
3572 *.......................  Extraction of Wipe Samples for Chemical
                                Agents.
3620C........................  Florisil Cleanup.
4025 *.......................  Screening for Polychlorinated
                                Dibenzodioxins and Polychlorinated
                                Dibenzofurans (PCDD/Fs) by Immunoassay.
4430 *.......................  Screening for Polychlorinated Dibenzo-p-
                                Dioxins and Furans (PCDD/Fs) by Aryl
                                Hydrocarbon Receptor PCR Assay.
4435 *.......................  Method for Toxic Equivalent (TEQS)
                                Determination for Dioxin-Like Chemical
                                Activity With the CALUX[supreg]
                                Bioassay.
5021A........................  Volatile Organic Compounds in Various
                                Sample Matrices Using Equilibrium
                                Headspace Analysis.
6010D........................  Inductively Coupled Plasma-Atomic
                                Emission Spectrometry.
6020B........................  Inductively Coupled Plasma-Mass
                                Spectrometry.
6800.........................  Elemental and Speciated Isotope Dilution
                                Mass Spectrometry.
8000D........................  Determinative Chromatographic
                                Separations.
8021B........................  Aromatic and Halogenated Volatiles by Gas
                                Chromatography Using Photoionization and/
                                or Electrolytic Conductivity Detectors.
8111.........................  Haloethers by Gas Chromatography.
8270D........................  Semivolatile Organic Compounds by Gas
                                Chromatography/Mass Spectrometry.
8276 *.......................  Toxaphene and Toxaphene Congeners by Gas
                                Chromatography/Negative Ion Chemical
                                Ionization Mass Spectrometry (GC-NICI/
                                MS).
8410.........................  Gas Chromatography/Fourier Transform
                                Infrared Spectrometry for Semivolatile
                                Organics: Capillary Column.
8430.........................  Analysis of Bis (2-Chloroethyl) Ester and
                                Hydrolysis Products by Direct Aqueous
                                Injection.
9013A........................  Cyanide Extraction Procedure for Solids
                                and Oils.
9014.........................  Titrimetric and Manual Spectrophotometric
                                Determinative Methods for Cyanide.
9015 *.......................  Metal Cyanide Complexes by Anion Exchange
                                Chromatography and UV Detection.
9320.........................  Radium 228.
------------------------------------------------------------------------
* New Methods.


    Dated: September 27, 2013.
Barnes Johnson,
Acting Director, Office of Resource Conservation and Recovery.
[FR Doc. 2013-24852 Filed 10-22-13; 8:45 am]
BILLING CODE 6560-50-P