an update on sw-846 · analysis of bis (2-cloroethyl) ester ... 6010 6010a -- 6010b (up. iii) ......
TRANSCRIPT
USEPA ORCR
Materials & Recovery Waste Management Division March 20, 2013
An Update on SW-846
Office of Resource
Conservation and Recovery (ORCR)
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Provide brief history about SW-846 and the issuance of methods
Provide info on the Status of Update V
Update V
ORCR Policy statement
Other Key Features
Schedule
Provide Information Regarding New Projects and Collaboration for the ORCR Methods Team
Other Resources
Purpose of this Update
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History of the SW-846 Methods Compendium
An analytical methods manual containing 200+ methods and 13 chapters designed for testing and monitoring under the Resource Conservation and Recovery Act (RCRA) Program
Methods are considered appropriate and reliable for the complexity of RCRA waste matrices
New methods incorporated through a lengthy validation approval process: Comprehensive technical evaluation Agency review
Existing methods are also updated, as needed Following a formal evaluation process by analytical experts
(e.g., SW-846 work, focus groups, internal EPA review) and an announcement of method availability and request for public comment in the Federal Register as a Notice of Data Availability (NODA)
Background
Methods Innovation Rule (MIR) [June 14, 2005 (70 FR 34537)]
Removed the required use of SW-846 and provides flexibility in choice of methods for wastes regulated or managed under RCRA
Exception only for method-defined parameters (MDPs) (see 40 CFR 260.11)
Formal rulemaking no longer required for publication of updates to SW-846 method Updates are made available through Notice of Data Availability (NODA)
A Summary table at the end of the method provides for significant revisions
PBMS/Performance Approach Method users have the flexibility to employ an SW-846 method or “any
appropriate method” from a reliable source When using an alternative method, the focus should be on measurement
objectives, rather than on measurement technologies Demonstration of performance is important Strongly promoted by ORCR
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ORCR will adopt 23 additional methods to the SW-846 compendium
Final Update V
1030 Ignitability of Solids
3200 Mercury Species Fractionation and Quantification By Microwave Assisted Extractions, Selective Solvent Extraction and/or Solid Phase Extraction
3511 Organic Compounds in Water By Mircroextraction
3572 Extraction of Chemical Agents from Wipe Samples Using Microextraction
3620C Florisil Cleanup
4025 Screening for Polychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans (PCDD/PCDFs) By Immunoassay
4430 Screening for Polychlorinated Dibenzo-p-Dioxins (PCDDs) And Polychlorinated Dibenzofurans (PCDFs) In Soils and Sediments Using an Aryl Hydrocarbon Receptor-based PCR Assay
4435 Screening for Dioxin-Like Chemical Activity in Soils and Sediments Using The Calux® Bioassay and TEQ Determinations
5021A Volatile Organic Compounds In Various Sample Matrices Using Equilibrium Headspace Analyses
6010D Inductively Coupled Plasma-Atomic Emission Spectrometry
6020B Inductively Coupled Plasma-Atomic Emission 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/Negative Ion Chemical Ionization mass Spectrometry (GC-NICI/MS)
8276 Toxaphene and Toxaphene Congeners by Gas Chromatography/Negative Ion Chemical Ionization Mass Spectrometry (GC-NICI-/MS)
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Final Update V List Cont.
8410 Gas Chromatography/Fourier Transform Infrared Spectrometry for Semivolatile Organics: Capillary Column
8430 Analysis of Bis(2-cloroethyl) Ester and Hydrolysis Products by Direct Aqueous Injection
9013A Cyanide Extraction Procedure for Solids and Oils
9014 Titrimetric and Manual Spectrophotometer Determinative Methods for Cyanide
9015 Metal Cyanide Complexes by Anion Exchange Chromatography and UV Detection
9320 Radium 228
Chapter 1 Quality Control
Chapter 2 Choosing the Correct Procedure
Chapter 3 Inorganic Analysis
Chapter 4 Organic Analysis
Chapter 5 Miscellaneous Test Methods
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Use of SW-846
Methods Compendium
3 Parts:
Background
General guidance on procedures for adopting methods into SW-846
Summary of definitions and terms
USEPA ORCR Policy Statement
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Summary of Definition and Terms
Terms regarding the use of methods that have been adopted in SW-846:
Final
Validated
Revised
Draft
Superseded
Withdrawn
Significant change
Key Features in SW-846
Chapter One – Chapter One has been revised to be more consistent with the Agency’s official guidance on QA/QC implementation and procedures.
IDP – The initial demonstration of proficiency is conducted by the lab technician to generate acceptable accuracy and precision for each preparation and determinative method performed by the laboratory. 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., instrument repair, significant change in procedure, etc.).
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New Information Cont.
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Lower limit of quantitation (LLOQ) - 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.
RSE – Relative Standard Error is a model used to demonstrate calibration acceptability, whereby the measured concentration for each point in the calibration curve are compared to the expected (true) values using a % error calculation. This approach indicates the drift of the individual points for each compound, rather than just the overall goodness of fit expressed by R squared.
Update V Schedule
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Action Item Tentative Schedule
Management Reviews of the Notice
and Communication Documents
Jan 14th – Feb 28rd
OGC Review and Concurrence Mar 14th – Mar 22nd
PARMS Review Mar1 4th - Mar 22nd
Revise Package Mar 25nd – Mar 29th
Notice to EPA Program Offices for
concurrence
Apr 1st – Apr 19th
Brief MRWMD DD and others Week of April 22nd
Briefing ORCR DD Week of April 29th
Signed Package Week of May 13th
Prep package for review and
Publication
May
Communication Docs released May
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Resources
Methods Information Communication Exchange
MICE was created by the Methods Team and is operated ORCR’s contractor (e.g., chemists, sampling experts, and environmentalists) who are knowledgeable in SW-846 technical and RCRA-related monitoring procedures.
How Does the MICE Service Work? Persons interested in contacting the MICE Service by telephone may call a voice-mail answering service at 703-818-3238 that is available 24-hours a day, 7-days a week. The caller can listen also to several recorded messages on common SW-846 topics and leave a message containing a question or comment.
Where to order copies of SW-846.
Where to find information on sample holding times, preservation, and storage.
The availability of SW-846 methods under development and other EPA methods.
Information on RCRA characteristics testing.
Solid waste sampling.
Questions and comments also can be submitted to the MICE Service via telefacsimile (fax, 703-818-8813) or e-mail ([email protected])
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Additional Resources Status Table
METHOD NUMBER
(Date in parenthesis is found at bottom right-hand corner of method)
METHOD TITLE THIRD ED
(9/86)
FIN. UP.
I
(7/92)
FIN. UP.
II (9/94)
IIA
(8/93)
IIB
(1/95)
FIN. UP.
III (12/96)
IIIA (4/98)
IIIB (11/04)
FIN.
UP.
IV
(2/07)
OTHER
METHODS
(VARIOUS
DATES)
Validate
Methods
Final
Up. V
(10/12)
6010 6010A -- 6010B (Up. III) 6010C -- 6010D Inductively Coupled Plasma-Atomic Emission
Spectrometry
-- -- 6020 (Up. II) -- 6020A -- 6020B Inductively Coupled Plasma-Mass Spectrometry
-- -- -- -- -- 3200
(7/05)
3200 Mercury Species Fractionation and Quantification By
Microwave Assisted Extractions, Selective Solvent
Extraction and/or Solid Phase Extraction
-- -- -- -- --
3511
(11/02)
3511A Organic Compounds in Water by Microextraction
-- -- -- -- -- 3572
(7/07) 3572 Extraction of Chemical Agents from Wipe Samples Using
Microextraction
-- -- -- --
6800 --
6800 Elemental and Speciated Isotope Dilution Mass
Spectrometry
8000 8000A --
8000B
(11/04)
--
8000C
(03/03)
8000D Determinative Chromatographic Separations
Update VI and Collaborations Update VI Methods
1340 Standard Operating Procedure for An In-Vitro Bioaccessibility Assay For Lead
in Soil
3050 Acid Digestion of Sediments, Sludges, and Soils
6850 Perchlorate in Water, Soils and Solid Wastes Using High Performance Liquid Chromatography/Electrospray Ionization/Mass Spectrometry
6860 Perchlorate in Water, Soils and Solid Wastes Using Ion Chromatography/Electrospray Ionization/Mass Spectrometry
8260 Volatile Organic Compounds By Gas Chromatography/Mass Spectrometry (GC/MS)
8261 Volatile Organic Compounds By Vacuum Distillation In Combination With Gas Chromatography/Mass SPECTROMETRY (VD/GC/MS)
8270 Semivolatile Organic Compounds By Gas Chromatography/Mass Spectrometry (GC/MS)
8330 Nitroaromatics, Nitramines, and Nitrate Esters By High Performance Liquid Chromatography (HPLC)
Workgroups Forum Environmental Monitoring (FEM), Independent Laboratory Institute
meeting group, Inside and Outside Stakeholders and commercial labs
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Collaborations Cont.
Collaborations Posting Methods 1313, 1314, 1315, and 1316 (LEAF test methods – leaching
procedures) on the SW-846 website.
Collaborating with USGS on a new hexavalent chromium extraction and evaluating the Regional hexavalent chromium holding time study.
Discussing the helium shortage supply impacting analysis of semivolatile and volatile organics with EPA program offices and interested parties.
Collaborate with OST, instrument vendors and analytical community, to design a study plan validating an extraction procedure for the analysis of semivolatiles to be used for CWA program.
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Relevant Contact Information THANKS!!!
Methods Team Home Page: www.epa.gov/SW-846
MICE
Phone: (703) 818-3238
E-mail: [email protected]
Kim Kirkland
Phone: (703) 308-0490
E-mail: [email protected]
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