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 (mice@techlawinc.com)

mailto:mice@techlawinc.com

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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: mice@techlawinc.com

Kim Kirkland

Phone: (703) 308-0490

E-mail: kirkland.kim@epa.gov

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mailto:mice@cpmx.saic.com