1
23 new and revised methods Revised Chapters 1, 2, 3, 4, and 5 NEW SW-846 Policy Statement Kim Kirkland USEPA Office of Resource Conservation and Recovery (703) 308-0490 [email protected] Shen-yi Yang USEPA Office of Resource Conservation and Recovery (703) 308-0437 [email protected] The Methods Information Communication Exchange ( MICE) Service provides a valuable service to the public by answering questions and taking comments regarding "Test Methods for Evaluating Solid Waste: Physical/Chemical Methods (SW-846)." The MICE Service is maintained by the EPA Office of Resource Conservation and Recovery and operated by TechLaw, Inc., utilizing chemists, sampling experts, and environmental scientists knowledgeable in SW-846 procedures. Here’s how to reach the MICE Service: E-mail: [email protected] Phone: (703) 818-3238 Fax: (703) 818-8813 1. Methods on New Methods webpage that have not been included in Updates V or VI. 2. Collaborate with USGS to develop new extraction procedure for hexavalent chromium. 3. Arsenic speciation – extraction and determinative methods developed by Region 10. 4. Address the Methods Users’ Request List. Examples include methods referencing mercury thermometers, Method 9040 (pH), other hazardous waste characteristics, and Method 3060A. 5. Collaborations with the American Council of Independent Laboratories (ACIL) work groups to improve timeliness regarding the issuance of methods. 6. Collaborations with EPA program offices and external partners for possible method and standard development. 7. Update of Methods 8330 (to refine analytical conditions and include degraded products) and 8261 (to update analytical conditions). 8. Update the SW-846 website to be more user-friendly, including the policy statement. 9. Ongoing updates of FAQs for MICE. Method 1340 In Vitro Bioaccessibility Assay for Lead in Soil New method to estimate in vivo bioavailability of lead in soil. Submitted by the Office of Superfund Remediation and Technology Innovation to assist in risk evaluations of sites contaminated with lead. Method 3050C Acid Digestion of Sediments, Sludges, and Soils Incorporates incremental sampling methodology for sample collection and laboratory preparation. Provides an alternative acid digestion procedure for tungsten. Replaces Method Detection Limit (MDL) with Lower Limit of Quantitation (LLOQ). Method 8260D Volatile Organic Compounds by Gas Chromatography/ Mass Spectrometry and Method 8270D Semivolatile Organic Compounds by Gas Chromatography/ Mass Spectrometry Add new analytes Include alternate carrier gas to helium Method 8270: advanced technology (MS/MS and Chemical Ionization) is considered for inclusion LEAF is a collaboration between: Vanderbilt University, Energy Research Centre of the Netherlands, DHI (Denmark), EPA Office of Research and Development, and EPA Office of Resource Conservation and Recovery. EPA has posted the following leaching tests on the New Methods page (http://www.epa.gov/osw/hazard/testmethods/sw846/new_meth.htm): Method 1313: Liquid-Solid Partitioning as a Function of Extract pH for Constituents in Solid Materials using a Parallel Batch Extraction Procedure Method 1314: Liquid-Solid Partitioning as a Function of Liquid-Solid Ratio for Constituents in Solid Materials using an Up-Flow Percolation Column Procedure Method 1315: Mass Transfer Rates of Constituents in Monolithic or Compacted Granular Materials using a Semi-Dynamic Tank Leaching Procedure Method 1316: Liquid-Solid Partitioning as a Function of Liquid-Solid Ratio for Constituents in Solid Materials using a Parallel Batch Extraction Procedure For more information, view the EPA’s report, Background Information for the Leaching Environmental Assessment Framework (LEAF) Test Methods http://nepis.epa.gov/Adobe/PDF/P1009TQ9.pdf Revised versions of heavily used methods: 6010D, 6020B, and 8000D Method 8276 - Toxaphene As recommended by the Office of Inspector General (OIG), the EPA Deputy Administrator directed development of a new analytical protocol for toxaphene degradation products. The Office of Resource Conservation and Recycling (ORCR) worked with the Office of Research and Development (ORD) and Region 4 to develop Method 8276. Method 8276 was validated for groundwater, soil, and sediment and posted for public comment and use in March 2010. The expanded Method 8276 (applicable for fish and biota) was posted on the SW-846 website in September 2012. Chapter One Rewritten to provide a road map for implementing quality systems to generate data of sufficient quality for their intended use Reflects the current quality assurance approach used by data users and decision-makers performing environmental work requiring government oversight General overview provided with specific references to important EPA guidance documents for details on implementing an effective quality assurance system Serves as a basis for new staff responsible for implementing and assessing data collection and generation activities SW-846 Policy Statement Application of Methods Innovation Rule (MIR) to SW-846 methods Method version naming convention Definitions All methods in Update V received the following updates: Revised Initial Demonstration of Proficiency (IDP) Replaced Method Detection Limit (MDL) with Lower Limit of Quantitation (LLOQ) Added Relative Standard Error (RSE) as an acceptable calibration model Number Method Title 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 Equivalents (TEQS) Determinations For Dioxin-Like Chemical Activity with the CALUX® 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) Ether 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 Federal Register Notice: August 2013 Estimated date for posting to SW-846 Online: December 2013

Federal Register Notice: August 2013 Method 1340 In Vitro ...nemc.us/docs/2013/presentations/-Poster-26.15-Dahl.pdf · 8276 Toxaphene and Toxaphene Congeners by Gas Chromatography/Negative

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Page 1: Federal Register Notice: August 2013 Method 1340 In Vitro ...nemc.us/docs/2013/presentations/-Poster-26.15-Dahl.pdf · 8276 Toxaphene and Toxaphene Congeners by Gas Chromatography/Negative

• 23 new and revised methods

• Revised Chapters 1, 2, 3, 4, and 5

• NEW SW-846 Policy Statement

Kim Kirkland

USEPA

Office of Resource Conservation and Recovery

(703) 308-0490

[email protected]

Shen-yi Yang

USEPA

Office of Resource Conservation and Recovery

(703) 308-0437

[email protected]

The Methods Information Communication Exchange (MICE) Service provides a valuable service to the public by answering questions and taking comments regarding "Test Methods for Evaluating Solid Waste: Physical/Chemical Methods (SW-846)." The MICE Service is maintained by the EPA Office of Resource Conservation and Recovery and operated by TechLaw, Inc., utilizing chemists, sampling experts, and environmental scientists knowledgeable in SW-846 procedures.

Here’s how to reach the MICE Service:

E-mail: [email protected]

Phone: (703) 818-3238

Fax: (703) 818-8813

1. Methods on New Methods webpage that have not been included in Updates V or VI.

2. Collaborate with USGS to develop new extraction procedure for hexavalent chromium.

3. Arsenic speciation – extraction and determinative methods developed by Region 10.

4. Address the Methods Users’ Request List. Examples include methods referencing mercury thermometers, Method 9040 (pH), other hazardous waste characteristics, and Method 3060A.

5. Collaborations with the American Council of Independent Laboratories (ACIL) work groups to improve timeliness regarding the issuance of methods.

6. Collaborations with EPA program offices and external partners for possible method and standard development.

7. Update of Methods 8330 (to refine analytical conditions and include degraded products) and 8261 (to update analytical conditions).

8. Update the SW-846 website to be more user-friendly, including the policy statement.

9. Ongoing updates of FAQs for MICE.

Method 1340 – In Vitro Bioaccessibility Assay for Lead in Soil

• New method to estimate in vivo bioavailability of lead in soil.

• Submitted by the Office of Superfund Remediation and Technology Innovation to assist in risk evaluations of sites contaminated with lead.

Method 3050C – Acid Digestion of Sediments, Sludges, and Soils

• Incorporates incremental sampling methodology for sample collection and laboratory preparation.

• Provides an alternative acid digestion procedure for tungsten.

• Replaces Method Detection Limit (MDL) with Lower Limit of Quantitation (LLOQ).

Method 8260D – Volatile Organic Compounds by Gas Chromatography/ Mass Spectrometry and

Method 8270D – Semivolatile Organic Compounds by Gas Chromatography/ Mass Spectrometry

• Add new analytes

• Include alternate carrier gas to helium

• Method 8270: advanced technology (MS/MS and Chemical Ionization) is considered for inclusion

LEAF is a collaboration between: Vanderbilt University, Energy Research Centre of the Netherlands, DHI (Denmark), EPA Office of Research and Development, and EPA Office of Resource Conservation and Recovery.

EPA has posted the following leaching tests on the New Methods page (http://www.epa.gov/osw/hazard/testmethods/sw846/new_meth.htm):

Method 1313: Liquid-Solid Partitioning as a Function of Extract pH for Constituents in Solid Materials using a Parallel Batch Extraction Procedure

Method 1314: Liquid-Solid Partitioning as a Function of Liquid-Solid Ratio for Constituents in Solid Materials using an Up-Flow Percolation Column Procedure

Method 1315: Mass Transfer Rates of Constituents in Monolithic or Compacted Granular Materials using a Semi-Dynamic Tank Leaching Procedure

Method 1316: Liquid-Solid Partitioning as a Function of Liquid-Solid Ratio for Constituents in Solid Materials using a Parallel Batch Extraction Procedure

For more information, view the EPA’s report, Background Information for the Leaching Environmental Assessment Framework (LEAF) Test Methods

http://nepis.epa.gov/Adobe/PDF/P1009TQ9.pdf

Revised versions of heavily used methods: 6010D, 6020B, and 8000D

Method 8276 - Toxaphene

• As recommended by the Office of Inspector General (OIG), the EPA Deputy Administrator directed development of a new analytical protocol for toxaphene degradation products.

• The Office of Resource Conservation and Recycling (ORCR) worked with the Office of Research and Development (ORD) and Region 4 to develop Method 8276.

• Method 8276 was validated for groundwater, soil, and sediment and posted for public comment and use in March 2010.

• The expanded Method 8276 (applicable for fish and biota) was posted on the SW-846 website in September 2012.

Chapter One

• Rewritten to provide a road map for implementing quality systems to generate data of sufficient quality for their intended use

• Reflects the current quality assurance approach used by data users and decision-makers performing environmental work requiring government oversight

• General overview provided with specific references to important EPA guidance documents for details on implementing an effective quality assurance system

• Serves as a basis for new staff responsible for implementing and assessing data collection and generation activities

SW-846 Policy Statement

• Application of Methods Innovation Rule (MIR) to SW-846 methods

• Method version naming convention

• Definitions

All methods in Update V received the following updates:

• Revised Initial Demonstration of Proficiency (IDP)

• Replaced Method Detection Limit (MDL) with Lower Limit of Quantitation (LLOQ)

• Added Relative Standard Error (RSE) as an acceptable calibration model

Number Method Title

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 Equivalents (TEQS) Determinations For Dioxin-Like Chemical Activity with the CALUX® 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) Ether 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

Federal Register Notice: August 2013Estimated date for posting to SW-846 Online: December 2013