United States Solid Waste and EPASW-846.3-3a
Environmental Protection Emergency Response March 1999
Agency (5305W) www.epa.gov/osw
Test Methods for
Evaluating Solid
Waste: Physical/
Chemical Methods;
Third Edition; Final
Update III-A
Printed on paper that contains at lest 20 percent postconsumer fiber
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FINAL UPDATE IIIA
Cover Sheet
THIS PACKET CONTMNS NEW AND REVISED MATERIAL
FOR INCLUSION IN:
TEST METHODS FOR EVALUATING SOLID WASTE
PHYSICAL/CHEMICAL METHODS
(SW-846) THIRD EDITION
Contents:
1. Cover sheet. (What you are currently reading)
2. Instructions. Read this section! It explains how Update IIIA relates to
the rest of your SW-846.
3. Update IPA Table of Contents. The Table of Contents (dated April 1998)
lists all of the methods [Third Edition, Updates I, II, IIA, IIB, III, and
IIIA) in the order of appearance in the manual.
4. Revised Chapter Five
5. Referral to Office of Water Method 1664. as replacement to Method 9070
i , . . . . . -
5. Method 9071B
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:[NSTRUCTIONS
SW-846, a methods manual, is a "living" document that changes when new data and
advances in analytical techniques are incorporated! into the manual as new or revised
methods. To date, the Agency has formally issued Final Updates I, II, IIA, IBB, and
III. This package contains Final Update III A. For specific and important
information regarding this update, please read the section below entitled "About
Final Update IHA."
These instructions describe how to get your basic manual up-to-date and what to do
with your Final Update IIIA package. Additional updates will be released by the
Agency hi the future. New instructions, to supersede these, will be included with
each of those new update releases. A number of SW-846 update packages have been
released to the public since the original Third Edition was released. The dates and
labels on these packages can be confusing. In general, final updates should always
be incorporated into SW-846 in chronological order (e.g. Update I should be
incorporated before Update II).
The following definitions are provided to you as a guide:
New subscribers are defined as individuals who have recently (6-8 weeks)
placed an order with the GPO and have received new copies of the 4 (four)
volume set of the Third 'Edition, a copy of Final Update I, a copy of Final
Update n/BLA, a copy of Final Update HE, a copy of Final Update III, a copy
of Draft Update IVA, and a copy of Final Update IIIA.
Previous subscribers are defined as individuals that have received copies of
the Third Edition and other SW-846 Updates (including proposed Updates)
hi the past and have just received their Final Update IIIA package in the mail.
Instructions - 1 Final Update IIIA
April 1998
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A?f»TTT FTNAT TTPTWTK TTTA
As of Update m to SW-846, the two SW-846 methods for determination of oil and grease
were Method 9070 for waters and aqueous wastes, and Method 9071A for solid and semi-solid
materials such as soil, sediment, and sludge. Method 9070 was virtually identical to Office of
Water methods for determination of oil and grease; and Method 9071 A employed drying of the
sample with magnesium sulfate and using Soxhlet extraction for the determination. Both methods
used l,l,2-tricnloro-l,2,2-trifluoroethane (CFC-113; Freon-113) as the extraction solvent in the
testing of samples for oil and grease levels.
The Agency recently published a final rule in the Federal Register which finalized Office
of Water Method 1664, Revision A, and SW-846 Method 9071B and withdrew previously
approved methods (including certain Office of Water methods and SW-846 Method 9070) for the
determination of oil and grease and non-polar material (NPM) in EPA's wastewater and hazardous
waste programs. These changes were made as a part of EPA's effort to reduce dependency on
the use of chlorofluorocarbons (CFCs) in order to protect Earth's ozone layer and to meet the CFC
phaseout agreed to in the Montreal Protocol and required by the Clean Air Act Amendments of
1990. Method 1664 now uses normal hexane (n-hexane) as the extraction solvent in place of
l,l,2-trichloro-l,2,2-trifluoroethane (CFC-113; Freon-113), a Class 1 CFC.
As part of that final rule, SW-846 was amended to delete Method 9070 and to include
revised Method 9071B as Final Update mA to the manual. Specifically, Method 9071B addresses
the use of n-hexane instead of CFC-113 as the extraction solvent, in a manner consistent with the
use of n-hexane in Method 1664. In addition, in place of Method 9070, which used CFC-1 13 as
the extraction solvent in the testing of waters and aqueous wastes, the Agency incorporated by
reference Method 1664 in the RCRA regulations. As part of Final Update mA, SW-846 refers
the regulated community to Method 1664 for testing previously conducted using Method 9070.
The' publication number for Method 1664 is EPA-821-R-98-002.
Final Update IKA has been issued by the EPA's Office of Solid Waste and contains
documents which have been promulgated for inclusion in the SW-846. methods manual. The Final
Update mA package includes one revised method (Method 9071B), one revised chapter (Chapter
Five), a page to replace Method 9070, and a revised Table of Contents. Method 9070 needs to
be removed from the manual when Final Update mA is incorporated.
FTNAL TTPDATE TTIA-
The following is a brief summary of what new subscribers and previous subscribers should
do upon receipt of the Update IDA package:
j
NEW SUBSCRIBERS - If you are a new subscriber, you should perform the following tasks
before addressing your new Update DIA:
Instructions - 2 Final Update
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• Place the original Third Edition of SW-846 (September 1986) in the properly labeled four
3-ring notebooks according to the instructions in Final Update III.
• Incorporate Final Update I (July 1992) into the manual according to the instructions in
Final Update m.
• Incorporate Final Updates H (September 1994) and HA (August 1993) into the manual
according to the instructions in Final Update HI.
• Incorporate Final Update HE (January 1995) into the manual according to the instructions
in Final Update m.
• Incorporate Final Update El (December 1996) into the manual according to its
instructions.
• Either incorporate Draft Update IVA in the manual (without removing any white pages),
or keep the colored draft update in a separate binder of your choice.
Finally, incorporate Final Update IQA. Final Update IIIA is printed on white paper and has the
date of "April 1998" in the lower right hand corner of each page. This package contains revised
material for SW-846, specifically a revised Table of Contents, Chapter Five, and Method 9071B.
In addition, it contains a page that should be used to replace Method 9070. Remove Method 9070
from the manual. This method has been deleted from SW-846 as part of Final Update IIIA.
Then, use the Table of Contents dated April 1998 to determine the correct location for each
document in the Final Update IDA package.'
PREVIOUS SUBSCRIBERS - If you are a previous subscriber, it is important to establish
exactly what is currently contained in your manual before addressing Final Update IIIA. If your
manual is properly updated, the ONLY white pages in the document should be dated September
'1986 (Third Edition), July 1992 (Final Update I), August 1993 (Final Update IIA), September
1994 (Final Update JJ), January 1995 ([Final Update IIB), and December 1996 (Final Update III).
Remove (and recycle or archive) any white pages from your manual that have any other dates.
There may also be colored pages (e.g., pink pages for Proposed Update III) inserted in the
manual. Remove all yellow, blue, green, or pink pages from the manual. These colored pages
represent proposed versions of methods and chapters that have since been finalized. (Some
individuals may chose to,keep their copies of colored versions in separate binders.) You may keep
your Draft Update IVA pages in the manual if you wish -- that update has not yet been finalized.
Follow the last paragraph in the instructions for new subscribers to determine how to incorporate
Final Update IIIA. The table below can be used as an aide to determine what should be in your
manual.
Instructions - 3 Final Update IIIA
April 1998
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UPDATE HISTORY OF SW-846
The table below can be used as an aid to understanding the update history of SW-846, Third
Edition. Finalized updates are printed in bold and underlined.
Package
Third Edition
Proposed Update I
Final Update I
(Released by accident)
Proposed Update n
(Released by accident)
Final Update I
Proposed Update n
Proposed Update HA
(Method 4010, available
from EPA by request.)
Final Update TTA
(Method 4010, included
with Final Update H.)
Final Update II
Final Update ITB*
Proposed Update HI
Final Undate ITT
Draft Update IVA
FJnaLUodate niA**
Date
September 1986
December 1987
November 1990
November 1990
July 1992
November 1992
October 1992
August 1993
September 1994
January 1995
January 1995
December 1996
January 1998
April 1998
Paper Color
White
Green
White
Blue
White
Yellow
White
White
White
White
Pink
White
Salmon
White
Status of Package
Finalized (Promulgated)
Obsolete
Obsolete! Never formally
finalized.
Obsolete! Never formally
proposed.
Finalized (Promulgated)
Obsolete
Obsolete
Finalized (Promulgated)
Finalized (Promulgated)
Finalized (Promulgated)
Proposed
Finalize*] (Promulgated)
Draft
Finalized (Promulgated)
* Contains only a revised Table of Contents, a revised Chapter Six,, and revised Methods
9040B and 9045C
** Contains only a revised Table of Contents, a revised Chapter Five, a page to replace
Method 9070, and revised Method 9071B.
Instructions - 4
Final Update fflA
April 1998
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ASSISTANCE
After reading these instructions, if you need help due to difficulties understanding the status of the
package, need assistance in obtaining Method 1664, or have technical questions regarding the
methods, you may telephone the Methods Information Communication Exchange (MICE) at
703-821-4690 or send an E-mail to: mice@lan828.ehsg.saic.com.
If you have questions concerning your SW-846 U.S. Government Printing Office (GPO)
subscription, you should telephone the GPO at 202-512-1806. If you did not purchase your SW-
846 from the GPO, the GPO will not be able to help you.
SW-846 AVAILABILITY ON CD-ROM
A CD-ROM version (Version 2.0) of Test Methods for Evaluating Solid Waste, Physical/Chemical
Methods (SW-846) has been developed by EPA in cooperation with the National Technical
Information Service (NTTS). On a single disc, it includes all text and figures found in the final
version of SW-846 as updated by Updates I, n, HA, HB, and ffl. (It does not include Final
Update HIA. This update may be included in a future revision to the CD.) It can be used for
word searching (e.g, analytes, keywords); and to cut and paste or export text and diagrams to
update or develop laboratory standard operating procedures (SOPs). To order by phone, call
NTIS at (800) 553-6847 and request order number PB97-501928GEI for a single user copy, PB97-
502512GEI for a 5-user LAN copy, or PB97-502520GEI for unlimited users. To receive
information by fax from NTIS about this CD-ROM, call (703) 365-0759 and enter publication
number code 8698.
A CD-ROM version of Draft Update TV on CD-ROM is planned for the future. To place an early
order by phone, call NTIS at (800) 553-6847 and request order number PB97-501936GEI (single
user), PB97-502538GEI (5-user LAN), or PB97-502546GEI (unlimited users)..
Instructions - 5 Final Update HIA
April 1998
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TABLE OF CONTENTS
VOLUME ONE
SECTION A
DISCLAIMER
ABSTRACT
TABLE OF CONTENTS
METHOD INDEX AND CONVERSION TABLE
PREFACE
ACKNOWLEDGEMENTS
PART I METHODS FOR ANALYTES AND PROPERTIES
CHAPTER ONE - QUALITY CONTROL j
1.0 Introduction
2.0 QA Project Plan
3.0 Field Operations
4.0 Laboratory Operations
5.0 Definitions
6.0 References
CHAPTER TWO - CHOOSING THE CORRECT PROCEDURE
2.1 Purpose
2.2 Required Information
2.3 Implementing the Guidance ' - '
2.4 Characteristics
2.5 Ground Water ',
2.6 References
CHAPTER THREE - INORGANIC ANALYTES
3.1 Sampling Considerations
3.2 Sample Preparation Methods
Method 3005A: Acid Digestion of Waters for Total Recoverable or Dissolved Metals
for Analysis by FLAA or ICP Spectroscopy
Method 301OA: Acid Digestion of Aqueous Samples and Extracts for Total Metals for
Analysis by FLAA or ICP Spectroscopy
Method 3015: Microwave Assisted Acid Digestion of Aqueous Samples and Extracts
CONTENTS - 1 Revision 5
April 1998
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Method 3020A:
Method 3031:
Method 3040A:
Method 3050B:
Method 3051:
Method 3052:
Method 3060A:
Acid Digestion of Aqueous Samples and Extracts for Total Metals for
Analysis by GFAA Spectroscopy
Acid Digestion of Oils for Metals Analysis by Atomic Absorption or
ICP Spectrometry
Dissolution Procedure for Oils, Greases, or Waxes
Acid Digestion of Sediments, Sludges, and Soils
Microwave Assisted Acid Digestion of Sediments, Sludges, Soils, and
Oils
Microwave Assisted Acid Digestion of Siliceous and Organically
Based Matrices
Alkaline Digestion for Hexavalent Chromium
3.3 Methods for Determination of Inorganic Analytes
... i • '''",'' '• ! ' • !
Method 601 OB: Inductively Coupled Plasma-Atomic Emission Spectrometry
Method 6020: Inductively Coupled Plasma-Mass Spectrometry
Method 7000A: Atomic Absorption Methods
Method 7020: Aluminum (Atomic Absorption, Direct Aspiration)
Method 7040: Antimony (Atomic Absorption, Direct Aspiration)
Method 7041: Antimony (Atomic Absorption, Furnace Technique)
Method 7060A: Arsenic (Atomic Absorption, Furnace Technique)
Method 7061A: Arsenic (Atomic Absorption, Gaseous Hydride)
Method 7062: Antimony and Arsenic (Atomic Absorption, Borohyclride Reduction)
Method 7063: Arsenic in Aqueous Samples and Extracts by Anodic Stripping
Voltammetry (ASV)
Method 7080A: Barium (Atomic Absorption, Direct Aspiration)
Method 7Q81: Barium (Atomic Absorption, Furnace Technique)
Method 7090: Beryllium (Atomic Absorption, Direct Aspiration)
Method 7091: Beryllium (Atomic Absorption, Furnace Technique)
Method 7130: Cadmium (Atomic Absorption, Direct Aspiration)
Method" 7131 A: Cadmium (Atomic Absorption, Furnace Technique)
Method 7140: Calcium (Atomic Absorption, Direct Aspiration)
Method 7190: Chromium (Atomic Absorption, Direct Aspiration)
Method 7191: Chromium (Atomic Absorption, Furnace Technique)
Method 7195: Chromium, Hexavalent (Coprecipltation)
Mejhod 7196A: Chromium, Hexavalent (Colorimetric)
Method 7197: Chromium, Hexavalent (Chelatiori/Extraction)
Method 7198: Chromium, Hexavalent (Differential Pulse Polarography)
Method 7199: Determination of Hexavalent Chromium in Drinking Water,
; Groundwater and Industrial Wastewater Effluents by Ion
Chromatography
Method 7200: Cobalt (Atomic Absorption, Direct Aspiration)
Method 7201: Cobalt (Atomic Absorption, Furnace Technique)
Method 7210: Copper (Atomic Absorption, Direct Aspiration)
Method 7211: Copper (Atomic Absorption, Furnace Technique)
Method 7380: Iron (Atomic Absorption, Direct Aspiration)
Method 7381: Iron (Atomic Absorption, Furnace Technique)
Method 7420: Lead (Atomic Absorption, Direct Aspiration)
Method 7421: Lead (Atomic Absorption, Furnace Technique)
Method 7430: Lithium (Atomic Absorption, Direct Aspiration)
CONTENTS - 2
Revision 5
April 1998
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Method 7450:
Method 7460:
Method 7461:
Method 7470A:
Method 7471A:
Method 7472:
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
Method
7480:
7481:
7520:
7521:
7550:
7580:
7610:
7740:
7741A:
7742:
7760A:
7761:
7770:
7780:
7840:
7841:
7870:
7910:
7911:
7950:
7951:
Magnesium (Atomic Absorption, Direct Aspiration)
Manganese (Atomic Absorption, Direct Aspiration)
Manganese (Atomic Absorption, Furnace Technique)
Mercury in Liquid Waste (Manual Cold-Vapor Technique)
Mercury in Solid or Semisolid Waste (Manual Cold-Vapor Technique)
Mercury in Aqueous Samples and Extracts by Anodic Stripping
Voltammetry (ASV)
Molybdenum (Atomic Absorption, Direct Aspiration)
Molybdenum (Atomic Absorption, Furnace Technique)
Nickel (Atomic Absorption, Direct Aspiration)
Nickel (Atomic Absorption, Furnace Method)
Osmium (Atomic Absorption, Direct Aspiration)
White Phosphorus (P4) ; by Solvent Extraction and Gas
Chromatography
Potassium (Atomic Absorption, Direct Aspiration)
Selenium (Atomic Absorption, Furnace Technique)
Selenium (Atomic Absorption, Gaseous Hydride)
Selenium (Atomic Absorption, Borohydride Reduction)
Silver (Atomic Absorption, Direct Aspiration)
Silver (Atomic Absorption, Furnace Technique)
Sodium (Atomic Absorption, Direct Aspiration)
Strontium (Atomic Absorption, Direct Aspiration)
Thallium (Atomic Absorption, Direct Aspiration)
Thallium (Atomic Absorption, Furnace Technique)
fin (Atomic Absorption, Direct Aspiration)
Vanadium (Atomic Absorption, Direct Aspiration)
Vanadium (Atomic Absorption, Furnace Technique)
Zinc (Atomic Absorption, Direct Aspiration)
Zinc (Atomic Absorption, Furnace Technique)
APPENDIX - COMPANY REFERENCES
NQTE: A suffix of "A" in the method number indicates revision one (the method has
been revised once). A suffix of "B" in the method number indicates revision two (the
method has been revised twice). A suffix of "C" in the method number indicates
revision three (the method has been revised three times). In order to properly
document the method used for analysis, the entire method number including the
suffix letter designation (e.g., A, B, or C) must be identified by the analyst. A
method reference found within the RCRA regulations and the text of SW-846 methods
and chapters refers to the latest promulgated revision of the method, even though the
method number does not include the appropriate letter suffix.
CONTENTS - 3
Revision 5
April 1998
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VOLUME ONE
SECTION B
DISCLAIMER
ABSTRACT
TABLE OF CONTENTS
METHOD INPEX AND CONVERSION TABLE
PREFACE
ACKNOWLEDGEMENTS
CHAPTER ONE. REPRINTED - QUALITY CONTROL
1.0 Introduction
2.0 QA Project Plan
3.0 Field Operations
4.0 Laboratory Operations
5.0 Definitions \
6.0 References
CHAPTER FOUR - ORGANIC ANALYTES
4.1 Sampling Considerations
4.2 Sample Preparation Methods
| j 'I,
4.2.1 Extractions and Preparations
Method 3500B: Organic Extraction and Sample Preparation
Method 351OC: Separatory Funnel Liquid-Liquid Extraction
Method 3520C: Continuous Liquid-Liquid Extraction
Method 3535: Solid-Phase Extraction (SPE)
Method 3540C: Soxhlet Extraction
Method 3541: Automated Soxhlet Extraction
Method 3542: Extraction of Semivolatile Analytes Collected Using Method 0010
(Modified Method 5 Sampling train)
Method 3545: Pressurized F-luid Extraction (PFE)
Method 3550B: Ultrasonic Extraction
Method 3560: Supercritical Fluid Extraction of Total Recoverable Petroleum
Hydrocarbons
Method 3561: Supercritical Fluid Extraction of Polynuclear Aromatic Hydrocarbons
MethodI 3580A: Waste Dilution
Method 3585: Waste Dilution for Volatile Organics
Method 5000: Sample Preparation for Volatile Organic Compounds
Method 5021: Volatile Organic Compounds in Soils and Other Solid Matrices Using
Equilibrium Headspace Analysis
Method 5030B: Purge-and-Trap for Aqueous Samples
CONTENTS-4 Revisions
April 1998
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Method 5031:
Method 5032:
Method 5035:
Method 5041A:
Volatile, Nonpurgeable, Water-Soluble Compounds by Azeotropjc
Distillation
Volatile Organic Compounds by Vacuum Distillation
Closed-System Purge-and-Trap and Extraction for Volatile Organics
in Soil and Waste Samples
Analysis for Desorption of St>rbent Cartridges from Volatile Organic
Sampling Train (VQST)
4.2.2 Cleanup
Method 3600C: Cleanup
Method 361 OB: Alumina Cleanup
Method 3611B: Alumina Column Cleanup and Separation of Petroleum Wastes
Method 3620B: Florisil Cleanup
Method 3630C: Silica Gel Cleanup
Method 3640A: Gel-Permeation Cleanup ;
Method 3650B: Acid-Base Partition Cleanup
Method 3660B: Sulfur Cleanup ;
Method 3665A: Sulfuric Acid/Permanganate ;Cleanup
4.3 Determination of Organic Analytes
4.3.1 Gas Chromatographic Methods
Method 8000B:
Method 8011:
Method 801 SB:
Method 8021B:
Method 8031:
Method 8032A:
Method 8033:
Method 8041:
Method 8061A:
by
Method
Method
Method
Method
Method
Method
Method
8070A:
8081A:
8082:
8091:
8100:
8111:
8121:
Method 8131:
Method 8141 A:
Method 8151 A:
Determinative Chromatographic Separations
1,2-Dibromoethane and ] 1,2-Dibromo-3-chloropropane
Microextraction and Gas Chromatography
Nonhalogenated Organics Using GC/FID
Aromatic and Halogenated Volatiles by Gas Chromatography Using
Pholtoionization and/or Electrolytic Conductivity Detectors
Acrylonitrile by Gas Chromatography
Acrylamide by Gas Chromatography
Acetonitrile by Gas Chromatography with Nitrogen-Phosphorus
Detection
Phenols by Gas Chromatography
Phthalate Esters by Gas Chromatography with Electron Capture
Detection (GC/ECD)
Nitrosamines by Gas Chromatography
Organochlorine Pesticides by Gas Chromatography
Polychlorinated Biphenyls (PCBs) by Gas Chromatography
Nitroaromatics and Cyclic Ketones by Gas Chromatography
Polynuclear Aromatic Hydrocarbons
Haloethers by Gas Chromatography
Chlorinated Hydrocarbons by Gas Chromatography: Capillary
Column Technique
Aniline and Selected Derivatives by Gas Chromatography
Organophosphorus Compounds by Gas Chromatography: Capillary
Column Technique
Chlorinated Herbicides by GC Using Methylation
Penllafluorobenzylation Derivatization
or
CONTENTS - 5
Revision 5
April 1998
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4.3.2 Gas Chromatographic/Mass Spectroscopic Methods
Method 8260B: Volatile Organic Compounds by Gas Chromatography/Mass
Spectrometry (GC/MS)
Method 8270C: Semivolatile Organic Compounds by Gas Chromatography/Mass
Spectrometry (GC/MS)
Method 8275A: Semivolatile Organic Compounds (PAHs and PCBs) in Soils/Sludges
and Solid Wastes Using Thermal Extraction/Gas
Chromatography/Mass Spectrometry (TE/GC/MS)
Method 8280A: The Analysis of Polychlorinated Dibenzo-p-Dioxins and
Polychlorinated Dibenzofurans by High Resolution Gas
Chromatography/Low Resolution Mass Spectrometry (HRGC/LRMS)
Method 8290: Polychlorinated Dibenzodioxins (PCDDs) and Polychlorinated
Dibenzofurans (PCDFs) by High-Resolution Gas
Chromatography/High-Resolution Mass Spectrometry (HRGC/HRMS)
Attachment A: Procedures for the Collection, Handling, Analysis, and
Reporting of Wipe Tests Performed within the Laboratory
4.3.3 High Performance Liquid Chromatographic Methods
Method 8310: Polynudear Aromatic Hydrocarbons
Method 8315A: Determination of Carbonyl Compounds by High Performance Liquid
Chromatography (HPLC)
Appendix A: Recrystallization of 2,4-Dinitrophenylhydrazine (DNPH)
Method 8316: Acrylamide, Acrylonitrile and Acrolein by High Performance Liquid
Chromatography (HPLC)
Method 8318: N-Methylcarbamates by High Performance Liquid Chromatography
(HPLC)
Method 8321A: Solvent Extractable Nonvolatile Compounds by High Performance
Liquid Chromatography/Thermospray/Mass Spectrometry
(HPLC/TS/MS) or Ultraviolet (UV) Detection
Method 8325: Solvent Extractable Nonvolatile Compounds by High Performance
Liquid Chromatography/Pariicle Beam/Mass Spectrometry
(HPLC/PB/MS)
Method 8330: Nitroaromatics and Nitramines by High Performance Liquid
Chromatography (HPLC)
Method 8331: Tetrazene by Reverse Phase High Performance Liquid
Chromatography (HPLC)
Method 8332: Nitroglycerine by High Performance Liquid Chromatography
4.3,4 Infrared Methods
Method 8410: Gas Chromatography/Fourier Transform Infrared (GC/FT-IR)
Spectrometry for Semivolatile Organics: Capillary Column
Method 8430: Analysis of Bis(2-chloroethyl) Ether and Hydrolysis Products by Direct
Aqueous Injection GC/FT-IR
Method 8440: Total Recoverable Petroleum Hydrocarbons by Infrared
Spectrophotometry
CONTENTS-6 Revisions
April 1998
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4.3.5 Miscellaneous Spectrometric Methods
Method 8520: Continuous Measurement of Formaldehyde in Ambient Air
4.4 Immunoassay Methods i
Method 4000: Immunoassay
Method 401OA: Screening for Pentachlorophenol by Immunoassay
Method 4015: Screening for 2,4-Dichlorophenoxyacetic Acid by Immunoassay
Method 4020: Screening for Polychlorinated Biphenyls by Immunoassay
Method 4030: Soil Screening for Petroleum Hydrocarbons by Immunoassay
Method 4035: Soil Screening for Polynuclear Aromatic Hydrocarbons by
Immunoassay
Method 4040: Soil Screening for Toxaphene by Immunoassay
Method 4041: Soil Screening for Chlordane by Immunoassay
Method 4042: Soil Screening for DDT by Immunoassay
Method 4050: TNT Explosives in Soil by Immunoassay
Method 4051: Hexahydro-I.S.S-trinitro-I.S.S-triazine (RDX) in Soil by .Immunoassay
4.5 Miscellaneous Screening Methods
Method 3810: Headspace
Method 3820: Hexadecane Extraction and Screening of Purgeable Organics
Method 8515: Colorimetric Screening Method for Trinitrotoluene (TNT) in Soil
Method 9078: Screening Test Method for Polychlorinated Biphenyls in Sorl
Method 9079: Screening Test Method for Poiychlorinated Biphenyls in Transformer
Oil
APPENDIX - COMPANY REFERENCES
NOTE: A suffix of "A" in the method number indicates revision one (the method has
been revised once). A suffix of "B" in the method number indicates revision two (the
method has been revised twice). A suffix of "C" in the method number indicates
revision three (the method has been revised three times). In order to properly
document the method used for analysis, the entire method number including the
suffix letter designation (e.g.,, A, B, or C) must be identified by the analyst. A
method reference found within.the RCRA regulations and the text of SW-846 methods
and chapters refers to the latest promulgated revision of the method, even though the
method number does not include the appropriate letter suffix.
CONTENTS - 7 Revision 5
April 1998
-------
VOLUME ONE
SECTION C
DISCLAIMER
ABSTRACT
TABLE OF CONTENTS
METHOD INDEX AND CONVERSION TABLE
PREFACE
CHAPTER ONE. REPRINTED - QUALITY CONTROL
1.0 Introduction
2.0 QA Project Plan
3.0 Field Operations
4.0 Laboratory Operations
5.0 Definitions
6.0 References
CHAPTER FIVE - MISCELLANEOUS TEST METHODS
Method 5050:
Method 901 OB:
Method 9012A:
Method 9013:
Method 9014:
Method 9020B:
Method 9021:
Method 9022:
Method 9023:
Method 9030B:
Method 9031:
Method 9034:
Method 9035:
Method 9036:
Method 9038:
Method 9056:
Method 9057:
Method 9060:
Method 9065:
Method 9066:
Method 9067:
Method 9070:
Method9071B:
Bomb Preparation Method for Solid Waste
Total and Amenable Cyanide: Distillation
Total and Amenable Cyanide (Automated Colorimetric, with Off-Line
Distillation)
Cyanide Extraction Procedure for Solids and Oils
Titrimetric and Manual Spectrophotometric Determinative Methods for
Cyanide
Total Organic Halides (TOX)
Purgeable Organic Halides (POX)
Total Organic Halides (TOX) by Neutron Activation Analysis
Extractable Organic Halides (EOX) in Solids
Acid-Soluble and Acid-Insoluble Sulfides: Distillation
Extractable Sulfides
Titrimetric Procedure for Acid-Soluble and Acid-Insoluble Sulfides
Sulfate (Colorimetric, Automated, Chlorari ilate)
Sulfate (Colorimetric, Automated, Methylthymol Blue, AA II)
Sulfate (Turbidimetric)
Determination of Inorganic Anions by Ion Chromatography
Determination of Chloride from HCI/CI2 Emission Sampling Train
(Methods 0050 and 0051) by Anion Chromatography
Total Organic Carbon
Phenolics (Spectrophotometric, Manual 4-AAP with Distillation)
Phenolics (Colorimetric, Automated 4-AAP with Distillation)
Phenolics (Spectrophotometric, MBTH with Distillation)
See Method 1664, Publication No. EPA-821-R-98-002
n-Hexane Extractable Material (HEM) for Sludge, Sediment, and Solid
Samples
CONTENTS - 8
Revision 5
April 1998
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Method 9075:
Method 9076:
Method 9077:
Method A:
Method B:
Method C:
Method 9131:
Method 9132:
Method 9210:
Method 9211:
Method 9212:
Method 9213:
Method 9214:
Method 9215:
Method 9250:
Method 9251:
Method 9253:
Method 9320:
Test Method for Total Chlorine in New and Used Petroleum Products
by X-Ray Fluorescence Spectrometry (XRF)
Test Method for Total Chlorine in New and Used Petroleum Products
by Oxidative Combustion and Microcoulometry
Test Methods for Total Chlorine in New and Used Petroleum
Products (Field Test Kit Methods)
Fixed End Point Test Kit Method
Reverse Titration Quantitative End Point Test Kit Method
Direct Titration Quantitative End Point Test Kit Method
Total Coliform: Multiple Tube Fermentation Technique
Total Coliform: Membrane-Filter Technique
Potentiometric Determination of Nitrate in Aqueous Samples with Ion-
Selective Electrode
Potentiometric Determination of Bromide in Aqueous Samples with
Ion-Selective Electrode
Potentiometric Determination of Chloride in Aqueous Samples with
Ion-Selective Electrode
Potentiometric Determination of Cyanide in Aqueous Samples and
Distillates with Ion-Selective Electrode
Potentiometric Determination of Fluoride in Aqueous Samples with
Ion-Selective Electrode
Potentiometric Determination of Sulfide in Aqueous Samples and
Distillates with Ion-Selective Electrode
Chloride (Colorimetric, Automated Ferricyanide AAI)
Chloride (Colorimetric, Automated Ferricyanide AAI I)
Chloride (Titrimetric, Silver Nitrate)
Radium-228
CHAPTER SIX - PROPERTIES
Method 1030:
Method 1120:
Method 1312:
Method 1320:
Method 1330A:
Method 9041 A:
Method 9045C:
Method 9050A:
Method 9080:
Method 9081:
Method 9090A:
Method 9095A:
Method 9096:
Appendix A:
Method 9100:
Method 9310:
Method 9315:
Ignitability of Solids
Dermal Corrosion
Synthetic Precipitation Leaching Procedure
Multiple Extraction Procedure
Extraction Procedure for Oily Wastes
pH Paper Method
Soil and Waste pH
Specific Conductance ;
Cation-Exchange Capacity of Soils (Ammonium Acetate)
Cation-Exchange Capacity of Soils (Sodium Acetate)
Compatibility Test for Wastes and Membrane Liners
Paint Filter Liquids Test
Liquid Release Test (LRT) Procedure
Liquid Release Test Pre-Test
Saturated Hydraulic Conductivity, Saturated Leachate Conductivity,
and Intrinsic Permeability
Gross Alpha and Gross Beta
Alpha-Emitting Radium Isotopes
CONTENTS - 9
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PART II CHARACTERISTICS
CHAPTER SEVEN - CHARACTERISTICS INTRODUCTION AND REGULATORY DEFINITIONS
7.1 Ignitability
7.2 Corrosivity
7.3 Reactivity
Test Method to Determine Hydrogen Cyanide Released from Wastes
Test Method to Determine Hydrogen Sulfide Released from Wastes
7.4 Toxicity Characteristic Leaching Procedure
CHAPTER EIGHT- METHODS FOR DETERMINING CHARACTERISTICS
8.1 Ignitability
Method 1010: Pensky-Martens Closed-Cup Method for Determining Ignitability
Method 1020A: Setaflash Closed-Cup Method for Determining Ignitability
8.2 Corrosivity
Method 9040B: pH Electrometric Measurement
Method 1110: Corrosivity Toward Steel
8.3 Reactivity
8.4 Toxicity
Method 1310A: Extraction Procedure (EP) Toxicity Test Method and Structural
Integrity Test
Method 1311: Toxicity Characteristic Leaching Procedure :
APPENDIX - COMPANY REFERENCES
MOTE: A suffix of "A" in the method number indicates revision one (the method has
been revised once). A suffix of "B" in the method number indicates revision two (the
method has been revised twice). A suffix of "C" in the method number indicates
revision three (the method has been revised three times). In order to properly
document the method used for analysis, the entire method number including the
suffix letter designation (e.g., A, B, or C) must be identified by the analyst. A
method reference found within the RCRA regulations and the text of SW-846 methods
and chapters refers to the latest promulgated revision of the method, even though the
method number does not include the appropriate letter suffix.
CONTENTS - 10 Revision 5
April 1998
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VOLUME TWO
DISCLAIMER
ABSTRACT
TABLE OF CONTENTS
METHOD INDEX AND CONVERSION TABLE
PREFACE
CHAPTER ONE, REPRINTED - QUALITY CONTROL
1.0 Introduction
2.0 QA Project Plan
3.0 Field Operations
4.0 Laboratory Operations
5.0 Definitions
6.0 References
PART III SAMPLING
CHAPTER NINE - SAMPL INin PLAN
9.1 Design and Development
9.2 Implementation
CHAPTER TEN - SAMPLING METHODS
Method 0010:
Appendix A:
Appendix B:
Method 0011:
Method 0020:
Method 0023A:
Method 0030:
Method 0031:
Method 0040:
Method 0050:
Method 0051:
Method 0060:
Method 0061:
Method 0100:
Modified Method 5 Sampling Train
Preparation of XAD-2 Sorbent Resin
Total Chromatographable Organic Material Analysis
Sampling for Selected Aldehyde and Ketone Emissions from
Stationary Sources
Source Assessment Sampling System (SASS)
Sampling Method for Polychlorinated Dibenzo-p-Dioxins and
Polychlorinated Dibenzo.furan Emissions from Stationary Sources
Volatile Organic Sampling Train
Sampling Method for Volatile Organic Compounds (SMVOC)
Sampling of Principal Organic Hazardous Constituents from
Combustion Sources Using Tedlar® Bags
Isokinetic HCI/CI2 Emission Sampling Train
Midget Impinger HCI/CI2 Emission Sampling Train
Determination of Metals in Stack Emissions
Determination of Hexavalent Chromium Emissions from Stationary
Sources
Sampling for Formaldehyde and Other Carbonyl Compounds in Indoor
Air
CONTENTS - 11
Revision 5
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PART IV MONITORING
CHAPTER ELEVEN - GROUND WATER MONITORING
11.1 Background and Objectives
11.2 Relationship to the Regulations and to Other Documents
11.3 Revisions and Additions
11.4 Acceptable Designs and Practices
11.5 Unacceptable Designs and Practices
CHAPTER TWELVE - LAND TREATMENT MONITORING
12.1 Background
12.2 Treatment Zone
12.3 Regulatory Definition
12.4 Monitoring and Sampling Strategy
12.5 Analysis
12.6 References and Bibliography
CHAPTER THIRTEEN - INCINERATION
13.1 Introduction
13.2 Regulatory Definition
13.3 Waste Characterization Strategy
13.4 Stack-Gas Effluent Characterization Strategy
13.5 Additional Effluent Characterization Strategy
13.6 Selection of Specific Sampling and Analysis Methods
13.7 References
APPENDIX- COMPANY REFERENCES
NOTE: A suffix of "A" in the method number indicates revision one (the method has
been revised once). A suffix of "B" in the method number indicates revision two (the
method has been revised twice). A suffix of "C" in the method number indicates
revision three (the method has been revised three times). In order to properly
document the method used for analysis, the entire method number including the
suffix letter designation (e.g., A, B, or C) must be identified by the analyst. A
method reference found within the RCRA regulations and the text of SW-846 methods
and chapters refers to the latest promulgated revision of the method, even though the
method number does not include the appropriate letter suffix.
CONTENTS-12
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CHAPTER FIVE
MISCELLANEOUS TEST METHODS
Prior to employing the methods in this chapter, analysts are advised to consult the disclaimer
statement at the front of this manual and the information in Chapter Two for guidance on the allowed
flexibility in the choice of apparatus, reagents, and supplies. In addition, unless specified in a
regulation, the use of SW-846 methods is not mandatory in response to Federal testing
requirements. The information contained in each procedure is provided by EPA as guidance to be
used by the analyst and the regulated community in making judgements necessary to meet the data
quality objectives or needs for the intended use of the data.
The following methods are found in Chapter Five:
Method 5050:
Method 9010B:
Method 9012A:
Method 9013:
Method 9014:
Method
Method
Method
Method
Method
Method
Method
9020B:
9021:
9022:
9023:
9030B:
9031:
9034:
Method 9035:
Method 9036:
Method 9038:
Method 9056:
Method 9057:
Method 9060:
Method 9065:
Method 9066:
Method 9067:
Method 9070:
Method 9071B:
Method 9075:
Method 9076:
Bomb Preparation Method for Solid Waste
Total and Amenable Cyanide: Distillation
Total and Amenable Cyanide (Automated Colorimetric, with
Off-line Distillation)
Cyanide Extraction Procedure for Solids and Oils
Titrimetric and Manual Spectrophotometric Determinative
Methods for Cyanide
Total Organic Halicles (TOX)
Purgeable Organic Halides (POX)
Total Organic Halicles (TOX) by Neutron Activation Analysis
Extractable Organic Halides (EOX) in Solids
Acid-Soluble and Acid-Insoluble Sulfides: Distillation
Extractable Sulfides
Titrimetric Procedure for AcidrSoluble and Acid-Insoluble
Sulfides .
Sulfate (Colorimetric, Automated, Chloranilate)
Sulfate (Colorimetric, Automated, Methylthymol Blue, AA II)
Sulfate (Turbidimetric)
Determination of Inorganic Anions by Ion Chromatography
Determination of Chloride from HCI/CI2 Emission Sampling
Train (Methods 0050 and 0051) by Anion Chromatography
Total Organic Carbon
Phenolics (Spectrophotometric, Manual 4-AAP with
Distillation) :
Phenolics (Colorimetric, Automated 4-AAP with Distillation)
Phenolics (Spectrophotometric, MBTH with Distillation)
See Method 1664, Publication No. EPA-821-R-98-002
n-Hexane Extractable Material (HEM) for Sludge, Sediment,
and Solid Samples
Test Method for Total Chlorine in New and Used Petroleum
Products by X-Ray Fluorescence Spectrometry (XRF)
Test Method for Total Chlorine in New and Used Petroleum
Products by Oxidative Combustion and Microcoulometry
FIVE - 1
Revision 3
April 1998
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Method 9077:
Method A:
Method B:
Method C:
Method 9131:
Method 9132:
Method 9210:
Method 9211:
Method 9212:
Method 9213:
Method 9214:
Method 9215:
Method 9250:
Method 9251:
Method 9253:
Method 9320:
Test Methods for Total Chlorine in New and Used Petroleum
Products (Field Test Kit Methods)
Fixed End Point Test Kit Method
Reverse Titration Quantitative End Point Test Kit
Method
Direct Titration Quantitative End Point Test Kit Method
Total Coliform: Multiple Tube Fermentation Technique
Total Coliform: Membrane-Filter Technique
Potentiometric Determination of Nitrate in Aqueous Samples
with Ion-Selective Electrode
Potentiometric Determination of Bromide in Aqueous Samples
with Ion-Selective Electrode
Potentiometric Determination of Chloride in Aqueous Samples
with Ion-Selective Electrode
Potentiometric Determination of Cyanide in Aqueous Samples
and Distillates with Ion-Selective Electrode
Potentiometric Determination of Fluoride in Aqueous Samples
with Ion-Selective Electrode
Potentiometric Determination of Sulfide in Aqueous Samples
and Distillates with Ion-Selective Electrode
Chloride (Colorimetric, Automated Ferricyanide AAI)
Chloride (Colorimetric, Automated Feirricyanide AAI I)
Chloride (titrimetric, Silver Nitrate)
Radium-228
FIVE - 2
Revision 3
April 1998
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METHOD 9070
See Method 1664, Publication No. EPA-821-R-98-002.
Referral to Method 1664
April 1998
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-------
METHOD 9071B
n-HEXANE EXTRACTABLE MATERIAL. fHEM^ FOR SLUDGE. SEDIMENT. AND SOLID SAMPLES
1.0 SCOPE AND APPLICATION , • • ;
1.1 Method 9071 may be used to quantify low concentrations of oil and grease in soil,
sediments, sludges, and other solid materials amenable to chemical drying and solvent extraction
with n-hexane. "Oil and grease" is a conventional pollutant under 40 CFR 401.16 and generally
refers to substances, including biological lipids and mineral hydrocarbons, that have similar physical
characteristics and common solubility in an organic extracting solvent. As such, oil and grease is
an operationally defined parameter, and the results will depend entirely on the extracting solvent and
method of extraction. Method 9071 employs n-hexane as the extraction solvent with Soxhlet
extraction and the results of this method are appropriately termed "n-hexane extractable material
(HEM)." Section 1.2 lists the type of materials that may be extracted by this method. In the context
of this method, "HEM" is used throughout this method and for operational purposes, may be
considered synonymous with "oil and grease" within the limitations discussed below.
1.2 Specifically, Method 9071 is suitable for extracting relatively non-volatile hydrocarbons,
vegetable oils, animal fats, waxes, soaps, greases, biological lipids, and related materials.
1.3 Method 9071 is not recommended for measuring materials that volatilize at
temperatures below 85°C. Petroleum fuels from gasoline through #2 fuel oil may be partially lost
during the solvent removal process.
1.4 Some crude oils and heavy fuel oils may contain materials that are not soluble in
n-hexane, and recovery of these materials may be low. ;
2.0 SUMMARY OF METHOD
2.1 A representative portion of wet (as received) waste is acidified with concentrated HCI
and chemically dried with magnesium sulfate or sodium sulfate. Magnesium sulfate monohydrate
is used to dry acidified sludges as it will combine with 75% of its own weight in water in forming
MgSO4 • 7H2O. Anhydrous sodium sulfate is used to dry soil and sediment samples.
2.2 After drying, the HEM is extracted with n-hexane using a Soxhlet apparatus. The
n-hexane extract is then distilled from the extract and the HEM is desiccated and weighed.
2.3 When necessary, a separate sample portion is evaluated for percent solids, and the
dry weight fraction may be used to calculate the dry-weight HEM concentration of the soil, sediment,
or waste.
3.0 DEFINITIONS ' ;
3.1 n-Hexane extractable material (HEM, oil and grease): Material that is extracted from
a sample using n-hexane and determined by this method. This material includes relatively non-
volatile hydrocarbons, vegetable oils, animal fats, waxes, soaps, greases, and related matter.
3:2 Refer to Chapter One for additional definitions. ,
9071B-1 : Revision 2
: April 1998
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4.0 INTERFERENCES
4.1 This method is entirely empirical, and duplicate results having a high degree of
precision can be obtained only by strict adherence to all details. The rate of cycling and time of
extraction in the Soxhlet apparatus must be consistent and length of time required for drying and
cooling extracted materials must be the same in order to generate consistent results. It is important
that the procedures be performed as directed due to the varying solubilities of the different greases
and heavy mineral oils.
4.2 Solvents, reagents, glassware, and other sample-processing hardware may yield
artifacts that could affect the results. All solvents and reagents used in the analysis should be
demonstrated to be free from interferences by processing a method blank with each analytical batch.
Specific selection of reagents, solvent washes, or purification of solvents may be required. Use of
plastic measuring devices, and/or plastic tubing attachments must be avoided.
4.3 Glassware should be cleaned by washing with hot tap water with detergent, rinsing with
tap water and reagent water, and rinsing with solvent. Glassware may also be baked at 200-250 °C
for 1 hour. Boiling flasks that are used to contain the extracted residues may be dried in an oven
at 105-115°C and stored in a desiccator until used. Depending on the project DQOs, strict
adherence to the washing and handling procedures cited above may not be necessary as long as
the laboratory can demonstrate that alternative cleaning procedures yield acceptable method
performance and meet method blank acceptance criteria.
4.4 A gradual increase in weight may result due to the absorption of oxygen; a gradual loss
of weight may result due to volatilization. Extracted residues should be maintained in a desiccator
during cooling and prior to weighing. Extracted residues should be weighed as soon as possible
after cooling.
4.5 The presence of non-oily extractable substance such as sulfur compounds, organic
dyes, and chlorophyll, may result in a positive bias. For the purpose of this method, all materials
extracted and retained during this procedure'are defined as HEM.
5.0 SAFETY
5.1 The toxicity or carcinogenicity of each reagent used in this method has not been
* precisely determined; however, each chemical should be treated as a potential health hazard.
Exposure to these chemicals should be reduced to the lowest possible level. It is suggested that the
laboratory perform personal hygiene monitoring of each analyst that uses this method. This
monitoring should be performed using Occupational Safety and Health Administration (OSHA) or
National Institute of Occupational Safety and Health (NIOSH) approved personal hygiene monitoring
methods. Results of this monitoring should be made available to the analyst.
5.2 n-Hexane has been shown to have increased neurotoxic effects over other hexanes
and some other solvents. OSHA has proposed a time-weighted average (TWA) of 50 parts-per-
million (ppm); NIOSH concurs that an 8-hour TWA/permissible exposure limit (PEL) of 50 ppm is
appropriate for n-hexane; and the American Conference of Governmental Industrial Hygienists
(ACGIH) has published a threshold limit value (TLV) of 50 ppm for n-hexanel Inhalation of n-hexane
should be minimized by performing all operations with n-hexane in a explosion-proof hood or well-
ventilated area.
9071B-2
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5.3 n-Hexane has a flash point of -23 °C (-9°F), has explosive limits in air in the range of
1 to 7 percent, and poses a serious fire risk when heated or exposed to flame. n-Hexane can react
vigorously with oxidizing materials. The laboratory should include procedures in its operations that
address the safe handling of n-hexane.
5.4 Unknown samples may contain high concentrations of volatile toxic compounds.
Sample containers should be opened in a hood and handled with gloves to prevent exposure.
5.5 This method does not address all safety issues associated with its use. The laboratory
is responsible for maintaining a safe work environment and a current awareness file of OSHA
regulations regarding the safe handling of the chemicals specified in this method. A reference file
of material safety data sheets (MSDSs) should be available to all personnel involved in these
analyses.
6.0 EQUIPMENT AND SUPPLIES
6.1 Soxhlet extraction apparatus.
6.2 Heating mantle - explosion-proof, with temperature control.
6.3 Boiling flask - 125-mL or appropriate size.
6.4 Analytical balance - capable of weighing 0.1 mg.
6,5 Vacuum pump, or other vacuum source.
6.6 Paper extraction thimble for Soxhlet apparatus. ;
6.7 Glass wool or small glass beads to fill thimble.
6.8 Grease-free, non-absorbent cotton - To remove possible interferences, each batch of
cotton should be washed with n-hexane. Solvent washing may not be necessary if the laboratory
can demonstrate that the unwashed cxrtton does not affect the performance of the method or that
the concentration of HEM in the sample is so high that low contaminant concentration is
insignificant.
6.9 Beakers-100-150-mL.
6.10 pH paper.
6.11 Porcelain mortar and pestle. '.
6.12 Extraction flask - 150-ml. or appropriate size.
6.13 Waterbath or steam bath-explosion-proof - capable of maintaining a temperature of at
least 85°C.
6.14 Distilling apparatus - For removing n-hexane from extract.
6.14.1 Distilling head-Claisen (VWR Scientific No 26339-005, or equivalent), includes
Claisen-type connecting tube and condenser.
9071B-3 ' Revision 2
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6.14.2 Distillation adapter (used to attach distilling head and to the waste collection
flask for recovery of solvent).
6.14.3 Distillate collection flask (attached to the distilling adaptor for collection of the
distilled solvent).
6.14.4 Ice bath or recirculating chiller (to aid in the condensation and collection of
the distilled solvent).
1 ' i . ''
6.15 Desiccator - Cabinet or jar type, capable of holding boiling flasiks during cooling and
storage.
6.16 Tongs - for handling the boiling flasks.
6.17 Glass fiber filter paper - Whatman No. 40 or equivalent.
"
6.18 Boiling chips - Silicon carbide or fluoropolymer.
1 !
7.0 REAGENTS
7.1 Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is
intended that all reagents shall conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society, where such specifications are available. Other grades
may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its
use without lessening the accuracy of the determination.
" •, • i ' '
7.2 Reagent water. All references to water in this method refer to reagent water, as defined
in Chapter One.
7.3 Concentrated hydrochloric acid (HCI).
7.4 Magnesium sulfate monohydrate. Prepare MgSO4 • H2O by spreading a thin layer in
a dish and drying in an oven at 150°C overnight. Store in a tightly sealed glass container until used.
I. • " I :,l I , ,
7.5 Sodium sulfate, granular, anhydrous (Na2SO4). Purify by heating at 400°C for 4 hours
in a shallow tray, or by precleaning the sodium sulfate with methylene chloride. If the sodium sulfate
5s precleaned with methylene chloride, a method blank must be analyzed, demonstrating that there
is no interference from the sodium sulfate. Store in a tightly sealed glass container until used.
. . i -r !• •
7.6 n-Hexane. Purity of 85%, 99.0% minimum saturated C6 isomers, residue less than 1
mg/L Boiling point, 69° C.
7.7 Hexadecane(CH3(CH2)14CH3)/stearic acid (CH3(CH2)16COOH). 1:1 spiking solution.
Prepare in acetone at a concentration of 2 mg/mL each.
Weigh 200 ± 2 mg of stearic acid and 200 ± 2 mg hexadecane into a 100 ml_ volumetric flask
and fill to the mark with acetone. The total concentration of this stock is 4000 mg/L (ppm) HEM. This
standard may be used for spiking samples and preparing laboratory control samples. Store in a
glass container with a fluoropolymer-lined cap at room temperature. Shield from light.
Note: The spiking solution may require warming for complete dissolution of stearic acid.
9071B-4
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!,, JAl'ii"
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8.0 SAMPLE COLLECTION, PRESERVATION, AND STORAGE
8.1 A minimum of 100 grams of sample should be collected using a metal spatula, spoon,
or equivalent device. Samples should be collected into a pre-cleaned wide-mouth glass container
fitted with a TFE-lined screw cap.
i
8.2 When practical (i.e., when the sample matrix allows the complete mixing of sample and
acid such as with a pourable sludge or sediment), the sample should be preserved to a pH < 2 by
adding 1 mL of concentrated HCI per 100 gram of sample and cooled to 4 ± 2 °C. If acidification is
not practical (as with a dry soil), the addition of the HCI is not required and the sample should be
cooled to 4 ± 2 °C. The laboratory must be notified so that the sample can be acidified prior to
analysis.
8.3 A holding time has not been established for HEM in solids, but it is recommended that
the sample be analyzed as soon as possible.
9.0 QUALITY CONTROL
9.1 Each laboratory that uses this method is required to operate a formal quality control
program. The minimum requirements of this program consist of an initial demonstration of laboratory
capability and the analysis of spiked samples as a continuing check on performance. The laboratory
is required to maintain performance records to define the quality of data that is generated.
9.2 Employ a minimum, of one method blank per analytical batch or twenty samples,
whichever is more frequent, to verify that all reagents, solvents, and equipment are contamination
free. Prepare the method blank from 5 g of inert matrix such as pre-deaned sand or similar material,
and carry it through the analytical process.
9.3 Run one matrix duplicate and matrix spike sample every twenty samples or analytical
batch, whichever is more frequent. Matrix duplicates and spikes are brought through the whole
sample preparation and analytical process.
9.4 The performance of the method should be evaluated by the use of a Laboratory Control
Sample (LCS). The LCS is prepared by spiking an inert matrix (as pre-cleaned sand or similar
material) with an appropriate volume of spiking solution (Sec. 7.7) and carrying it through the
analytical process. . :
10.0 CALIBRATION AND STANDARDIZATION
10.1 Calibrate the analytical balance at 2 mg and 1000 mg using class "S" weights.
10.2 Calibration shall be within ± 10% (i.e., ± 0,2 mg) at 2 mg and ± 0.5 % (i.e., ± 5 mg) at
1000 mg. If values are not within these limits, recalibrate the: balance.
9071B-5 Revision 2
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11.6 PROCEDURE
11.1 Determination of Sample Dry Weight Fraction
- , . . • • „ , i
11.1.1 When it is necessary to report the HEM on a dry weight basis, determine the
' dry weight fraction using a separate aliquot of sample, as discussed below. The aliquot used
for this determination cannot be used to evaluate HEM.
11.1.2 Weigh 5-10 gram (± 0.01 gram) of the sample into pre-weighed crucible.
Determine the weight of the wet sample by subtracting the weight of the crucible.
11.1.3 Place the crucible with the wet sample in an oven overnight at 105°C.
Remove crucible from oven and place in a desiccator to cool. Weigh. Determine dry weight
of sample by subtracting the weight of the crucible. Determine the dry weight fraction of the
sample as follows:
NOTE: The drying oven should be contained in a hood or vented. Significant
laboratory contamination may result from a heavily contaminated hazardous
waste sample.
i
• u*«. « g of dry sample
dry weight fraction = M -* -~L—
g of sample
11.2 Sample Preparation.
11.2.1 Sludge/Waste Samples
11.2.1.1 Weigh out 20 ± 0.5 grams of wet sample into a 150-mL beaker.
11.2.1.2 If the sample has not been acidified, acidify to a pH <; 2 with
approximately 0.3 ml_ concentrated HCI.
11.2.1.3 Add 25 grams Mg2SO4 • H2O (Sec. 7.4) and stir to a smooth
paste.
11.2.1.4 Spread paste on sides of beaker to facilitate evaporation. Let
stand about 15-30 min or until material is solidified.
: i I . '
11.2.1.5 Remove solids and grind to fine powder in a mortar.
11.2.1.6 Add the powder to the paper extraction thimble.
11.2.1.7 Wipe beaker and mortar with pieces of filter paper moistened with
n-hexane and add to thimble.
11.2.1.8 Fill thimble with glass wool (or glass beads).
9071B - 6 Revision 2
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11.2.2 Sediment/Soil Samples
11.2.2.1 Decant and discard any water layer on a sediment sample. Mix
sample thoroughly, especially composited samples. Discard any foreign objects such
as sticks, leaves, and rocks.
11.2.2.2 Blend 10 grams of the sample with 10 grams of anhydrous sodium
sulfate (Sec. 7.5) as described in Section 11.2.1. Transfer homogenized paste to an
extraction thimble and cover with glass wool or glass beads. The extraction thimble
must drain freely for the duration of the extraction period.
11.3 Extraction
11.3.1 Set-up the Soxhlet apparatus containing the extraction thimble and sample
and attach a 125-mL boiling flask containing 90 mL of n-hexane. Add boiling chips. Adjust the
heating control on the heating mantle so that a cycling rate of 20 cycles/h is obtained. Extract
for a period of 4 hrs.
11.3.2 Tare a clean 250-mL or appropriate sized boiling flask as follows:
11.3.2.1 Dry the flask in an oven at 105-115°C for a minimum of 2 h.
11.3.2.2 Remove from the oven and immediately transfer to a desiccator
to cool at room temperature.
11.3.2.3 When cool, remove from the desiccator with tongs and weigh
immediately on a calibrated balance.
11.3.3 At the end of the 4 h extraction period, filter the extract through grease-free
cotton, into the pre-weighed boiling flask (Sec. 11.3.2). Use gloves to avoid adding fingerprints
to the flask.
11.3.4 Rinse flask and cotton with n-hexane and add to the 250-mL boiling flask.
NOTE: If the extract is clear and no suspended particles are present, the filtration
Step may be omitted.
11.3.5 Connect the boiling flask to the distilling head apparatus and distill the solvent
by immersing the lower half of the flask in a water bath or a steam bath. A heating mantle may
also be used. Adjust the temperature of the heating device to complete the distillation in less
than 30 minutes. Collect the solvent for reuse or appropriate disposal.
11.3.6 When the distillation is complete, remove the distilling head. Immediately
remove the flask from the heat source and wipe the outside to remove excess moisture and
fingerprints. To remove solvent vapor, sweep out the flask for 15 sec with air by inserting a
glass tube that is connected to a vacuum source.
11.3.7 Cool the boiling flask in a desiccator for 30 min and weigh. Determine the
gain in weight of the boiling flask by subtracting the weight of the boiling flask (Sec. 11.3.2)
from the final boiling flask weight.
9071B - 7 Revision 2
April 1998
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12.0 DATA ANALYSIS AND CALCULATIONS
Calculate the concentration of HEM in the sample as follows:
,._.. ... . ... gam in weight of flask(mg) X 1000
HEM (mg/kg wet weight) = *- . * . —\.., .
weight of wet solid (g)
NOTE: If it is necessary to report the results on a dry weight basis, divide the result
obtained above by the dry weight fraction calculated in Sec. 11.1.3. Report
the results as mg/kg HEM dry weight. If it is necessary to report the results
as a percentage of the wet or dry weight, divide the wet-weight concentration
or dry weight concentration by 10,000 and report the result as % HEM wet or
dry weight.
i i . •• .
•
13.0 METHOD PERFORMANCE
In a preliminary study designed to find a suitable replacement for F:reon-113, three EPA
contract laboratories evaluated a total of 28 solid samples derived from various industrial and
commercial processes for oil and grease. This study evaluated a total of six solvents, including n-
hexane, to determine which of the alternative solvents produced results most closely with that of
Freon-113. In tfiis study, each waste was Soxhlet-extractecl in triplicate using Freon-113 and each
of the alternative solvents. Based on the overall results, n-hexane was judged to be the best
alternative solvent. The data provided in Table i compare the results for Freon-113 and n-hexane
for each waste. For a complete discussion of this study, refer to reference 1 in Section 16.0.
14.0 POLLUTION PREVENTION
14.1 Pollution prevention encompasses any technique that reduces or eliminates the quantity
and/or toxicity of waste at the point of generation. Numerous opportunities for pollution prevention
exist in laboratory operation. The EPA has established a preferred hierarchy of environmental
management techniques that places pollution prevention as the management option of first choice.
Whenever feasible, laboratory personnel should use pollution prevention techniques to address their
waste generation. When wastes cannot be feasibly reduced at the source, the Agency recommends
recycling as the next best option.
14.2 For information about pollution prevention that may be applicable to laboratories and
research institutions consult Less is Better Laboratory Chemical management for Waste Reduction
available from the American Chemical Society's Department of Government Relations and Science
Policy, 1155 16th St., N.W. Washington, D.C. 20036, (202) 872-4477.
15.0 WASTE MANAGEMENT
„• !| • '• |
The Environmental Protection Agency requires that laboratory waste management practices
be conducted consistent with all applicable Federal, state and local rules and regulations. The
Agency urges laboratories to protect the air, water, and land by minimizing and controlling all
releases from hoods and bench operations, complying with the letter and spirit of any sewer
i
9071B - 8 Revision 2
April 1998
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discharge permits and regulations, and by complying with all solid and hazardous waste regulations,
particularly the hazardous waste identification rules and land disposal restrictions. For further
information on waste management, consult The Waste Management Manual for Laboratory
Personnel available from the American Chemical Society at the address listed in Sec. 14.2.
16.0 REFERENCES , :
1. Preliminary Report of EPA Efforts to Replace Freon for the Determination of Oil and Grease,
United States Environmental Protection Agency, Office of Water, EPA-821-93-009. June 1993.
2. Method 1664, Revision A: n-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel
Treated N-Hexane Extractable Material (SGT-HEM) by Extraction and Gravimetry.
17.0 TABLES, DIAGRAMS, FLOWCHARTS, AND VALIDATION DATA
The pages to follow contain Table 1, and a flow diagram of the method procedure.
9071B-9 Revision 2
April 1998
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TABLE 1
SOXHLET EXTRACTION OF SOLIDS USING FREON-113 AND N-HEXANE
All concentrations in mg/kg
Facility/
Process
Paper Mill
POTW
Leather
Tannery
POTW
Petroleum
Refinery
Industrial
Laundry
Fish Oil
Plant
Coke Plant
Wood
Preserving
Plant
Drilling Fluid
Supplier
Contam.
Soils
Poultry Plant
Rolling Mill
Mayonnaise
•Plant
Seafood
Plant
Waste Stream
Dewatered
Sludge
Sewage
Sludge
Dewatered
Sludge
Digested
Sludge
API Separator
Sludge
DAF
Sludge
Oily
Sludge
Waste
Activated
Sludge
Solid
Waste
Used drilling
mud
kerosene
Contaminated
Soil
Waste
Activated
Sludge
Dewatered
Scale
Oily Sludge
Waste Sludge
Solvent:
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Rep
No. 1
11000
6600
98000
110000
11000
21000
130000
54000
320000
240000
310000
290000
890000
440000
8300
14000
150000
140000
1300
1300
2000
2500
38000
5900
11000
14000
880000
590000
64000
34000
9071 B-
Rep
No. 2
5300
2400
81000
86000
12000
15000
97000
76000
350000
320000
310000
360000
1000000
530000
8000
19000
140000
130000
1600
1200
1400
3200
11000
11000
14000
14000
850000
780000
31000
10
Rep
No. 3
7900
11000
81000
80000
12000
19000
66000
48000
250000
240000
240000
180000
770000
460000
18000
15000
140000
130000
1300
1600
1900
2600
40000
46000
17000
16000
780000
520000
53000
27000
Mean
Concen-
tration
8000
6600
87000
91000
42000
18000
98000
59000
310000
270000
290000
280000
890000
480000
11000
16000
140000
130000
1400
1400
1700
2800
30000
21000
14000
15000
840000
630000
58000
31000
!
Standard
Deviation
2762
4203
9940
13281
732
3201
33028
14516
53257
43822
41717
90819
131249
46318
5505
2732
3512
6557
.157
201
352
410
16263
21795
2884
983
50521
132020
7526
3867
Revision 2
April 1998
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TABLE 1
(CONTINUED) ;
Facility/
Process
Seafood
Plant
Poultry
Plant
Railroad
Yard
Can
Manufact
Plant
Soup Plant
Oily Water
Treatment
Plant
Can
Manufact
Plant
Can
Manufact
Plant
Drum
Handling
Facility
Polymer
Plant
Restaurant
Leather
Tannery
Waste Stream
Oily Sludge
DAF Sludge
Oily Sludge
Filter Cake
DAF Sludge
Oily Sludge
Oily Sludge
Filter Cake
Oily Sludge
Dewatered
Sludge
Vegetable Oil
Waste
Waste Sludge
Solvent:
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Freon
Hexane
Source: Reference 1
Rep
No. 1
400000
400000
670000
530000
870000
850000
62000
69000
600000
580000
76000
77000
94000
80000
290000
290000
1200000
990000
13000
8400
760000
1100000
180000
240000
9071 B-
Rep
No. 2
410000
390000
600000
530000
920000
840000
62000
64000
590000
520000
75000
60000
88000,
90000
290000
290000
1100000
1000000
12000
6900
610000
980000
220000
270000
11
Rep
No. 3
430000
390000
570000
530000
870000
830000
60000
66000
610000
600000
70000
79000
94000
83000
300000
290000
1200000
980000
8200
9100
780000
980000
190000
210000
Mean
Concen-
tration
410000
400000
610000
530000
890000
840000
61000
66000
600000
570000
74000
72000
92000
85000
290000
290000
1200000
1000000
11000
8100
720000
1000000
190000
240000
Standard
Deviation
16371
7095
49549
2449
27906
6884
976
2615
10066
40361
3215
107-13
3291
4992
6217
.2029
57735
27319
2524
1122
92060
80064
22140
31177
Revision 2
April 1998
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METHOD 9071B
n-HEXANE EXTRACTABLE MATERIAL fHEM^ FOR SLUDGE SEDIMENT. AND SOLID SAMPLES
11.1 Determine
dry weight fraction
of sample.
11.2.1.1 Weigh
a sample of
wet sludge
and place in
beaker.
11.2.1.2
Acidify to
pH <2.
11.2 Is
sample
sludge or
sediment/
soil?
11.2.2.1 Decant
water; mix
sample; discard
foreign objects.
11.2.2.2 Blend
with sodium
sulfate; add
to extraction
thimble.
11.2.1.3 Add
magnesium sulfate
monohydrate and
stir.
B
11.2.1.5
Remove and
grind solids
to a fine
powder.
9071 B- 12
Revision 2
April 1998
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METHOD 9071B
n-HEXANE EXTRACTABLE MATERIAL. (HEM) FOR SLUDGE.
(Continued)
SEDIMENT. AND SOLID SAMPLES
B
11.2.1.6 Add
powder to
paper
extraction
thimble.
11.2.1.7 Wipe
beaker and
mortar; add
to thimble.
11.2.1.8 Fill
thimble with
glass wool.
11.3.1 Extract
in Soxhlet
apparatus for
4 hours.
11.3.3 Filter
extract into
boiling flask.
11.3.4 Rinse
flask with
solvent.
11.3.5
Evaporate and
collect
solvent for
reuse.
11.3.6 Remove
solvent vapor.
11.3.7 Cool
and weigh
boiling flask.
12.0
Calculate
concentration
of HEM
Stop
9071 B- 13
Revision 2
April 1998
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