&EPA
United States
Environmental Protection
Agency
Standardized Analytical Methods for
Use During Homeland Security Events
Revision 2.0
September 29, 2005
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EPA/600/R-04/126B
September 2005
for
2.0
29,
Prepared by
Computer Sciences Corporation
Alexandria, VA 22304-3540
Prepared under
EPA Contract No. 68-W-01-034
Prepared for
Oba Vincent
Work Assignment Manager
National Homeland Security Research Center
United States Environmental Protection Agency
Office of Research and Development
Cincinnati, OH 45268
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Disclaimer
The U.S. Environmental Protection Agency through its Office of Research and Development funded and
managed the research described here under Contract 68-W-01-034 to Computer Sciences Corporation
(CSC). This document has been subjected to the Agency's peer and administrative review and has been
approved for publication as an EPA document.
Mention of trade names or commercial products in this document or in the methods referenced in this
document does not constitute endorsement or recommendation for use.
Questions concerning this documentor its application should be addressed to:
Oba Vincent
National Homeland Security Research Center
Office of Research and Development (163)
U.S. Environmental Protection Agency
26 West Martin Luther King Drive
Cincinnati, OH 45268
(513)569-7456
vincent.oba@epa.gov
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Use of This Document
The information contained in this document represents the latest step in an ongoing National
Homeland Security Research Center effort to provide standardized analytical methods for use by
laboratories tasked with performing analyses in response to a homeland security event.
Although at this time, many of the methods listed have not been tested for a particular analyte
(e.g., analytes not explicitly identified in the method) or matrix, the methods are considered to
contain the most appropriate currently available techniques. Unless a published method that is
listed in this document states specific applicability to the analyte/matrix pair for which it has been
selected, it should be assumed that method testing is needed. In these cases, adjustment may
be required to accurately account for variations in environmental matrices, analyte
characteristics, and target risk levels. Many of the target analytes listed in this document have
only recently become an environmental concern, and EPA is actively pursuing development and
validation of Standard Analytical Protocols (SAPs) based on the methods listed, including
optimization of procedures for measuring target compounds. In those cases where method
procedures are determined to be insufficient for a particular situation, EPA will provide guidance
regarding appropriate actions. This will be an ongoing process as EPA will strive to establish a
consistent level of validation for all listed analytes.
SAM Revision 2.0 Hi September 29, 2005
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Foreword
The U.S. Environmental Protection Agency is charged by Congress with protecting the Nation's land, air,
and water resources. Under a mandate of national environmental laws, the Agency strives to formulate
and implement actions leading to a compatible balance between human activities and the ability of
natural systems to support and nurture life. To meet this mandate, EPA's research program is providing
data and technical support for solving environmental problems today and building a scientific base
necessary to manage our ecological resources wisely, understand how pollutants affect our health, and
prevent or reduce environmental risks in the future.
The National Homeland Security Research Center (NHSRC) is the Agency's center for conducting
research to facilitate protection and decontamination of structures and water infrastructure subject to
chemical, biological, or radiological (CBR) terror attacks. NHSRC's research is designed to provide
appropriate, effective, and validated technologies, methods, and guidance to understand the risk posed by
CBR agents to enhance our ability to detect, contain, and clean up in the event of such attacks. NHSRC
will also provide direct technical assistance to response personnel in the event of a CBR attack, as well as
provide related interagency liaisons.
This publication has been produced as part of the Center's long-term research plan. It is published and
made available by EPA's Office of Research and Development to assist the user community and to link
researchers with their clients.
Andrew P. Avel, Acting Director
National Homeland Security Research Center
SAM Revision 2.0 iv September 29, 2005
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Abbreviations and Acronyms
AEM Applied and Environmental Microbiology
AGI sampler All Glass Impinger Sampler
AOAC AOAC International (formerly the Association of Official Analytical Chemists)
ASTM ASTM International (formerly the American Society for Testing and Materials)
BSL Biosafety Level
°C Degrees Celsius
Campy-BAC Campylobacter-Brucella agar base with sheep blood and antibiotics
CDC Centers for Disease Control and Prevention
CFR Code of Federal Regulations
CLP Contract Laboratory Program
CVAA Cold Vapor Atomic Absorption
CVAFS Cold Vapor Atomic Fluorescence Spectrometry
DAPI 4',6-diamidino-2-phenylindole
DHS Department of Homeland Security
DIC Differential Interference Contrast
DNA Deoxyribonucleic Acid
DNPH 2,4-dinitrophenylhydrazine
DoD Department of Defense
ED Electron Diffraction
EDTA Ethylenediaminetetraacetic acid
EDXA Energy Dispersive X-ray Analysis
EEB EHEC Enrichment Broth
EHEC Enterohemorrhagic Escherichia coll
EIA Enzyme Immunoassay
ELISA Enzyme-Linked Immunosorbent Assay
EMMI Environmental Monitoring Methods Index
EPA U.S. Environmental Protection Agency
EQL Estimated Quantitation Limit
FA Fluorescence Assay
FBI Federal Bureau of Investigation
FDA Food and Drug Administration
FID Flame lonization Detector
FITC Fluorescein isothiocyanate
FSIS Food Safety and Inspection Service
GC Gas Chromatograph or Gas Chromatography
GC/MS Gas Chromatograph/Mass Spectrometer or Gas Chromatography/Mass Spectrometry
GFAA Graphite Furnace Atomic Absorption Spectrophotometer or Graphite Furnace Atomic
Absorption Spectrophotometry
GITC Guanidinium isothiocyanate
HAV Hepatitis A Virus
HPLC High Performance Liquid Chromatograph or High Performance Liquid Chromatography
HPLC-FL High Performance Liquid Chromatograph - Fluorescence
HPLC-MS High Performance Liquid Chromatograph - Mass Spectrometer
1C Ion Chromatograph or Ion Chromatography
ICC Integrated cell culture
ICP Inductively Coupled Plasma
ICP-AES Inductively Coupled Plasma - Atomic Emission Spectrometry
SAM Revision 2.0
September 29, 2005
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ICR Information Collection Rule
IMS Immunomagnetic Separation
INCHEM INCHEM is a means of rapid access to internationally peer reviewed information on
chemicals commonly used throughout the world, which may also occur as contaminants
in the environment and food. It consolidates information from a number of
intergovernmental organizations whose goal it is to assist in the sound management of
chemicals, http://www.inchem.org/
IO Inorganic
ISO International Organization for Standardization
ISE Ion Specific Electrode
K-D Kuderna-Danish
LIA Lysine Iron Agar
LRN Laboratory Response Network
LSE Liquid/Solid Extraction
MS Mass Spectrometer or Mass Spectrometry or Matrix Spike
MSB Matrix Spike Duplicate
MW Molecular Weight
NA Not Applicable
NEMI National Environmental Methods Index
NERL-CI National Exposure Risk Laboratory-Cincinnati
NHSRC National Homeland Security Research Center
NIOSH National Institute for Occupational Safety and Health
NOS Not Otherwise Specified
NTIS National Technical Information Service
ONPG Ortho-nitrophenyl-p-D-galactopyranoside
OSHA Occupational Safety and Health Administration
OW Office of Water
PAHs Polycyclic Aromatic Hydrocarbons
PCBs Polychlorinated biphenyls
PCDDs Polychlorinated dibenzo-p-dioxins
PCDFs Polychlorinated dibenzofurans
PCR Polymerase Chain Reaction
PFE Pressurized Fluid Extraction
QC Quality Control
RNA Ribonucleic Acid
RP/HPLC Reversed-Phase High Performance Liquid Chromatography
RT-PCR Reverse Transcription-Polymerase Chain Reaction
SAED Selected Area Electron Diffraction
SM Standard Methods for the Examination of Water and Wastewater
SPE Solid-Phase Extraction
SW Solid Waste
TBD To Be Determined
TCBS Thiosulfate Citrate Bile Salts Sucrose
TC SMAC Tellurite Cefixime Sorbitol MaConkey agar
TCLP Toxicity Characteristic Leaching Procedure
TEM Transmission Electron Microscope or Microscopy
TOXNET National Library of Medicine, Toxicological Database
TRF Time resolved fluorescence
TRU Trans Uranic
TS Thermospray
TSI Triple Sugar Iron
SAM Revision 2.0 vi September 29, 2005
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USD A U.S. Department of Agriculture
USGS U.S. Geological Survey
UV Ultraviolet
VEE Venezeulan Equine Encephalitis
VOCs Volatile Organic Compounds
VOA Volatile Organic Analysis
XLD Xylose lysine desoxycholate
SAM Revision 2.0 vii September 29, 2005
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Acknowledgments
The contributions of the following persons and organizations to the development of this document are
gratefully acknowledged:
EPA Homeland Security Laboratory Capability Workgroup Analytical Methods Subteam
Steve Allgeier, Office of Water
David Friedman, Office of Research and Development
Ben Hull, Office of Radiation and Indoor Air
Michael S. Johnson, Office of Solid Waste and Emergency Response
Alan Lindquist, Office of Research and Development
Rob Rothman, Office of Research and Development
Oba Vincent, Office of Research and Development
United States Environmental Protection Agency
• Office of Research and Development
Nancy Adams, National Homeland Security Research Center
Don Betowski, National Exposure Research Laboratory
Dermont Bouchard, National Exposure Research Laboratory
George Brilis, National Exposure Research Laboratory
Bill Brumley, National Exposure Research Laboratory
Bill Budde, National Exposure Research Laboratory
Joan Bursey, National Homeland Security Research Center
Christian Daughton, National Exposure Research Laboratory
Jane Denne, National Exposure Research Laboratory
Julius Enriquez, National Risk Management Research Laboratory
Bob Graves, National Exposure Research Laboratory
Ann C. Grimm, National Exposure Research Laboratory
Ed Heithmar, National Exposure Research Laboratory
Michael Hiatt, National Exposure Research Laboratory
Tammy Jones-Lepp, National Exposure Research Laboratory
Robert Lewis, National Exposure Research Laboratory
John Lyon, National Exposure Research Laboratory
William McClenney, National Exposure Research Laboratory
Georges-Marie Momplaisir, National Exposure Research Laboratory
Lantis Osemwengie, National Exposure Research Laboratory
Steven Pia, National Exposure Research Laboratory
Eugene Rice, National Homeland Security Research Center
Lee Riddick, National Exposure Research Laboratory
Kim Rogers, National Exposure Research Laboratory
Charlita Rosal, National Exposure Research Laboratory
Brian Schumacher, National Exposure Research Laboratory
Christopher Sibert, National Exposure Research Laboratory
Jerry Stelma, National Exposure Research Laboratory
Wayne Sovocool, National Exposure Research Laboratory
Jeanette VanEmon, National Exposure Research Laboratory
Katrina Varner, National Exposure Research Laboratory
John Zimmerman, National Exposure Research Laboratory
SAM Revision 2.0 viii September 29, 2005
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• Office of Water
Herb Brass, Office of Ground Water and Drinking Water
Jafrul Hasan, Office of Science and Technology, Health and Ecological Criteria Division
Carrie Moulton, Office of Ground Water and Drinking Water
Sandhya Parshionikar, Office of Ground Water and Drinking Water
Cindy Simbanin, Office of Ground Water and Drinking Water, Water Security Division
Steve Wendelken, Office of Ground Water and Drinking Water
• Office of Radiation and Indoor Air
George Dillbeck
John Griggs
David Musick
• Office of Solid Waste and Emergency Response
Barry Lesnik
John Nebelsick
Terry Smith
Shen-yi Yang
• Office of Environmental Information
Margo Hunt, Quality Staff
• Office of Pesticides Programs
Fred Siegelman, Biological and Economic Analysis Division
• EPA Regions
Linda Anderson-Carnahan, Region 10
Isa Chamberlain, Region 10
Joe Dorsey, Region 3
Diane Gregg, Region 6
Stephanie Harris, Region 10
Bonita Johnson, Region 4
Irwin Katz, Region 2
Peggy Knight, Region 10
Jose Negron, Region 4
Steve Reimer, Region 10
Dennis Revell, Region 4
Lavon Revells, Region 4
Dave Stockton, Region 6
Sue Warner, Region 3
Laura Webb, Region 7
Wayne Whipple, Region 5
National Laboratories
Todd Kimmell, Argonne National Laboratory
United States Centers for Disease Control and Prevention
Matthew J. Arduino, National Center for Infectious Diseases - Division of Health Quality Promotion
Cheryl Bopp, Foodborne and Diarrheal Diseases Branch
Collette Fitzgerald, Foodborne and Diarrheal Diseases Branch
Jay E. Gee, National Center for Infectious Diseases - Division of Bacterial and Mycotic Diseases
SAM Revision 2.0 ix September 29, 2005
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Martin Harper, National Institute for Occupational Safety and Health - Health Effects Laboratory
Division
Vincent Hill, National Center for Infectious Diseases - Division of Parasitic Diseases
Dennis Juranek, National Center for Infectious Diseases - Division of Parasitic Diseases
Laura J. Rose, Division of Health Quality Promotion
Lihua Xiao, National Center for Infectious Diseases - Division of Parasitic Diseases
United States Department of Homeland Security
Lance Brooks
United States Federal Bureau of Investigation
Ben Garrett, Hazard Materials Response Unit
Paul Keller, Hazard Materials Response Unit
Jarrad Wagner, Hazard Materials Response Unit
United States Food and Drug Administration
David L. Craft, Forensic Chemistry Center
United States Department of Defense
Johnathan Kiel, U.S. Air Force
Philip Koga, U.S. Army, Edgewood Chemical Biological Center
Alfredo Rayms-Keller, U.S. Navy
Dennis Reutter, U.S. Army, Edgewood Chemical Biological Center
Jose-Luis Sagripanti, U.S. Army, Edgewood Chemical Biological Center
John D. Wright, U.S. Army, Dugway Proving Ground, Life Sciences Division
United States Department of Agriculture
Ronald Payer
United States Department of Energy
Kathy Hall (on detail to EPA's National Homeland Security Research Center)
United States Geological Survey
Merle Shockey
State and Local Agencies
Mary M. Abrams, Oregon Department of Environmental Quality
Jack Bennett, State of Connecticut Department of Health
David Degenhardt, Wisconsin State Lab of Hygiene
Patrick M. Dhooge, New Mexico Department of Health, Scientific Laboratory Division
Dennis Flynn, New Jersey Department of Health and Senior Services
Rebecca Hoffman, Wisconsin State Lab of Hygiene
Edward Horn, New York Department of Health
Sharon Kluender, Wisconsin State Lab of Hygiene
Bart Koch, Metropolitan Water District of Southern California
Charles D. McGee, Orange County Sanitation District
Steve Rhode, Massachusetts Water Resources Authority
SAM Revision 2.0 x September 29, 2005
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Other
Zia Bukhari, American Water
Richard Danielson, BioVir Laboratories, Inc.
Mohammad R. Karim, American Water
Deborah A. Killeen, Lockheed Martin
Joel A. Pedersen, University of Wisconsin
E. Barry Skolnick
Caryn Wojtowicz, formerly of Ecology and Environment, Inc.
SAM Revision 2.0 xi September 29, 2005
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SAM Revision 2.0 xii September 29, 2005
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Standardized Analytical Methods for Use
During Homeland Security Events
Revision 2.0
September 29, 2005
Contents
Disclaimer ii
Use of This Document iii
Foreword iv
Abbreviations and Acronyms v
Acknowledgments viii
Section 1.0: Introduction 1
Section 2.0: Scope and Application 5
Section 3.0: Points of Contact 7
Section 4.0: Chemical Methods 9
4.1 General Guidance 9
4.1.1 Standard Operating Procedures for Identifying Chemical Methods 10
4.1.2 General Quality Control (QC) Guidance for Chemical Methods 11
4.1.3 Safety and Waste Management 12
4.2 Method Summaries 13
4.2.1 EPA CLP Method SOW ILM05.3 Cyanide: Analytical Methods for Total Cyanide
Analysis 13
4.2.2 EPA Office of Air Quality Planning and Standards (OAQPS) Method 207-2: Analysis
for Isocyanates by High Performance Liquid Chromatography (HPLC) 14
4.2.3 EPA NERL Method 365.1, Revision 2: Determination of Phosphorus by Semi-
Automated Colorimetry 14
4.2.4 EPA Method 200.8: Determination of Trace Elements in Waters and Wastes by
Inductively Coupled Plasma-Mass Spectrometry 15
4.2.5 EPA Method 245.2: Mercury (Automated Cold Vapor Technique) 15
4.2.6 EPA Method 252.2: Osmium (Atomic Absorption, Furnace Technique) 16
4.2.7 EPA Method 300.1: Determination of Inorganic Anions in Drinking Water by Ion
Chromatography 16
4.2.8 EPA Method 335.4: Determination of Total Cyanide by Semi-Automated Colorimetry
17
4.2.9 EPA Method 350.3: Nitrogen, Ammonia (Potentiometric, Ion Selective Electrode) .. 17
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4.2.10 EPA Method 508: Determination of Chlorinated Pesticides in Water by Gas
Chromatography with an Electron Capture Detector 17
4.2.11 EPA Method 524.2: Measurement of Purgeable Organic Compounds in Water by
Capillary Column Gas Chromatography / Mass Spectrometry 18
4.2.12 EPA Method 525.2: Determination of Organic Compounds in Drinking Water by Liquid-
Solid Extraction and Capillary Column Gas Chromatography / Mass Spectrometry . . 18
4.2.13 EPA Method 531.2: Measurement of N-Methylcarbamoyloximes and N-
Methylcarbamates in Water by Direct Aqueous Injection HPLC with Postcolumn
Derivatization 19
4.2.14 EPA Method 549.2: Determination of Diquat and Paraquat in Drinking Water by Liquid-
Solid Extraction and High-Performance Liquid Chromatography with Ultraviolet
Detection 19
4.2.15 EPA Method 3031 (SW-846): Acid Digestion of Oils for Metals Analysis by Atomic
Absorption or ICP Spectrometry 20
4.2.16 EPA Method 3050B (SW-846): Acid Digestion of Sediments, Sludges, and Soils ... 20
4.2.17 EPA Method 3520C (SW-846): Continuous Liquid-Liquid Extraction 21
4.2.18 EPA Method 3535A (SW-846): Solid-Phase Extraction 23
4.2.19 EPA Method 3541 (SW-846): Automated Soxhlet Extraction 25
4.2.20 EPA Method 3545A (SW-846): Pressurized Fluid Extraction (PFE) 27
4.2.21 EPA Method 3580A (SW-846): Waste Dilution 29
4.2.22 EPA Method 3585 (SW-846): Waste Dilution for Volatile Organics 31
4.2.23 EPA Method 5030C (SW-846): Purge-and-Trap for Aqueous Samples 31
4.2.24 EPA Method 5035A (SW-846): Closed-System Purge-and-Trap and Extraction for
Volatile Organics in Soil and Waste Samples 32
4.2.25 EPA Method 60IOC (SW-846): Inductively Coupled Plasma - Atomic Emission
Spectrometry 33
4.2.26 EPA Method 6020A (SW-846): Inductively Coupled Plasma - Mass Spectrometry . . 34
4.2.27 EPA Method 7010 (SW-846): Graphite Furnace Atomic Absorption Spectrophotometry
34
4.2.28 EPA Method 7470A (SW-846): Mercury in Liquid Wastes (Manual Cold-Vapor
Technique) 35
4.2.29 EPA Method 747IB (SW-846): Mercury in Solid or Semisolid Wastes (Manual Cold-
Vapor Technique) 35
4.2.30 EPA Method 8015C (SW-846): Nonhalogenated Organics Using GC/FID 35
4.2.31 EPA Method 8260B (SW-846): Volatile Organic Compounds by Gas
Chromatography/Mass Spectrometry (GC/MS) 36
4.2.32 EPA Method 8270D (SW-846): Semivolatile Organic Compounds by Gas
Chromatography/Mass Spectrometry (GC/MS) 37
4.2.33 EPA Method 8082A (SW-846): Polychlorinated Biphenyls (PCBs) by Gas
Chromatography 38
4.2.34 EPA Method 8315A (SW-846): Determination of Carbonyl Compounds by High
Performance Liquid Chromatography (HPLC) 39
4.2.35 EPA Method 8318A (SW-846): 7V-Methylcarbamates by High Performance Liquid
Chromatography (HPLC) 39
4.2.36 EPA Method 8321B (SW-846): Solvent-Extractable Nonvolatile Compounds by High
Performance Liquid Chromatography/Thermospray/Mass Spectrometry (HPLC/TS/MS)
or Ultraviolet (UV) Detection 40
4.2.37 ASTM Method D5755-03: Standard Test Method for Microvacuum Sampling and
Indirect Analysis of Dust by Transmission Electron Microscopy (TEM) for Asbestos
Structure Number Surface Loading 40
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4.2.38 ASTM Method D6480-99: Standard Test Method for Wipe Sampling of Surfaces,
Indirect Preparation, and Analysis for Asbestos Structure Number Concentration by
Transmission Electron Microscopy 41
4.2.39 ISO Method - 10312: Ambient Air - Determination of Asbestos Fibres - Direct-transfer
Transmission Electron Microscopy Method (TEM) 41
4.2.40 ISO Method - 12884: Ambient Air - Determination of Total (Gas and Particle-phase)
Polycyclic Aromatic Hydrocarbons - Collection on Sorbent-backed Filters with Gas
Chromatographic/Mass Spectrometric Analysis 42
4.2.41 ISO Method - 16000-3: Indoor Air - Part 3: Determination of Formaldehyde and Other
Carbonyl Compounds - Active Sampling Method 43
4.2.42 NIOSH Method 1402: Alcohols III 43
4.2.43 NIOSH Method 1612: Propylene Oxide 44
4.2.44 NIOSH Method 2010: Amines, Aliphatic 44
4.2.45 NIOSH Method 2513: Ethylene Chlorohydrin 44
4.2.46 NIOSHMethod 3510: Monomethylhydrazine 45
4.2.47 NIOSHMethod 6001: Arsine 45
4.2.48 NIOSH Method 6002: Phosphine 45
4.2.49 NIOSH Method 6004: Sulfur Dioxide 46
4.2.50 NIOSH Method 6010: Hydrogen Cyanide 46
4.2.51 NIOSHMethod 6011: Bromine and Chlorine 46
4.2.52 NIOSH Method 6013: Hydrogen Sulfide 47
4.2.53 NIOSH Method 6015: Ammonia 47
4.2.54 NIOSHMethod 6402: Phosphorus Trichloride 47
4.2.55 NIOSH Method 7903: Acids, Inorganic 48
4.2.56 NIOSH Method 7904: Cyanides, Aerosol and Gas 48
4.2.57 NIOSH Method 7906: Fluorides, Aerosol and Gas 49
4.2.58 NIOSHMethod S301-1: Fluoroacetate Anion 49
4.2.59 OSHA Method ID-188: Ammonia in Workplace Atmospheres - Solid Sorbent 49
4.2.60 OSHA Method ID-216SG: Boron Trifluoride (BF3) 50
4.2.61 Standard Method 4110 B: Ion Chromatography with Chemical Suppression of Eluent
Conductivity 50
4.2.62 Standard Method 4500-NH3 B: Preliminary Distillation Step 50
4.2.63 Standard Method 4500-NH3 G: Automated Phenate Method 51
4.2.64 Standard Method 4500-C1 G: DPD Colorimetric Method 51
4.2.65 IO Compendium Method IO-3.1: Selection, Preparation, and Extraction of Filter
Material 52
4.2.66 IO Compendium Method IO-3.4: Determination of Metals in Ambient Particulate Matter
Using Inductively Coupled Plasma (ICP) Spectroscopy 52
4.2.67 IO Compendium Method IO-3.5: Determination of Metals in Ambient Particulate Matter
Using Inductively Coupled Plasma/Mass Spectrometry (ICP/MS) 53
4.2.68 IO Compendium Method IO-5: Sampling and Analysis for Vapor and Particle Phase
Mercury in Ambient Air Utilizing Cold Vapor Atomic Fluorescence Spectrometry
(CVAFS) 53
4.2.69 EPA Air Method, Toxic Organics - 6 (TO-6): Method for the Determination of Phosgene
in Ambient Air Using High Performance Liquid Chromatography 54
4.2.70 EPA Air Method, Toxic Organics - 10A (TO-10A): Determination of Pesticides and
Polychlorinated Biphenyls in Ambient Air Using Low Volume Polyurethane Foam
(PUF) Sampling Followed by Gas Chromatographic/Multi-Detector Detection (GC/ MD)
54
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4.2.71 EPA Air Method, Toxic Organics - 15 (TO-15): Determination of Volatile Organic
Compounds (VOCs) in Air Collected in Specially-Prepared Canisters and Analyzed by
Gas Chromatography/Mass Spectrometry (GC/MS) 55
4.2.72 Journal of Analytical Atomic Spectrometry, 2000, 15, pp. 277-279: Boron Trichloride
Analysis 57
4.2.73 Analytical Letters, 1994, 27 (14), pp. 2703-2718: Screening-Procedure for Sodium
Fluoroacetate (Compound 1080) at Sub-Microgram/Gram Concentrations in Soils . . 57
Section 5.0: Biological Methods 59
5.1 General Guidance 60
5.1.1 Standard Operating Procedures for Identifying Biological Methods 60
5.1.2 General Quality Control (QC) Guidance for Biological Methods 61
5.1.3 Safety and Waste Management 62
5.2 Method Summaries 62
5.2.1 Laboratory Response Network (LRN) 63
5.2.2 Biosafety Level 4 Viruses 64
5.2.3 Standard Methods 9260 B: Salmonella typhi 64
5.2.4 Standard Methods 9260 E: Shigella species 65
5.2.5 Standard Methods 9260 F: PathogenicEscherichia coll 65
5.2.6 Standard Methods 9260 G: Campylobacter jejuni 66
5.2.7 Standard Methods 9260H: Vibrio cholerae 66
5.2.8 Literature Reference for Enteric Viruses (Applied and Environmental Microbiology.
69(6): 3158-3164) 67
5.2.9 Literature Reference for Noroviruses (Applied and Environmental Microbiology. 69(9):
5263-5268) 67
5.2.10 Literature Reference for Hepatitis E virus (Journal of Virological Methods. 101: 175-
188) 68
5.2.11 Literature Reference for Astroviruses (Canadian Journal of Microbiology. 50: 269-278)
69
5.2.12 Literature Reference for Togaviruses (Journal of Clinical Microbiology. 38(4): 1527-
1535) 69
5.2.13 Literature Reference for Adenoviruses (Applied and Environmental Microbiology. 71(6):
3131-3136) 70
5.2.14 Literature Reference for Coronaviruses (SARS) (Journal of Virological Methods. 122:
29-36) 70
5.2.15 EPA Method 1622: Cryptosporidium in Water by Filtration/MS/FA 71
5.2.16 Draft EPA Method 1693: Cryptosporidium andGiardia in Disinfected Wastewater and
Combined Sewer Overflows (CSOs) by Concentration/IMS/IFA 71
5.2.17 Literature References for Toxoplasma gondii (Applied and Environmental Microbiology.
70(7): 4035-4039) 72
5.2.18 Entamoeba histolytica: PCR 73
5.2.19 Literature Reference for Shiga Toxin Gene (Journal of Clinical Microbiology. 39(1):
370-374) 73
Section 6.0: Radiochemical Methods 75
6.1 General Guidance 75
6.1.1 Standard Operating Procedures for Identifying Radiochemical Methods 76
6.1.2 General Quality Control (QC) Guidance for Radiochemical Methods 77
6.1.3 Safety and Waste Management 78
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6.2 Method Summaries 79
6.2.1 EPA Method 901.1: Gamma Emitting Radionuclides in Drinking Water 79
6.2.2 EPA Method 903.0: Alpha-Emitting Radium Isotopes in Drinking Water 80
6.2.3 EPA Method 903.1: Radium-226 in Drinking Water - Radon Emanation Technique . 80
6.2.4 EPA Method 905.0: Radioactive Strontium in Drinking Water 81
6.2.5 EPA Method 908.0: Uranium in Drinking Water - Radiochemical Method 81
6.2.6 EPA Method EMSL-19: Determination of Radium-226 and Radium-228 in Water, Soil,
Air and Biological Tissue 82
6.2.7 EPA Method EMSL-33: Isotopic Determination of Plutonium, Uranium, and Thorium in
Water, Soil, Air, and Biological Tissue 82
6.2.8 ASTM Method D3084: Standard Practice for Alpha Spectrometry in Water 83
6.2.9 ASTM Method D3972: Standard Test Method for Isotopic Uranium in Water by
Radiochemistry 83
6.2.10 U.S. DHS EML Method Am-01-RC: Americiumin Soil 84
6.2.11 U.S. DHS EML Method Am-02-RC: Americium-241 in Soil-Gamma Spectrometry . 84
6.2.12 U.S. DHS EML Method Am-04-RC: Americium in QAP Water and Air Filters -
Eichrom's TRU Resin 85
6.2.13 U.S. DHS EML Method Ga-01-R: Gamma Radioassay 85
6.2.14 U.S. DHS EML Method Sr-03-RC: Strontium-90 in Environmental Samples 86
6.2.15 Standard Method 7120: Gamma-Emitting Radionuclides 86
6.2.16 Standard Method 7500-Ra B: Radium: Precipitation Method 87
6.2.17 Standard Method 7500-Ra C: Radium: Emanation Method 87
6.2.18 Standard Method 7500-Sr B: Total Radioactive Strontium and Strontium-90:
Precipitation Method 88
6.2.19 Standard Method 7500-U B: Uranium: Radiochemical Method 88
6.2.20 Standard Method 7500-U C: Uranium: Isotopic Method 89
Section 7.0: Biotoxin Methods 91
7.1 General Guidance 91
7.1.1 Standard Operating Procedures for Identifying Biotoxin Methods 92
7.1.2 General Quality Control (QC) Guidance for Biotoxin Methods 93
7.1.3 Safety and Waste Management 94
7.2 Method Summaries 94
7.2.1 Laboratory Response Network (LRN) 95
7.2.2 AOAC Official Method 994.08: Aflatoxin in Corn, Almonds, Brazil Nuts, Peanuts, and
Pistachio Nuts 96
7.2.3 Shiga Toxin Genes (StX; Stx2) 96
7.2.4 Staphyloccocal Enterotoxin (Method to be determined) 96
Section 8.0: Conclusions 97
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Appendices
Appendix A: Chemical Methods A-l
Appendix B: Biological Methods
B-l Waterborne Biological Methods B-l - 1
B-2 Dustborne Biological Methods B-2 - 1
B-3 Aerosol Biological Methods B-3 - 1
Appendix C: Radiochemical Methods C-l
Appendix D: Biotoxin Methods D-l
Figures
1-1. Analytical Response Roadmap for Homeland Security Events 2
SAM Revision 2.0 xviii September 29, 2005
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Section 1.0: Introduction
In the aftermath of the terrorist attacks of September 11, 2001, and the anthrax attacks in the Fall of
2001, Federal and State personnel successfully carried out their mission to provide response, recovery,
and remediation under trying circumstances, including an unprecedented demand on their capabilities to
analyze environmental samples. In reviewing these incidents, the Environmental Protection Agency's
(EPA) 9/77 Lessons Learned and its Anthrax Lessons Learned1 reports identified several areas where the
country could better prepare itself in the event of future terrorist incidents. One of the most important
areas identified was the need to improve the nation's laboratory capacity and capability to respond to
incidents requiring the analysis of large numbers of environmental samples in a short time.
In response, EPA formed the Homeland Security Laboratory Capacity Workgroup to identify and
implement opportunities for near-term improvements and to develop recommendations for addressing
longer-term, cross-cutting laboratory issues. The EPA Homeland Security Laboratory Capacity
Workgroup consists of representatives from the Office of Research and Development, Office of
Radiation and Indoor Air, Office of Water, Office of Solid Waste and Emergency Response, Office of
Environmental Information, Office of Pesticide Programs, and several EPA Regional Offices.
A critical area identified by the workgroup was the need for a list of standardized analytical methods to
be used by all laboratories when analyzing homeland security incident samples. Having standardized
methods would reduce confusion, permit sharing of sample load between laboratories, improve data
comparability, simplify the task of outsourcing analytical support to the commercial laboratory sector,
and improve the follow-up activities of validating results, evaluating data and making decisions. To this
end, workgroup members formed an Analytical Methods Subteam to address homeland security methods
issues.
The Analytical Methods Subteam recognized that widely different needs for analytical methods could be
required for various analytical activities that will be performed, including (1) constant monitoring and
surveillance to determine if a terrorist event has occurred, (2) rapid screening for determining the
presence of agents or contaminants of concern, (3) screening for identification of agents or contaminants
used in an event, and (4) quantitation of the amount or levels of agents or contaminants identified for
extent of contamination and the efficacy of decontamination determinations.
Figure 1 -1 represents the analytical decision tree for responding to homeland security incidents.
'U.S. EPA internal report: Lessons Learned in the Aftermath of September 11, 2001 (February 2002).
2U.S. EPA internal report: Challenges Faced During the Environmental Protection Agency's Response to
Anthrax and Recommendations for Enhancing Response Capabilities: A Lessons Learned Report (September 2002).
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Figure 1-1. Analytical Response Roadmap for Homeland Security Events
Hazards Screening
Preliminary
Identification
Confirmatory
Identification - Quantification
T>i>e or ;:,IMifJes include:
Risk .'issessment
Remediation
Clem Mice
~i
The "Confirmatory" phase of environmental samp/e analysis in
response to a home/and securty event is discussed within this
document. Other phases witlbe addressed in a separate document.
During 2004, the Analytical Methods Subteam recognized that selection of standardized analytical
methods is dependent on the intended application, and focused on selection of a single preferred
confirmatory method per each individual analyte/matrix for use in assessing the extent of contamination
and the efficacy of decontamination (e.g., identification and quantification of contaminants). A survey of
available confirmatory analytical methods for approximately 120 biological and chemical analytes was
conducted using existing resources including the following:
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• National Environmental Methods Index (NEMI) and NEMI-Chemical, Biological, and
Radiological (NEMI-CBR)3
• Environmental Monitoring Method Index (EMMI)
• EPA Test Methods Index
EPA Office of Solid Waste SW-846 Methods On-line
• EPA Microbiology Methods
• National Institute for Occupational Safety and Health (NIOSH) method index
• Occupational Safety and Health Administration (OSHA) method index
• AOAC International
• ASTM International
• International Organization for Standardization (ISO) methods
• Standard Methods for the Examination of Water and Wastewater
• PubMED Literature Database
In 2004, EPA's National Homeland Security Research Center brought together experts from across EPA
and its sister agencies to develop a compendium of analytical methods to be used when responding to
future incidents. Participants included representatives from U.S. EPA program offices, EPA regions,
EPA national laboratories, Centers for Disease Control and Prevention (CDC), Food and Drug
Administration (FDA), Department of Homeland Security (DHS), Federal Bureau of Investigation (FBI),
Department of Defense (DoD), Department of Agriculture (USD A), and U.S. Geological Survey (USGS).
Methodologies were considered for both chemical and biological agents of concern in the types of
environmental sample matrices that were anticipated for analysis in homeland security incidents. The
primary objective of this effort was to identify appropriate SAM Analytical Methods Subteam consensus
methods that represent a balance between existing determinative techniques and methodologies and
providing consistent analytical results.
In September 2004, EPA published Standardized Analytical Methods for Use During Homeland Security
Events, Revision 1.0 (EPA/600/R-04/126), SAM. This document provided a list of analytical and sample
preparation methods that were selected for measurement of 82 chemical analytes in aqueous/liquid, solid,
oily solid, and air matrices, and 27 biological analytes in water, dust, and aerosol matrices.
During 2005, SAM was expanded to include several persistent chemical warfare agent degradation
products and radioisotopes, a drinking water matrix, methods for determination of the viability of
biological organisms, and a separate section for biotoxin analytes. Where necessary, the methods
included in SAM Revision 1.0 were updated to reflect more recent or appropriate methodologies.
Similar efforts to those used for method selection during development of SAM Revision 1.0 were
undertaken to select and include methods for measurement of radioisotopes and chemical warfare agent
degradation products in all matrices, for measurement of chemical, biological, and radiochemical
analytes in drinking water, and to determine the viability of biological organisms. These additional
analytes and the corresponding methods selected are included in SAM Revision 2.0.
3NEMI-CBR is being developed by the U.S. EPA Office of Water's Water Security Division to provide a
central system for locating, evaluating, comparing, and retrieving analytical methods for rapid and effective analysis
of environmental samples. NEMI-CBR displays and summarizes multiple screening and confirmatory methods for
contaminants that may be associated with terrorist attacks, and is scheduled for release in December 2005.
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Section 2.0: Scope and Application
The purpose of this document is to identify and briefly describe the specific methodologies that EPA and
its contracted laboratories will employ when called upon to analyze environmental samples in times of
national emergency. The document also is intended as a tool that will be available to assist State and
local laboratories in responding to homeland security events. The methodologies presented in this
document should be used to:
• Evaluate the nature and extent of contamination
Evaluate the effectiveness of decontamination
Methods are provided as corresponding to specific analyte/matrix pairs that are listed in Appendices A
(chemical), B (biological), C (radiochemical), and D (biotoxin). Summaries of each method are provided
in numerical order by developing agency, throughout Sections 4.2 (chemical), 5.2 (biological), 6.2
(radiochemical), and 7.2 (biotoxin).
The list of methods provided is limited to those methods that would be used to determine, to the extent
possible within analytical limitations, the presence of chemical, biological, radiochemical, and biotoxin
analytes of concern and to determine their concentrations in environmental media. The methods are not
designed to be used for conducting an initial evaluation (triage or screening) of suspected material to
determine if it poses an immediate danger or if it needs to be analyzed in specially designed, highly
secure facilities. Methods for addressing these needs are and will be the subject of other efforts. It is
hoped that this document will assist Federal, State and local governments in preparing for future
emergencies.
It is important to note that, in some cases, the methods included in this document have not been
verified for the analyte/matrix combination(s) for which they have been selected. The information
contained in this document represents the latest step in an ongoing National Homeland Security
Research Center effort to provide standardized analytical methods for use by laboratories tasked
with performing analyses in response to a homeland security event. Although at this time, many of
the methods listed have not been tested for a particular analyte (e.g., analytes not explicitly
identified in the method) or matrix, the methods are considered to contain the most appropriate
currently available techniques. Unless a published method that is listed in this document states
specific applicability to the analyte/matrix pair for which it has been selected, it should be assumed
that method testing is needed. In these cases, adjustment may be required to accurately account for
variations in environmental matrices, analyte characteristics, and target risk levels. Many of the
target analytes listed in this document have only recently become an environmental concern, and
EPA is actively pursuing development and validation of Standard Analytical Protocols (SAPs)
based on the methods listed, including optimization of procedures for measuring target compounds.
In those cases where method procedures are determined to be insufficient for a particular situation,
EPA will provide guidance regarding appropriate actions. This will be an ongoing process as EPA
will strive to establish a consistent level of validation for all listed analytes.
EPA is developing and validating Standardized Analytical Protocols (SAPs) based on the methods that
are listed in this document, where further development and verification are necessary. Once validation is
complete, data regarding specific method performance and data quality objectives will be available. The
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SAM document and corresponding SAPs will be reviewed frequently. EPA plans to continue to update
the SAM document periodically to address the needs of homeland security, reflect improvements in
analytical methodology and new technologies, and incorporate changes in analytes based on needs. The
Agency also anticipates that addendums may be generated to provide guidance regarding issues that
currently are not addressed by this document. Any deviations from the methods referenced in this
document should be coordinated with the appropriate point(s) of contact identified in Section 3.
Having data of known and documented quality is critical for public officials to accurately assess the
activities that may be needed in responding to emergency situations. Quality control (QC) pertains to
both sample collection and analysis. Data must be of sufficient quality to support decision making.
Quality control, however, takes time and time is often critical in emergency response activities, where
there will be tremendous pressure to conduct sampling and analytical operations quickly and efficiently.
While reduced levels of QC might be tolerated during the rapid screening stage of emergency response,
implementation of analytical methods for risk assessment and site release will require a higher and more
appropriate level of QC. Many of the methods listed in this document include QC requirements for
collecting and analyzing samples. These QC requirements may or may not be appropriate for addressing
emergency response situations, and may be adjusted as necessary to maximize data and decision quality.
Specific QC recommendations for analysis of samples for chemical, biological, radiochemical, and
biotoxin analytes are provided in each corresponding section of this document (i.e., Sections 4.1.2, 5.1.2,
6.1.2, and 7.1.2, respectively).
Participants in the biological, chemical, and radiochemistry work groups, including representatives from
the U.S. EPA, CDC, FDA, DHS, FBI, DoD, USDA, and USGS evaluated the suitability of existing
methodologies and selected this set of methods for use by EPA laboratories and contract laboratories if
called upon to respond to an emergency. The Agency recognizes that this advanced selection of such
methods may pose potential risks, including the following:
• Selecting technologies that may not be the most cost-effective technologies currently available for
addressing the particular situation at hand
Selecting methodologies that may not be appropriate for use in responding to a particular
emergency because the Agency did not anticipate having to analyze for a particular analyte or
analyte/matrix combination
Preventing development and adoption of new and better measurement technologies
To address these potential risks as soon as possible, the Agency plans to take several steps. These
include the following:
• Developing and specifying measurement quality objectives (i.e., required minimum standards of
accuracy (bias and precision) and sensitivity for the analysis of samples that support the data
quality needs of the particular stage of the emergency response/recovery process) for all
analyte/matrix combinations listed in this document
• Specifying minimum measurement system verification (e.g., ASTM Standard D6956-03) and
documentation standards for homeland security analyses
• Working with other government agencies and the private sector to establish a laboratory
accreditation system to ensure that laboratories selected to assist the Agency and its Federal, State,
and local partners in responding to homeland security incidents have the requisite expertise and
systems to perform this type of testing
Continue working with multiple agencies and stakeholders to periodically update SAM and
supporting documents
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Section 3.0: Points of Contact
Questions concerning this document, or the methods identified in this document, should be addressed to
the appropriate point(s) of contact identified below. As previously indicated, any deviations from the
recommended method(s) should be reported immediately to ensure data comparability is maintained
when responding to homeland security events. The appropriate point(s) of contact identified below
should be consulted regarding any deviations.
General
Oba Vincent - Primary
National Homeland Security Research Center
U.S. EPA Office of Research and Development
(163)
26 West Martin Luther King Jr. Drive
Cincinnati, OH 45268
(513)569-7456
vincent.oba@epa.gov
Rob Rothman -Alternate
National Homeland Security Research Center
U.S. EPA Office of Research and Development
(163)
26 West Martin Luther King Jr. Drive
Cincinnati, OH 45268
(513)569-7187
rothman.rob@epa.gov
Biological Methods
Alan Lindquist - Primary
National Homeland Security Research Center
U.S. EPA Office of Research and Development
(163)
26 West Martin Luther King Jr. Drive
Cincinnati, OH 45268
(513)569-7192
lindquist.alan@epa.gov
Ann Grimm -Alternate
National Exposure Research Laboratory
U.S. EPA Office of Research and Development
(320)
26 West Martin Luther King Jr. Drive
Cincinnati, OH 45268
(513)569-7397
grimm.ann@epa.gov
Chemical Methods
Michael S. Johnson -Primary
Office of Solid Waste and Emergency Response
(5204G)
U.S. EPA Headquarters Ariel Rios Building
1200 Pennsylvania Avenue, NW
Washington, DC 20460
(703) 603-0266
iohnson.michaels@epa.gov
Matthew Magnuson - Alternate
National Homeland Security Research Center
U.S. EPA Office of Research and Development
(681)
26 West Martin Luther King Jr. Drive
Cincinnati, OH 45268
(513)569-7321
magnuson.matthew@epa.gov
Radiochemical Methods
John Griggs - Primary
U.S. EPA Office of Radiation and Indoor Air
Environmental Laboratory / OAR
540 South Morris Avenue
Montgomery, AL 36115-2601
(334) 270-3450
griggs.john@epa.gov
David Musick - Alternate
U.S. EPA Office of Radiation and Indoor Air
P.O. Box 98517
Las Vegas, NV 89193-8517
(702) 798-2104
musick.david@epa.gov
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Biotoxins Methods
Gerard Stelma - Primary
U.S. EPA Office of Research and Development
26 West Martin Luther King Jr. Drive
Cincinnati, OH 45268
(513)569-7384
stelma.gerard@epa.mail
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Section 4.0: Chemical Methods
A list of analytical methods to be used in analyzing environmental samples for chemical contaminants
during homeland security events is provided in Appendix A. Methods are listed for each analyte and for
each sample matrix that potentially may need to be measured and analyzed when responding to an
environmental emergency. Protocols from peer reviewed journal articles have been identified for
analyte-matrix pairs where standardized methods are not available, and it should be noted that the
limitations of these protocols differ from the limitations of the standardized methods identified. Once
standard procedures are available, the literature references will be replaced.
The methods table in Appendix A is sorted alphabetically by analyte and includes the following
information:
• Analyte(s). The compound or compound(s) of interest.
• Chemical Abstract Survey Registration Number (CAS RN). A unique identifier for chemical
substances that provides an unambiguous way to identify a chemical or molecular structure when
there are many possible systematic, generic, or trivial names.
Determinative technique. An analytical instrument or technique used to determine the quantity and
identification of compounds or components in a sample.
• Determinative method. An analytical method or procedure used to determine the quantity and
identification of compounds or components in a sample.
• Determinative method identifier. The unique identifier or number assigned to an analytical
method by the method publisher.
• Solid sample preparation procedure. The recommended method/procedure for sample preparation
to measure the analyte of interest in solid phase samples.
• Oily solid sample preparation procedure. The recommended method/procedure for sample
preparation to measure the analyte of interest in oily phase samples.
• Aqueous/Liquid sample preparation procedure. The recommended method/procedure for sample
preparation to measure the analyte of interest in aqueous and/or liquid phase samples.
Drinking water sample preparation procedure. The recommended method/procedure for sample
preparation to measure the analyte of interest in drinking water samples.
Air sample preparation procedure. The recommended method/procedure for sample preparation
and analysis to measure the analyte of interest in air samples.
4.1 General Guidance
The guidance summarized in this section provides a general overview of how to identify the appropriate
chemical method(s) for a given analyte-matrix combination as well as recommendations for quality
control procedures.
For additional information on the properties of the chemicals listed in Appendix A, TOXNET
(http://toxnet .nlm.nih.gov/index.html). a cluster of databases on toxicology, hazardous chemicals, and
related areas maintained by the National Library of Medicine, is an excellent resource.
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Additional resources include:
• Syracuse Research Corporation's Physprop and Chemfate, part of the Environmental Fate Database
supported by EPA. http://www.svrres.com/esc/databases.htm
• INCHEM at http://www.inchem.org/ contains both chemical and toxicity information.
• The RTECS database can be accessed via the NIOSH Web site at
http://www.cdc.gov/niosh/rtecs/vz72d288.htmltfJWIDAW for toxicity information.
EPA's Integrated Risk Information System (IRIS): http://www.epa.gov/iris/ contains toxicity
information.
• The Forensic Science and Communications Journal published by the Laboratory Division of the
Federal Bureau of Investigation, http://www.fbi.gov/hq/lab/fsc/current/backissu.htm.
Additional research on chemical contaminants is ongoing within EPA, and databases to manage this
information are currently under development.
4.1.1 Standard Operating Procedures for Identifying Chemical Methods
Determine the appropriate method and sample preparation technique that is to be used on the
environmental samples by locating the analyte of concern in Appendix A: Chemical Methods under the
"Analyte" column. After locating the analyte of concern, continue across the table to identify the
determinative technique and determinative method identifier for that particular compound. Determine
the sample preparation technique by selecting the appropriate matrix column (Solid, Oily Solid,
Aqueous/Liquid, Drinking Water, or Air) for that particular analyte.
Sections 4.2.1 through 4.2.73 below provide summaries of the determinative and sample preparation
methods listed in Appendix A. Where available, a direct link to the full text of the selected analytical
method is provided in the method summary. For additional information on preparation procedures and
methods available through consensus standards organizations, please use the contact information
provided in Table 1.
Table 1. Sources of Chemical Methods
Name
National Environmental Methods Index
(NEMI)
U.S. EPA Office of Water (OW)
Methods
U.S. EPA SW-846 Methods
U.S. EPA Office of Research and
Development Methods
U.S. EPA Air Toxics Methods
Occupational Safety and Health
Administration Methods
National Institutes for Occupational
Safety and Health Methods
Publisher
EPA, USGS
EPA Office of Water
EPA Office of Solid Waste
EPA Office of Research and
Development
EPA Office of Air and
Radiation
OSHA
NIOSH
Reference
http://wvwv.nemi.qov
http://www.epa.qov/safewater/methods/
sourcalt.html
http://www.epa.qov/epaoswer/hazwaste
/test/main, htm
http://www.epa.qov/nerlcwww/ordmeth.
htm
http://www.epa.qov/ttn/amtic/airtox.html
http://www.osha-slc.qov/dts/sltc/method
s/toc.html
http://www.cdc.qov/niosh/nmam/
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Name
Standard Methods for the Examination
of Water and Wastewater, 20th Edition,
1998*
Annual Book of ASTM Standards*
International Organization for
Standardization Methods*
Official Methods of Analysis of AOAC
International*
Publisher
American Public Health
Association (APHA),
American Water Works
Association (AWWA), and
Water Environment
Federation (WEF)
ASTM International
ISO
AOAC International
Reference
http://wvwv.standardmethods.orq
http://www.astm.orq
http://www.iso.orq
http://www.aoac.orq
' Subscription and/or purchase required.
4.1.2 General Quality Control (QC) Guidance for Chemical Methods
The level or amount of quality control (QC) needed during sample analysis and reporting depends on the
intended purpose of the data that are generated (i.e., the decision(s) to be made). The specific decisions
that will be made should be identified, and quality objectives (including QC requirements) should be
derived based on those decisions. In establishing the appropriate level of QC, activities should be
focused on specific elements needed to support decision making.
Having analytical data of appropriate quality requires that laboratories: (1) conduct the necessary QC to
ensure that measurement systems are in control and operating properly, (2) properly document results of
the analyses, and (3) properly document measurement system evaluation of the analysis-specific QC,
including corrective actions. In emergency response situations, however, speed and efficiency are also
important. Laboratories must be prepared with calibrated instruments, the proper standards,
method-specific standard analytical procedures, and qualified and trained technicians. Laboratories also
must be capable of providing rapid turnaround of sample analyses and data reporting.
A minimum set of analytical QC procedures should be planned and conducted for all chemical testing.
Method-specific QC requirements are described in many of the individual methods that are cited in this
manual and will be referenced in any standardized analytical protocols developed to address specific
analytes and matrices of concern. Individual methods, analysis protocols, or contractual statements of
work also should be consulted to determine any additional QC that may be needed. Analytical QC
requirements generally consist of analysis of laboratory control samples to document whether the
analytical system is in control, matrix spikes to identify and quantify measurement system accuracy for
the media of concern and at the levels of concern, various blanks as a measure of freedom from
contamination, and matrix spike duplicates (MSB) or sample replicates to assess data precision.
In general, for measurement of chemical analytes, appropriate QC includes an initial demonstration of
measurement system capability as well as ongoing analysis of standards and other samples to ensure the
continued reliability of the analytical results. Examples of appropriate quality control includes:
• Demonstration that measurement system is operating properly
*• Initial calibration
•• Method blanks
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Demonstration of analytical method suitability for intended use
•• Detection and quantitation limits
*• Precision and recovery (verify measurement system has adequate accuracy)
*• Analyte/matrix/level of concern-specific QC samples (verify that measurement system has
adequate sensitivity at levels of concern)
Demonstration of continued analytical method reliability
•• Matrix spike/matrix spike duplicates (recovery and precision)
•• QC samples (system accuracy and sensitivity at levels of concern)
•• Surrogate spikes (where appropriate)
•• Continuing calibration verification
»• Method blanks
QC tests should be run as frequently as necessary to ensure the reliability of analytical results. As with
the identification of needed QC samples, frequency should be established based on an evaluation of data
quality objectives. The type and frequency of QC can be focused over time. For example, as
measurements become routine and the sources of analytical variability understood, the frequency of some
types of QC samples (matrix spikes and matrix spike duplicates) or protocols (calibration checks, etc.)
may be reduced without affecting analytical data quality.
Ensuring data quality also requires that laboratory results are properly evaluated and the results of the
data quality evaluation are transmitted to decision makers. This evaluation is as important as the data in
ensuring informed and effective decisions. While some degree of data evaluation is necessary in order to
be able to confirm data quality, 100% verification and/or validation is neither necessary nor conducive to
efficient decision making in emergency response situations. The level of such reviews should be
determined based on the specific situation being assessed and on the corresponding data quality
objectives. In every case, the levels of QC and data review necessary to support decision making should
be determined as much in advance of data collection as possible.
Please note: The appropriate point of contact identified in Section 3 should be consulted regarding
appropriate quality assurance and quality control (QA/QC) procedures prior to sample analysis. These
contacts will consult with their respective QA/QC managers regarding QA/QC issues.
4.1.3 Safety and Waste Management
It is imperative that safety precautions are used during collection, processing, and analysis of
environmental samples, particularly in emergency response situations that may include unknown hazards.
Laboratories should have a documented health and safety plan for handling samples that may contain the
target chemical, biological, or radiological contaminants, and laboratory staff should be trained in and
implement the safety procedures included in the plan. In addition, many of the methods summarized or
cited in Section 4.2 contain some specific requirements, guidance, or information regarding safety
precautions that should be followed when handling or processing environmental samples and reagents.
These methods also provide information regarding waste management.
Other resources that can be consulted for additional information include the following:
• Occupational Health and Safety Administration's (OSHA) standard for Occupational Exposure to
Hazardous Chemicals in Laboratories (29 CFR 1910.1450)
• OSHA regulations for hazardous waste operations and emergency response (29 CFR 1910)
• Environmental Protection Agency's standards regulating hazardous waste (40 CFR parts 260 - 270)
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U.S. Department of Transportation (DOT) regulations for transporting hazardous materials (49 CFR
Part 172)
U.S. Department of Health and Human Services, Centers for Disease Control and Prevention's
requirements for possession, use, and transfer of select agents and toxins (42 CFR Part 1003)
4.2 Method Summaries
Method summaries for the analytical methods listed in Appendix A, including methods for sample
preparation and determinative techniques, are provided in Sections 4.2.1 through 4.2.73. Information
provided in these sections contains summary information only, extracted from the selected methods. The
full version of the method needs to be consulted prior to sample analysis.
Each method summary contains a table identifying the contaminants in Appendix A to which the method
applies, a brief description of the analytical method, and a link to the full version of the method or source
for obtaining a full version of the method.
Please note: Not all methods have been verified for the analyte/matrix combination listed in Appendix A.
Please refer to the specified method to identify analyte/matrix combinations that have been verified. Any
questions regarding information discussed in this section should be addressed to the appropriate
contact(s) listed in Section 3.
4.2.1 EPA CLP Method SOW ILM05.3 Cyanide: Analytical Methods for Total Cyanide
Analysis
This method should be used for preparation and analysis of solid and aqueous/liquid samples for the
contaminant identified below and listed in Appendix A.
Contaminant
Cyanide
CASRN
57-12-5
The method allows for either large volume (500-mL aqueous/liquid samples or 1-g to 5-g solid samples
mixed with 500 mL of reagent water) or medium volume (50-mL aqueous/liquid samples, or 1-g solid
samples mixed with 50 mL of reagent water) sample preparation. Aqueous/liquid samples are tested for
sulfides and oxidizing agents prior to preparation. Sulfides are removed with cadmium carbonate or lead
carbonate. Samples are treated with sulfuric acid and magnesium chloride and distilled into a sodium
hydroxide solution. The solution is treated with color agents and the cyanide determined as an ion
complex by visible spectrophotometry. The method quantitation limits are 10 (ig/L or 2.5 mg/kg.
Surfactants may interfere with the distillation procedure.
Source: http://www.epa.gov/superfund/programs/clp/download/ilm/ilm53d.pdf
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4.2.2 EPA Office of Air Quality Planning and Standards (OAQPS) Method 207-2:
Analysis for Isocyanates by High Performance Liquid Chromatography (HPLC)
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Methyl isocyanate
CASRN
624-83-9
Samples are withdrawn from an emission source at an isokinetic sampling rate and collected in a
multicomponent sampling train that includes a heated probe, three impingers containing the derivatizing
reagent in toluene, an empty impinger, an impinger containing charcoal, and an impinger containing
silica gel. The impinger contents are concentrated to dryness under a vacuum, brought to volume with
acetonitrile, and analyzed with a high pressure liquid chromatograph (HPLC). Known interferences
come from a derivatizing agent, l-(2-pyridyl)piperazine. The detection limit for methyl isocyanate is 228
ng/m3.
Source: http://www.epa.gov/ttn/emc/proposed/m-207.pdf
4.2.3 EPA NERL Method 365.1, Revision 2: Determination of Phosphorus by Semi-
Automated Colorimetry
This method should be used for preparation and analysis of aqueous/liquid and drinking water samples
for the contaminant identified below and listed in Appendix A.
Contaminant
Red Phosphorus
CASRN
7723-14-0
This method measures all forms of phosphorus present in the sample, converting them to orthophosphate.
The analyte is determined as a reduced antimony-phospho-molybdate complex. A 50-mL sample is
digested with sulfuric acid and ammonium persulfate. The digestate is analyzed by automated
spectrophotometry (colorimetry) in which the sample reacts with color agents. The range of the method
is 0.01 to 1.0 mg P/L. Silica, arsenate, nitrite, and sulfide may cause interference.
Source: http://webl.er.usgs.gov/nemi/method summary.!sp?param method id=4823
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4.2.4 EPA Method 200.8: Determination of Trace Elements in Waters and Wastes by
Inductively Coupled Plasma-Mass Spectrometry
This method should be used for preparation and am
for the contaminants identified below and listed in A
Contaminant
Arsenic III compound
Arsenic trichloride (analyze for Arsenic)
Arsine
Cadmium
Metals, NOS *
dysis of aqueous/liquid and drinking water samples
ppendix A.
CASRN
22569-72-8
7784-34-1
7784-42-1
7440-43-9
NA
* NOS = Not otherwise specified
This method will determine arsine, arsenic (III) compounds, and arsenic trichloride as arsenic. An
aliquot of a well mixed, homogeneous sample is accurately weighed or measured for sample processing.
For total recoverable analysis of a sample containing undissolved material, analytes are first solubilized
by gentle refluxing with nitric and hydrochloric acids. After cooling, the sample is made up to volume,
mixed, and centrifuged or allowed to settle overnight prior to analysis. For determination of dissolved
analytes in a filtered aqueous sample aliquot, or for the "direct analysis" total recoverable determination
of analytes in drinking water where sample turbidity is < 1 NTU, the sample is made ready for analysis
by the appropriate addition of nitric acid, and then diluted to a predetermined volume and mixed before
analysis. The prepared sample is analyzed using Inductively Coupled Plasma-Mass Spectrometry (ICP-
MS).
Source: http://webl.er.usgs.gov/nemi/method summary.isp?param method id=4665
4.2.5 EPA Method 245.2: Mercury (Automated Cold Vapor Technique)
This method should be used for preparation and analysis of drinking water samples for the contaminant
identified below and listed in Appendix A.
Contaminant
Mercury
CASRN
7439-97-6
If dissolved mercury is desired, the sample is filtered. To detect total mercury (inorganic and organic
mercury), the sample is treated with potassium permanganate and potassium persulfate to oxidize organic
mercury compounds prior to analysis. Inorganic mercury is reduced to the elemental state (using tin
sulfate or tin chloride) and aerated from solution. The mercury vapor passes through a cell positioned in
the light path of a cold vapor atomic absorption (CVAA) spectrophotometer. The concentration of
mercury is measured using the CVAA spectrophotometer. Applicable concentration range is 0.2 - 20.0
jig/L.
Source: http://webl.er.usgs.gov/nemi/method summary.jsp?param method id=4822
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4.2.6 EPA Method 252.2: Osmium (Atomic Absorption, Furnace Technique)
This method should be used for the preparation and analysis of aqueous/liquid and drinking water
samples for the contaminant identified below and listed in Appendix A.
Contaminant
Osmium tetraoxide
CASRN
20816-12-0
This method will determine osmium tetraoxide as osmium. Samples are prepared according to Section
4.1 of EPA Method 200.0 (Metals: Atomic Absorption Methods) based on type of data desired (i.e.,
dissolved, suspended, total, or total recoverable). If only dissolved osmium is determined, the sample
should be filtered before acidification with nitric acid. For total osmium, the sample is digested with
nitric and hydrochloric acid and made up to volume. Samples are analyzed according to Section 9.3
"Furnace Procedure" of EPA Method 200.0, using a graphite furnace atomic absorption spectrometer. A
representative aliquot of sample is placed in the graphite tube in the furnace, evaporated to dryness,
chaffed, and atomized. Radiation from an excited element is passed through the vapor containing ground
state atoms of the element. The intensity of the transmitted radiation decreases in proportion to the
amount of the ground state element in the vapor. A monochromator isolates the characteristic radiation
from the hollow cathode lamp and a photosensitive device measures the attenuated transmitted radiation.
Optimal applicable concentration range is 50 - 500 (ig/L.
Source: http://webl.er.usgs.gov/nemi/method summary.isp?param method id=5299
4.2.7 EPA Method 300.1: Determination of Inorganic Anions in Drinking Water by Ion
Chromatography
This method should be used for the preparation and analysis of aqueous/liquid and drinking water
samples for the contaminant identified below and listed in Appendix A.
Contaminant
Fluoroacetate Salts
CASRN
NA
A small volume of an aqueous/liquid sample (10 \\L or 50 \\L) is introduced into an ion chromatograph.
The volume selected depends on the concentration of fluoroacetate ion in the sample. The anions of
interest are separated and measured, using a system comprising a guard column, analytical column,
suppressor device, and conductivity detector. The separator columns and guard columns, as well as
eluent conditions, are identical. To achieve comparable detection limits, an ion chromatographic system
must use suppressed conductivity detection, be properly maintained, and be capable of yielding a
baseline with no more than 5 nS noise/drift per minute of monitored response over the background
conductivity. The method detection limit varies depending upon the nature of the sample and the specific
instrumentation employed. The estimated calibration range is approximately 2 orders of magnitude.
Source: http://webl.er.usgs.gov/nemi/method summary.isp?param method id=4674
SAM Revision 2.0 16 September 29, 2005
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4.2.8 EPA Method 335.4: Determination of Total Cyanide by Semi-Automated
Colorimetry
This method should be used for preparation and analysis of drinking water samples for the contaminant
identified below and listed in Appendix A.
Contaminant
Cyanide
CASRN
57-12-5
Cyanide is released from cyanide complexes as hydrocyanic acid by means of a manual reflux-distillation
operation and absorbed in a scrubber containing sodium hydroxide solution. The cyanide ion in the
absorbing solution is converted to cyanogen chloride by reactions with chloramine-T, which
subsequently reacts with pyridine and barbituric acid to give a red-colored complex. Some interferences,
such as aldehydes, nitrate-nitrite, oxidizing agents, thiocyanate, thiosulfate, and sulfide, are eliminated or
reduced by distillation. The applicable range is 5 to 500 (ig/L.
Source: http://webl.er.usgs.gov/nemi/method summary.isp?param method id=5759
4.2.9 EPA Method 350.3: Nitrogen, Ammonia (Potentiometric, Ion Selective Electrode)
This method should be used for preparation and analysis of drinking water samples for the contaminant
identified below and listed in Appendix A.
Contaminant
Ammonia
CASRN
7664-41-7
Ammonia is determined potentiometrically using an ion selective ammonia electrode and a pH meter
having an expanded millivolt scale or a specific ion meter. The ammonia electrode uses a hydrophobic
gas-permeable membrane to separate the sample solution from an ammonium chloride internal solution.
Ammonia in the sample diffuses through the membrane and alters the pH of the internal solution, which
is sensed by a pH electrode. The constant level of chloride in the internal solution is sensed by a chloride
selective ion electrode which acts as the reference electrode. This method covers a range of 0.03 to 1400
mg NH3-N/L.
Source: http://webl.er.usgs.gov/nemi/method summary.jsp?param method id=4871
4.2.10 EPA Method 508: Determination of Chlorinated Pesticides in Water by Gas
Chromatography with an Electron Capture Detector
This method should be used for preparation and analysis of drinking water samples for the contaminant
identified below and listed in Appendix A.
Contaminant
Polychlorinated biphenyls (PCBs)
CASRN
1 336-36-3
A measured volume of sample is extracted with methylene chloride by shaking in a separatory funnel or
mechanical tumbling in a bottle. The methylene chloride extract is isolated, dried and concentrated after
solvent substitution with methyl tert-butyl ether. The concentration of pesticides in the extract are
SAM Revision 2.0 17 September 29, 2005
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measured using a capillary column gas chromatography (GC) system equipped with an electron capture
detector (BCD). This method has been validated in a single laboratory. Resulting estimated detection
limits (EDLs) and method detection limits (MDLs) differ depending on the congener.
Source: http://webl.er.usgs.gov/nemi/method summary.isp?param method id=4826
4.2.11 EPA Method 524.2: Measurement of Purgeable Organic Compounds in Water by
Capillary Column Gas Chromatography/ Mass Spectrometry
This method should be used for preparation (purging) and analysis of drinking water samples for the
contaminant identified below and listed in Appendix A.
Contaminant
Carbon disulfide
1,2-Dichloroethane
Volatile Organic Compounds, NOS *
CASRN
75-15-0
107-06-2
NA
* NOS = Not otherwise specified
Volatile organic compounds and surrogates with low water solubility are extracted (purged) from the
sample matrix by bubbling an inert gas through the aqueous sample. Purged sample components are
trapped in a tube containing suitable sorbent materials. When purging is complete, the sorbent tube is
heated and backflushed with helium to desorb the trapped sample components into a capillary gas
chromatography (GC) column interfaced to a mass spectrometer (MS). The column is temperature
programmed to facilitate the separation of the method analytes, which are then detected with the MS.
Source: http://webl.er.usgs.gov/nemi/method summary.!sp?param method id=4803
4.2.12 EPA Method 525.2: Determination of Organic Compounds in Drinking Water by
Liquid-Solid Extraction and Capillary Column Gas Chromatography / Mass
Spectrometry
This method should be used for preparation and analysis of drinking water samples for the
contaminants identified below and listed in Appendix A.
Contaminant
Dichlorvos
Fenamiphos
Mevinphos
Semivolatile Organic Compounds, NOS *
CASRN
62-73-7
22224-92-6
7786-34-7
NA
* NOS = Not otherwise specified
Organic compounds, internal standards, and surrogates are extracted from a water sample by passing 1 L
of sample water through a cartridge or disk containing a solid matrix with chemically bonded C18 organic
phase (liquid-solid extraction, LSE). The organic compounds are eluted from the LSE cartridge or disk
with small quantities of ethyl acetate followed by methylene chloride. The resulting extract is
SAM Revision 2.0 18 September 29, 2005
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concentrated further by evaporation of some of the solvent. Sample components are separated,
identified, and measured by injecting an aliquot of the concentrated extract into a high resolution fused
silica capillary column of a gas chromatography/mass spectrometry (GC/MS) system.
Source: http://webl.er.usgs.gov/nemi/method summary.! sp?param method id=4804
4.2.13 EPA Method 531.2: Measurement of N-Methylcarbamoyloximes and N-
Methylcarbamates in Water by Direct Aqueous Injection HPLC with Postcolumn
Derivatization
This method should be used for preparation and analysis of drinking water samples for the
contaminants identified below and listed in Appendix A.
Contaminant
Aldicarb (Temik)
Carbofuran (Furadan)
Oxamyl
CASRN
116-06-3
1563-66-2
23135-22-0
An aliquot of sample is measured in a volumetric flask. Samples are preserved, spiked with appropriate
surrogates and filtered. Analytes are chromatographically separated by injecting an aliquot (up to 1000
(iL) into a high performance liquid chromatographic (HPLC) system equipped with a reverse phase (C-
18) column. After elution from the column, the analytes are hydrolyzed in a post column reaction to
form methyl amine, which is in turn reacted to form a fluorescent isoindole that is detected by a
fluorescence detector. Analytes also are quantitated using the external standard technique.
Source: http://www.epa.gov/ogwdwOOO/methods/met531 2.pdf
4.2.14 EPA Method 549.2: Determination of Diquat and Paraquat in Drinking Water by
Liquid-Solid Extraction and High-Performance Liquid Chromatography with
Ultraviolet Detection
This method should be used for preparation and analysis of aqueous/liquid and drinking water samples
for the contaminant identified below and listed in Appendix A.
Contaminant
Paraquat
CASRN
4685-14-7
A 250-mL sample is extracted using a C-8 liquid/solid extraction (LSE) cartridge or a C-8 disk that has
been specially prepared for the reversed-phase, ion-pair mode. The LSE disk or cartridge is eluted with
acidic aqueous solvent to yield the eluate/extract. An ion-pair reagent is added to the eluate/extract. The
concentrations of paraquat in the eluate/extract are measured using high performance liquid
chromatography (HPLC) system equipped with a UV absorbance detector. A photodiode array detector
is used to provide simultaneous detection and confirmation of the method analytes. The analytical range
depends on the sample matrix and the instrumentation used.
Source: http://www.epa.gov/nerlcwww/rn 549 2.pdf
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4.2.15 EPA Method 3031 (SW-846): Acid Digestion of Oils for Metals Analysis by Atomic
Absorption or ICP Spectrometry
This method should be used for preparation of oily solid samples for the contaminants identified below
and listed in Appendix A. Note: SW-846 Method 60 IOC or 6020A should be used for sample analysis
(refer to Appendix A).
Contaminant
Arsenic (III) compounds
Arsenic trichloride
Cadmium
Metals, NOS *
CASRN
22569-72-8
7784-34-1
7440-43-9
NA
* NOS = Not otherwise specified
This method will determine arsenic (IE) compounds and arsenic trichloride as arsenic. The method also
will determine osmium tetraoxide as osmium. A 0.5-g sample of oil, oil sludge, tar, wax, paint, or paint
sludge is mixed with potassium permanganate and sulfuric acid. The mixture is then treated with nitric
and hydrochloric acids, filtered and diluted to volume. Excess manganese may be removed with
ammonium hydroxide. Digestates are analyzed by Method 6020A or 6010C (SW-846).
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/3031 .pdf
4.2.16 EPA Method 3050B (SW-846): Acid Digestion of Sediments, Sludges, and Soils
This method should be used for preparation of solid and/or oily solid samples for the contaminants
identified below and listed in Appendix A. Note: SW-846 Method 60 IOC, 6020A, or 7010 should be
used for sample analysis (refer to Appendix A).
Contaminant
Arsenic (III) compounds
Arsenic Trichloride
Arsine
Cadmium
Metals, NOS *
Osmium tetraoxide
Titanium tetrachloride
CASRN
22569-72-8
7784-34-1
7784-42-1
7440-43-9
NA
20816-12-0
7550-45-0
* NOS = Not otherwise specified
This method will determine arsine, arsenic (HI) compounds, and arsenic trichloride as arsenic. The
method also will determine titanium tetrachloride as titanium. A 1-g to 2-g sample is digested with nitric
acid and hydrogen peroxide. Samples to be analyzed by Method 60IOC (SW-846) for cadmium are also
treated with hydrochloric acid. Sample volumes are reduced, then brought up to a final volume of 100
mL. Samples are analyzed for arsenic by Method 6020A (SW-846) and for cadmium by either Method
60IOC or 6020A (SW-846).
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/3050b.pdf
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4.2.17 EPA Method 3520C (SW-846): Continuous Liquid-Liquid Extraction
This method should be used for preparation of aqueous/liquid and/or drinking water samples for the
contaminants identified below and listed in Appendix A. Note: SW-846 Method 6020A, 8015C, 8082A,
8270D, or 8321B should be used for sample analysis (refer to Appendix A).
Contaminant
Bromadiolone
Chloropicrin
Chlorosarin
Chlorosoman
2-Chlorovinylarsonous acid (CVAA)
Cyclohexyl sarin (GF)
Dichlorvos
Dicrotophos
Diesel Range Organics
Diisopropyl methylphosphonate (DIMP)
Dimethylphosphite
Dimethylphosphoramidic acid
EA2192
Ethyldichloroarsine (ED)
Ethylmethyl phosphonate (EMPA)
Fenamiphos
GE (1-methylethyl ester ethyl-phosphonofluoridic acid)
Isopropyl methylphosphonic acid (IMPA)
Kerosene
Lewisite 1 (L-1) [2-chlorovinyldichloroarsine]
Lewisite 2 (L-2) [bis(2-chlorovinyl)-chloroarsine]
Lewisite 3 (L-3) [tris(2-chlorovinyl)-arsine]
Lewisite oxide
Methyl hydrazine
Methyl parathion
Methylphosphonic acid (MPA)
Mevinphos
Mustard, nitrogen (HN-2) [unstable compound]
CASRN
28772-56-7
76-06-2
1445-76-7
7040-57-5
85090-33-1
329-99-7
62-73-7
141-66-2
NA
1445-75-6
868-85-9
33876-51-6
73207-98-4
598-14-1
1832-53-7
22224-92-6
1189-87-3
1832-54-8
64742-81-0
541-25-3
40334-69-8
40334-70-1
1306-02-1
60-34-4
298-00-0
993-13-5
7786-34-7
51-75-2
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Contaminant
Mustard, sulfur (HD) / Mustard gas (H)
Nicotine
Perfluoroisobutylene (PFIB)
Phencyclidine
Phenol
Phorate
Polychlorinated biphenyls (PCBs)
Sarin (GB)
Semivolatile Organic Compounds, NOS *
Soman (GD)
Strychnine
Tabun (GA)
Tear gas (CS) [chlorobenzylidene malonitrile]
Tetraethyl pyrophosphate
Tetramethylenedisulfotetramine
Thiodiglycol (TDG)
Trimethyl phosphite
VE
VG
VM
VX [O-ethyl-S-(2-di isopro pylami noethyl Jmethyl
phosphonothiolate]
CASRN
505-60-2
54-11-5
382-21-8
77-10-1
108-95-2
298-02-2
1336-36-3
107-44-8
NA
96-64-0
57-24-9
77-81-6
2698-41-1
107-49-3
80-12-6
111-48-8
121-45-9
21738-25-0
78-53-5
21770-86-5
50782-69-9
* NOS = Not otherwise specified
This method describes a procedure for isolating organic compounds from aqueous/liquid samples. This
method is applicable to the isolation and concentration of water-insoluble and slightly soluble organics in
preparation fora variety of chromatographic procedures. A measured volume of sample, usually 1 L, is
placed into a continuous liquid-liquid extractor, adjusted, if necessary, to a specific pH (see Table 1 in
Method 3520C), and extracted with organic solvent for 18 to 24 hours. The extract is filtered through
sodium sulfate to remove residual moisture, concentrated, and exchanged as necessary into a solvent
compatible with the cleanup or determinative procedure used for analysis.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/3520c.pdf
SAM Revision 2.0
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4.2.18 EPA Method 3535A (SW-846): Solid-Phase Extraction
This method should be used for preparation of aqueous/liquid and/or drinking water samples for the
contaminants identified below and listed in Appendix A. Note: SW-846 Method 6020A, 8015C, 8082A,
8270D, or 8321B should be used for sample analysis (refer to Appendix A).
Contaminant
Bromadiolone
Chloropicrin
Chlorosarin
Chlorosoman
2-Chlorovinylarsonous acid (CVAA)
Cyclohexyl sarin (GF)
Dichlorvos
Dicrotophos
Diesel Range Organics
Diisopropyl methylphosphonate (DIMP)
Dimethylphosphite
Dimethylphosphoramidic acid
EA2192
Ethyldichloroarsine (ED)
Ethylmethyl phosphonate (EMPA)
Fenamiphos
GE (1-methylethyl ester ethyl-phosphonofluoridic acid)
Isopropyl methylphosphonic acid (IMPA)
Kerosene
Lewisite 1 (L-1) [2-chlorovinyldichloroarsine]
Lewisite 2 (L-2) [bis(2-chlorovinyl)-chloroarsine]
Lewisite 3 (L-3) [tris(2-chlorovinyl)-arsine]
Lewisite oxide
Methyl hydrazine
Methyl parathion
Methylphosphonic acid (MPA)
Mevinphos
Mustard, nitrogen (HN-2) [unstable compound]
CASRN
28772-56-7
76-06-2
1445-76-7
7040-57-5
85090-33-1
329-99-7
62-73-7
141-66-2
NA
1445-75-6
868-85-9
33876-51-6
73207-98-4
598-14-1
1832-53-7
22224-92-6
1189-87-3
1832-54-8
64742-81-0
541-25-3
40334-69-8
40334-70-1
1306-02-1
60-34-4
298-00-0
993-13-5
7786-34-7
51-75-2
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Contaminant
Mustard, sulfur (HD) / Mustard gas (H)
Nicotine
Perfluoroisobutylene (PFIB)
Phencyclidine
Phenol
Phorate
Polychlorinated biphenyls (PCBs)
Sarin (GB)
Semivolatile Organic Compounds, NOS *
Soman (GD)
Strychnine
Tabun (GA)
Tear gas (CS) [chlorobenzylidene malonitrile]
Tetraethyl pyrophosphate
Tetramethylenedisulfotetramine
Thiodiglycol (TDG)
Trimethyl phosphite
VE
VG
VM
VX [O-ethyl-S-(2-di isopro pylami noethyl Jmethyl
phosphonothiolate]
CASRN
505-60-2
54-11-5
382-21-8
77-10-1
108-95-2
298-02-2
1336-36-3
107-44-8
NA
96-64-0
57-24-9
77-81-6
2698-41-1
107-49-3
80-12-6
111-48-8
121-45-9
21738-25-0
78-53-5
21770-86-5
50782-69-9
* NOS = Not otherwise specified
This method describes a procedure for isolating target organic analytes from aqueous/liquid samples
using solid-phase extraction (SPE) media. Sample preparation procedures vary by analyte group.
Following any necessary pH adjustment, a measured volume of sample is extracted by passing it through
the solid-phase extraction medium (disks or cartridges), which is held in an extraction device designed
for vacuum filtration of the sample. Target analytes are eluted from the solid-phase media using an
appropriate solvent which is collected in a receiving vessel. The resulting solvent extract is dried using
sodium sulfate and concentrated, as needed.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/3535a.pdf
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4.2.19 EPA Method 3541 (SW-846): Automated Soxhlet Extraction
This method should be used for preparation of solid and/or oily solid samples for the contaminants
identified below and listed in Appendix A. Note: SW-846 Method 6020A, 8015C, 8082A, 8270D, or
8321B should be used for sample analysis (refer to Appendix A).
Contaminant
Bromadiolone
Chloropicrin
Chlorosarin
Chlorosoman
2-Chlorovinylarsonous acid (CVAA)
Cyclohexyl sarin (GF)
Dichlorvos
Dicrotophos
Diesel Range Organics
Diisopropyl methylphosphonate (DIMP)
Dimethylphosphite
Dimethylphosphoramidic acid
EA2192
Ethyldichloroarsine (ED)
Ethylmethyl phosphonate (EMPA)
Fenamiphos
GE (1-methylethyl ester ethyl-phosphonofluoridic acid)
Isopropyl methylphosphonic acid (IMPA)
Kerosene
Lewisite 1 (L-1) [2-chlorovinyldichloroarsine]
Lewisite 2 (L-2) [bis(2-chlorovinyl)-chloroarsine]
Lewisite 3 (L-3) [tris(2-chlorovinyl)-arsine]
Lewisite oxide
Methyl hydrazine
Methyl parathion
Methylphosphonic acid (MPA)
Mevinphos
Mustard, nitrogen (HN-2) [unstable compound]
CASRN
28772-56-7
76-06-2
1445-76-7
7040-57-5
85090-33-1
329-99-7
62-73-7
141-66-2
NA
1445-75-6
868-85-9
33876-51-6
73207-98-4
598-14-1
1832-53-7
22224-92-6
1189-87-3
1832-54-8
64742-81-0
541-25-3
40334-69-8
40334-70-1
1306-02-1
60-34-4
298-00-0
993-13-5
7786-34-7
51-75-2
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Contaminant
Mustard, sulfur (HD) / Mustard gas (H)
Nicotine
Perfluoroisobutylene (PFIB)
Phencyclidine
Phenol
Phorate
Polychlorinated biphenyls (PCBs)
Sarin (GB)
Semivolatile Organic Compounds, NOS *
Soman (GD)
Strychnine
Tabun (GA)
Tear gas (CS) [chlorobenzylidene malonitrile]
Tetraethyl pyrophosphate
Tetramethylenedisulfotetramine
Thiodiglycol (TDG)
Trimethyl phosphite
VE
VG
VM
VX [O-ethyl-S-(2-di isopro pylami noethyl Jmethyl
phosphonothiolate]
CASRN
505-60-2
54-11-5
382-21-8
77-10-1
108-95-2
298-02-2
1336-36-3
107-44-8
NA
96-64-0
57-24-9
77-81-6
2698-41-1
107-49-3
80-12-6
111-48-8
121-45-9
21738-25-0
78-53-5
21770-86-5
50782-69-9
* NOS = Not otherwise specified
Approximately 10 g of solid sample is mixed with an equal amount of anhydrous sodium sulfate, placed
in an extraction thimble or between two plugs of glass wool, and after adding the appropriate surrogate
amount, is extracted using an appropriate solvent in an automated Soxhlet extractor. The extract is dried
with sodium sulfate to remove residual moisture, concentrated and exchanged, as necessary into a solvent
compatible with the cleanup or determinative procedure for analysis.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/3541 .pdf
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4.2.20 EPA Method 3545A (SW-846): Pressurized Fluid Extraction (PFE)
This method should be used for preparation of solid and/or oily solid samples for the contaminants
identified below and listed in Appendix A. Note: SW-846 Method 6020A, 8015C, 8082A, 8270D, or
8321B should be used for sample analysis (refer to Appendix A).
Contaminant
Bromadiolone
Chloropicrin
Chlorosarin
Chlorosoman
2-Chlorovinylarsonous acid (CVAA)
Cyclohexyl sarin (GF)
Dichlorvos
Dicrotophos
Diesel Range Organics
Diisopropyl methylphosphonate (DIMP)
Dimethylphosphite
Dimethylphosphoramidic acid
EA2192
Ethyldichloroarsine (ED)
Ethylmethyl phosphonate (EMPA)
Fenamiphos
GE (1-methylethyl ester ethyl-phosphonofluoridic acid)
Isopropyl methylphosphonic acid (IMPA)
Kerosene
Lewisite 1 (L-1) [2-chlorovinyldichloroarsine]
Lewisite 2 (L-2) [bis(2-chlorovinyl)-chloroarsine]
Lewisite 3 (L-3) [tris(2-chlorovinyl)-arsine]
Lewisite oxide
Methyl hydrazine
Methyl parathion
Methylphosphonic acid (MPA)
Mevinphos
Mustard, nitrogen (HN-2) [unstable compound]
CASRN
28772-56-7
76-06-2
1445-76-7
7040-57-5
85090-33-1
329-99-7
62-73-7
141-66-2
NA
1445-75-6
868-85-9
33876-51-6
73207-98-4
598-14-1
1832-53-7
22224-92-6
1189-87-3
1832-54-8
64742-81-0
541-25-3
40334-69-8
40334-70-1
1306-02-1
60-34-4
298-00-0
993-13-5
7786-34-7
51-75-2
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Contaminant
Mustard, sulfur (HD) / Mustard gas (H)
Nicotine
Perfluoroisobutylene (PFIB)
Phencyclidine
Phenol
Phorate
Polychlorinated biphenyls (PCBs)
Sarin (GB)
Semivolatile Organic Compounds, NOS *
Soman (GD)
Strychnine
Tabun (GA)
Tear gas (CS) [chlorobenzylidene malonitrile]
Tetraethyl pyrophosphate
Tetramethylenedisulfotetramine
Thiodiglycol (TDG)
Trimethyl phosphite
VE
VG
VM
VX [O-ethyl-S-(2-diisopropylaminoethyl)methyl
phosphonothiolate]
CASRN
505-60-2
54-11-5
382-21-8
77-10-1
108-95-2
298-02-2
1336-36-3
107-44-8
NA
96-64-0
57-24-9
77-81-6
2698-41-1
107-49-3
80-12-6
111-48-8
121-45-9
21738-25-0
78-53-5
21770-86-5
50782-69-9
* NOS = Not otherwise specified
Approximately 10 to 30 g of soil sample is prepared for extraction either by air drying the sample, or by
mixing the sample with anhydrous sodium sulfate or pelletized diatomaceous earth. (Note: Sodium
sulfate can cause clogging, and air drying or diatomaceous earth may be preferred.) The sample is then
ground and loaded into the extraction cell. The extraction cell containing the sample is heated to the
extraction temperature, pressurized with the appropriate solvent system, and extracted for 5 minutes (or
as recommended by the instrument manufacturer). The extract may be concentrated, if necessary, and, as
needed, exchanged into a solvent compatible with the cleanup or determinative step being employed.
This method has been validated for solid matrices containing 250 to 12,500 u,g/kg of semivolatile organic
compounds, 250 to 2500 u,g/kg of organophosphorus pesticides, 5 to 250 u,g/kg of organochlorine
pesticides, 50 to 5000 u,g/kg of chlorinated herbicides, 1 to 1400 u,g/kg of PCBs, and 1 to 2500 ng/kg of
PCDDs/PCDFs.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/3545a.pdf
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4.2.21 EPA Method 3580A (SW-846): Waste Dilution
This method should be used for preparation of oily solid samples for the contaminants identified below
and listed in Appendix A. Note: SW-846 Method 6020A, 8015C, 8082A, 8270D, or 8321B should be
used for sample analysis (refer to Appendix A).
Contaminant
Bromadiolone
Chloropicrin
Chlorosarin
Chlorosoman
2-Chlorovinylarsonous acid (CVAA)
Cyclohexyl sarin (GF)
Dichlorvos
Dicrotophos
Diesel Range Organics
Diisopropyl methylphosphonate (DIMP)
Dimethylphosphite
Dimethylphosphoramidic acid
EA2192
Ethyldichloroarsine (ED)
Ethylmethyl phosphonate (EMPA)
Fenamiphos
GE (1-methylethyl ester ethyl-phosphonofluoridic acid)
Isopropyl methylphosphonic acid (IMPA)
Kerosene
Lewisite 1 (L-1) [2-chlorovinyldichloroarsine]
Lewisite 2 (L-2) [bis(2-chlorovinyl)-chloroarsine]
Lewisite 3 (L-3) [tris(2-chlorovinyl)-arsine]
Lewisite oxide
Methyl hydrazine
Methyl parathion
Methylphosphonic acid (MPA)
Mevinphos
CASRN
28772-56-7
76-06-2
1445-76-7
7040-57-5
85090-33-1
329-99-7
62-73-7
141-66-2
NA
1445-75-6
868-85-9
33876-51-6
73207-98-4
598-14-1
1832-53-7
22224-92-6
1189-87-3
1832-54-8
64742-81-0
541-25-3
40334-69-8
40334-70-1
1306-02-1
60-34-4
298-00-0
993-13-5
7786-34-7
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Contaminant
Mustard, nitrogen (HN-2) [unstable compound]
Mustard, sulfur (HD) / Mustard gas (H)
Nicotine
Perfluoroisobutylene (PFIB)
Phencyclidine
Phenol
Phorate
Polychlorinated biphenyls (PCBs)
Sarin (GB)
Semivolatile Organic Compounds, NOS *
Soman (GD)
Strychnine
Tabun (GA)
Tear gas (CS) [chlorobenzylidene malonitrile]
Tetraethyl pyrophosphate
Tetramethylenedisulfotetramine
Thiodiglycol (TDG)
Trimethyl phosphite
VE
VG
VM
VX [O-ethyl-S-(2-di isopro pylami noethyl )methyl
phosphonothiolate]
CASRN
51-75-2
505-60-2
54-11-5
382-21-8
77-10-1
108-95-2
298-02-2
1336-36-3
107-44-8
NA
96-64-0
57-24-9
77-81-6
2698-41-1
107-49-3
80-12-6
111-48-8
121-45-9
21738-25-0
78-53-5
21770-86-5
50782-69-9
* NOS = Not otherwise specified
This method describes a solvent dilution of a non-aqueous waste sample prior to cleanup and/or analysis.
One gram of sample is weighed into a capped tube, and the sample is diluted to 10.0 mL with an
appropriate solvent. The method is designed for wastes that may contain organic chemicals at a
concentration greater than 20,000 mg/kg and that are soluble in the dilution solvent.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/3580a.pdf
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4.2.22 EPA Method 3585 (SW-846): Waste Dilution for Volatile Organics
This method should be used for preparation of oily solid samples for the contaminants identified below
and listed in Appendix A. Note: SW-846 Method 8015C or 8260B should be used for sample analysis
(refer to Appendix A).
Contaminant
Allyl alcohol
Carbon disulfide
2-Chloroethanol
3-Chloro-1 ,2-propanediol
Cyanogen chloride
1,2-Dichloroethane
1,4-Dithiane
Ethylene oxide
Gasoline Range Organics
Phosgene
Propylene oxide
1,4-Thioxane
Volatile Organic Compounds, NOS *
CASRN
107-18-6
75-15-0
107-07-3
96-24-2
506-77-4
107-06-2
505-29-3
75-21-8
NA
75-44-5
75-56-9
15980-15-1
NA
* NOS = Not otherwise specified
This method describes a solvent dilution of a non-aqueous waste sample prior to direct injection analysis.
It is designed for use in conjunction with GC or GC/MS analysis of wastes that may contain organic
chemicals at a concentration greater than 1 mg/kg and that are soluble in the dilution solvent. Highly
contaminated or highly complex samples may be diluted prior to analysis for volatiles using direct
injection. One gram of sample is weighed into a capped tube or volumetric flask. The sample is diluted
to 2.0 to 10.0 mL with «-hexadecane or other appropriate solvent. Diluted samples are injected into the
GC or GC/MS for analysis.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/3585.pdf
4.2.23 EPA Method 5030C (SW-846): Purge-and-Trap for Aqueous Samples
This method should be used for preparation of aqueous/liquid and/or drinking water samples for the
contaminants identified below and listed in Appendix A. Note: SW-846 Method 8015C or 8260B should
be used for sample analysis (refer to Appendix A).
Contaminant
Allyl alcohol
Carbon disulfide
2-Chloroethanol
3-Chloro-1 ,2-propanediol
CASRN
107-18-6
75-15-0
107-07-3
96-24-2
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Contaminant
Cyanogen chloride
1,2-Dichloroethane
1,4-Dithiane
Ethylene oxide
Gasoline Range Organics
Kerosene
Propylene oxide
1,4-Thioxane
Volatile Organic Compounds, NOS *
CASRN
506-77-4
107-06-2
505-29-3
75-21-8
NA
64742-81-0
75-56-9
15980-15-1
NA
* NOS = Not otherwise specified
This method describes a purge-and-trap procedure for the analysis of volatile organic compounds (VOCs)
in aqueous/liquid samples and water miscible liquid samples. It also describes the analysis of high
concentration soil and waste sample extracts prepared using Method 5035A (SW-846). The gas
chromatographic determinative steps for this sample preparation technique can be found in the
determinative method identified in Appendix A.
Aqueous/Liquid Samples: An inert gas is bubbled through a portion of the aqueous/liquid sample at
ambient temperature, and the volatile components are efficiently transferred from the aqueous/liquid
phase to the vapor phase. The vapor is swept through a sorbent column where the volatile components
are adsorbed. After purging is completed, the sorbent column is heated and backflushed with inert gas to
desorb the components onto a gas chromatographic column.
High Concentration Extracts from Method 5035A (SW-846): An aliquot of the extract prepared using
Method 5 03 5A is combined with organic-free reagent water in the purging chamber. It is then analyzed
by purge-and-trap GC or GC/MS following the procedure used for the aqueous/liquid samples.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/5030c.pdf
4.2.24 EPA Method 5035A (SW-846): Closed-System Purge-and-Trap and Extraction for
Volatile Organics in Soil and Waste Samples
This method should be used for preparation of solid samples for the contaminants identified below and
listed in Appendix A. Note: SW-846 Method 8015C or 8260B should be used for sample analysis (refer
to Appendix A).
Contaminant
Allyl alcohol
Carbon disulfide
2-Chloroethanol
3-Chloro-1 ,2-propanediol
Cyanogen chloride
CASRN
107-18-6
75-15-0
107-07-3
96-24-2
506-77-4
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Contaminant
1,2-Dichloroethane
1,4-Dithiane
Ethylene oxide
Gasoline Range Organics
Kerosene
Phosgene
Propylene oxide
1,4-Thioxane
Volatile Organic Compounds, NOS *
CASRN
1 07-06-2
505-29-3
75-21-8
NA
64742-81-0
75-44-5
75-56-9
15980-15-1
NA
* NOS = Not otherwise specified
This method describes a closed-system purge-and-trap process for analysis of volatile organic compounds
(VOCs) in solid samples containing low levels (0.5 to 200 u.g/kg) of VOCs. The method also provides
specific procedures for preparation of samples containing high levels (>200 u,g/kg ) of VOCs. For low-
level VOCs, a 5-g sample is collected into a vial, that is placed into an autosampler device. Reagent
water, surrogates, and internal standards are automatically added, and the vial heated to 40°C. The
volatiles are purged into an appropriate trap using an inert gas combined with sample agitation. When
purging is complete, the trap is heated and backflushed with helium to desorb the trapped sample
components into a gas chromatograph for analysis. For high-level VOCs, samples are either collected
into a vial that contains a water-miscible organic solvent or a portion of sample is removed from the vial
and dispersed in a water-miscible solvent. An aliquot of the solvent is added to reagent water, along with
surrogates and internal standards, then purged and analyzed using an appropriate determinative method
(e.g., 8260B (SW-846)).
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/5035a rl .pdf
4.2.25 EPA Method 601OC (SW-846): Inductively Coupled Plasma - Atomic Emission
Spectrometry
This method should be used for analysis of the contaminants identified below and listed in Appendix A.
Contaminant
Arsenic (III) compounds
Arsenic trichloride
Cadmium
Metals, NOS *
Osmium tetraoxide
Titanium tetrachloride
CASRN
22569-72-8
7784-34-1
7440-43-9
NA
20816-12-0
7550-45-0
* NOS = Not otherwise specified
This method determines arsenic (IE) compounds and arsenic trichloride as arsenic, osmium tetraoxide as
osmium, and titanium tetrachloride as titanium. Any other metals are determined as the metal. Aqueous
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samples (prepared using SW-846 Method 5050), soil samples (prepared using SW-846 Methods 3050B
or 5050), oily solid samples (prepared using SW-846 Methods 3050B or 3031), and air filter/particle
samples (prepared using Inorganic (IO) Method 3.4) are analyzed by Inductively Coupled Plasma -
Atomic Emission Spectrometry (ICP-AES). Detection limits vary with each analyte. The analytical
range may be extended by sample dilution.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/601 Oc.pdf
4.2.26 EPA Method 6020A (SW-846): Inductively Coupled Plasma - Mass Spectrometry
This method should be used for analysis of the contaminants identified below and listed in Appendix A.
Contaminant
Arsenic (III) compounds
Arsenic trichloride
Cadmium
2-Chlorovinylarsonous acid (CVAA)
Lewisite oxide
Metals, NOS *
Titanium tetrachloride
CASRN
22569-72-8
7784-34-1
7440-43-9
85090-33-1
1306-02-1
NA
7550-45-0
* NOS = Not otherwise specified
This method will determine arsenic (IE) compounds, arsenic trichloride, Lewisite oxide, and CVAA as
arsenic. The method also will determine titanium tetrachloride as titanium. Any other metals are
determined as the metal. Aqueous samples (prepared using SW-846 Method 5050), soil samples
(prepared using SW-846 Methods 3050B or 5050), oily solid samples (prepared using SW-846 Methods
3050B or 3031), and air filter/particle samples (prepared using IO Method 3.5) are analyzed by
Inductively Coupled Plasma - Mass Spectrometry. Detection limits vary with each analyte. The
analytical range may be extended by sample dilution.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/6020a.pdf
4.2.27 EPA Method 7010 (SW-846): Graphite Furnace Atomic Absorption
Spectrophotometry
This method should be used for analysis of the contaminant identified below and listed in Appendix A.
Contaminant
Arsine
CASRN
7784-42-1
This method determines arsine as arsenic in environmental samples. Soil samples (prepared using SW-
846 Method 3 05 OB) are analyzed by Graphite Furnace Atomic Absorption Spectrophotometry (GFAA).
A representative aliquot of the sample is placed in the graphite tube in the furnace, evaporated to dryness,
charred, and atomized. Detection limits vary with each matrix and instrument used. The analytical range
may be extended by sample dilution.
Source: http: //www .epa. gov/epao swer/hazwaste/te st/pdfs/7010 .pdf
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4.2.28 EPA Method 7470A (SW-846): Mercury in Liquid Wastes (Manual Cold-Vapor
Technique)
This method should be used for preparation and analysis of aqueous/liquid samples for the contaminant
identified below and listed in Appendix A.
Contaminant
Mercury
CASRN
7439-97-6
A 100-mL aqueous or liquid waste sample is digested with acids, permanganate solution, persulfate
solution, and heat. The sample is cooled and reduced with hydroxylamine - sodium chloride solution.
Just prior to analysis, the sample is treated with Sn(II), reducing the mercury to Hg(0). The reduced
sample is sparged and the mercury vapor is analyzed by cold vapor atomic absorption. The detection
limit for the method is less than 0.2 (ig/L. Chloride and copper are potential interferences.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/7470a.pdf
4.2.29 EPA Method 7471B (SW-846): Mercury in Solid or Semisolid Wastes (Manual Cold-
Vapor Technique)
This method should be used for preparation and analysis of solid phase samples for the contaminant
identified below and listed in Appendix A.
Contaminant
Mercury
CASRN
7439-97-6
A 0.5-g to 0.6-g sample is digested with aquaregia, permanganate solution, and heat. The sample is
cooled and reduced with hydroxylamine - sodium chloride solution. Just prior to analysis, the sample is
treated with Sn(II), reducing the mercury to Hg(0). The reduced sample is sparged and the mercury
vapor is analyzed by cold vapor atomic absorption. Chloride and copper are potential interferences.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/7471b.pdf
4.2.30 EPA Method 8015C (SW-846): Nonhalogenated Organics Using GC/FID
This method should be used for analysis of the contaminants identified below and listed in Appendix A.
Contaminant
Diesel Range Organics
Gasoline Range Organics
Kerosene
CASRN
NA
NA
64742-81-0
This method provides gas chromatographic conditions for the detection of certain nonhalogenated
volatile and semivolatile organic compounds. Depending on the analytes of interest, samples may be
introduced into the GC by a variety of techniques including purge-and-trap, direct injection of
aqueous/liquid samples, and solvent extraction. An appropriate column and temperature program are
used in the gas chromatograph to separate the organic compounds. Detection is achieved by a flame
ionization detector (FID). The method allows the use of packed or capillary columns for the analysis and
SAM Revision 2.0 35 September 29, 2005
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confirmation of the non-halogenated individual analytes. The estimated method detection limits vary
with each analyte and range between 2 and 48 u,g/L for aqueous/liquid samples. The method detection
limits in other matrices have not been evaluated for this method. The analytical range depends on the
target analyte(s) and the instrument used.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/8015c.pdf
4.2.31 EPA Method 8260B (SW-846): Volatile Organic Compounds by Gas
Chromatography/Mass Spectrometry (GC/MS)
This method should be used for analysis of the contaminants identified below and listed in Appendix A.
Contaminant
Allyl alcohol
Carbon disulfide
2-Chloroethanol
3-Chloro-1 ,2-propanediol
Cyanogen chloride
1,2-Dichloroethane
1,4-Dithiane
Ethylene oxide
Phosgene
Propylene oxide
1,4-Thioxane
Volatile Organic Compounds, NOS *
CASRN
107-18-6
75-15-0
107-07-3
96-24-2
506-77-4
107-06-2
505-29-3
75-21-8
75-44-5
75-56-9
15980-15-1
NA
NOS = Not otherwise specified
Volatile compounds are introduced into a gas chromatograph by purge-and-trap or other methods (see
Sec. 1.2 in Method 8260B). The analytes can be introduced directly to a wide-bore capillary column or
cryofocused on a capillary pre-column before being flash evaporated to a narrow-bore capillary for
analysis. Alternatively, the effluent from the trap is sent to an injection port operating in the split mode
for injection to a narrow-bore capillary column. The column is temperature-programmed to separate the
analytes, which are then detected with amass spectrometer (MS) interfaced to the gas chromatograph
(GC). Analytes eluted from the capillary column are introduced into the mass spectrometer via a jet
separator or a direct connection. The estimated quantitation limit (EQL) of Method 8260B for an
individual analyte is dependent on the instrument as well as the choice of sample
preparation/introduction method. Using standard quadrupole instrumentation and the purge-and-trap
technique, estimated quantitation limits are 5 u,g/kg (wet weight) for soil/sediment samples and 5 u,g/L
for ground water (see Table 3 in Method 8260B). Somewhat lower limits may be achieved using an ion
trap mass spectrometer or other instrumentation of improved design. No matter which instrument is
used, EQLs will be proportionately higher for sample extracts and samples that require dilution or when a
reduced sample size is used to avoid saturation of the detector.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/8260b.pdf
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4.2.32 EPA Method 8270D (SW-846): Semivolatile Organic Compounds by Gas
Chromatography/Mass Spectrometry (GC/MS)
This method should be used for analysis of the contaminants identified below and listed in Appendix A.
Contaminant
Chloropicrin
Chlorosarin
Chlorosoman
Cyclohexyl sarin (CF)
Dichlorvos
Dicrotophos
Dimethylphosphite
Ethyldichloroarsine (ED)
Fenamiphos
GE (1-methylethyl ester ethyl-phosphonofluoridic acid)
Lewisite 1 (L-1) [2-chlorovinyldichloroarsine]
Lewisite 2 (L-2) [bis(2-chlorovinyl)-chloroarsine]
Lewisite 3 (L-3) [tris(2-chlorovinyl)-arsine]
Methyl hydrazine
Methyl parathion
Mevinphos
Mustard, nitrogen (HN-2) [unstable compound]
Mustard, sulfur (HD) / Mustard gas (H)
Nicotine
Perfluoroisobutylene (PFIB)
Phencyclidine
Phenol
Phorate
Sarin (GB)
Semivolatile Organic Compounds, NOS *
Soman (GD)
Strychnine
Tabun (GA)
CASRN
76-06-2
1445-76-7
7040-57-5
329-99-7
62-73-7
141-66-2
868-85-9
598-14-1
22224-92-6
1189-87-3
541-25-3
40334-69-8
40334-70-1
60-34-4
298-00-0
7786-34-7
51-75-2
505-60-2
54-11-5
382-21-8
77-10-1
108-95-2
298-02-2
107-44-8
NA
96-64-0
57-24-9
77-81-6
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Contaminant
Tear gas (CS) [chlorobenzylidene malonitrile]
Tetraethyl pyrophosphate
Thiodiglycol (TDG)
Trimethyl phosphite
VE
VG
VM
VX [O-ethyl-S-(2-di isopro pylami noethyl )methyl
phosphonothiolate]
CASRN
2698-41-1
107-49-3
111-48-8
121-45-9
21738-25-0
78-53-5
21770-86-5
50782-69-9
* NOS = Not otherwise specified
Samples are prepared for analysis by gas chromatography/mass spectrometry (GC/MS) using the
appropriate sample preparation and, if necessary, sample cleanup procedures. Semivolatile compounds
are introduced into the GC/MS by injecting the sample extract into a gas chromatograph (GC) with a
narrow-bore fused-silica capillary column. The GC column is temperature-programmed to separate the
analytes, which are then detected with amass spectrometer (MS) connected to the gas chromatograph.
Analytes eluted from the capillary column are introduced into the mass spectrometer. The estimated
method detection limits vary with each analyte and range between 10 and 1000 |ig/L for aqueous/liquid
samples and 660 and 3300 ng/kg for soil samples. The analytical range depends on the target analyte(s)
and the instrument used.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/8270d.pdf
4.2.33 EPA Method 8082A (SW-846): Polychlorinated Biphenyls (PCBs) by Gas
Chromatography
This method should be used for analysis of samples for the contaminant identified below and listed in
Appendix A.
Contaminant
Polychlorinated biphenyls (PCBs)
CASRN
1336-36-3
This method is to be employed following sample preparation by the appropriate sample preparation
procedure listed in Appendix A. Method 8082A is used to determine the concentration of
polychlorinated biphenyls (PCBs) as Aroclors or as individual PCB congeners in extracts from solid, oily
solid, aqueous, non-aqueous liquid, drinking water, and air samples. The method uses open-tubular,
capillary columns with electron capture detectors (BCD) or electrolytic conductivity detectors (ELCD).
The target compounds may be determined using either a single- or dual-column analysis system.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/8082a.pdf
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4.2.34 EPA Method 8315A (SW-846): Determination of Carbonyl Compounds by High
Performance Liquid Chromatography (HPLC)
This method should be used for preparation and analysis of solid, aqueous/liquid, and drinking water
samples for the contaminant identified below and listed in Appendix A.
Contaminant
Formaldehyde
CASRN
50-00-0
A measured volume of aqueous/liquid sample (approximately 100 mL) or an appropriate amount of
solids extract (approximately 25 g), is buffered to pH 3 and derivatized with 2,4-dinitrophenylhydrazine
(DNPH). Using the appropriate extraction technique, the derivatives are extracted using methylene
chloride and the extracts are exchanged with acetonitrile prior to HPLC analysis. HPLC conditions are
described permitting the separation and measurement of various carbonyl compounds in the extract by
absorbance detection at 360 nm. If formaldehyde is the only analyte of interest, the aqueous/liquid
sample and/or solid sample extract should be buffered to pH 5.0 to minimize the formation of artifact
formaldehyde. The method detection limit for formaldehyde varies depending on sample conditions and
instrumentation but is approximately 6.2 |ig/L for aqueous/liquid samples.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/8315a.pdf
4.2.35 EPA Method 8318A (SW-846): A/-Methylcarbamates by High Performance Liquid
Chromatography (HPLC)
This method should be used for preparation and analysis of solid, oily solid, and aqueous/liquid
samples for the contaminants identified below and listed in Appendix A.
Contaminant
Aldicarb (Temik)
Carbofuran (Furadan)
Oxamyl
CASRN
116-06-3
1563-66-2
23135-22-0
TV-methylcarbamates are extracted from aqueous/liquid samples with methylene chloride, and from soils,
oily solid waste, and oils with acetonitrile. The extract solvent is exchanged to methanol/ethylene glycol,
and the extract is cleaned using a C-18 cartridge, filtered, and eluted on a C-18 analytical column. After
separation, the target analytes are hydrolyzed and derivatized post-column, then quantified
fluorometrically. The sensitivity of the method usually depends on the level of interferences present,
rather than on the instrumental conditions. Waste samples with a high level of extractable fluorescent
compounds are expected to yield significantly higher detection limits. The estimated method detection
limits vary with each analyte and range between 1.7 and 9.4 fig/L for aqueous/liquid samples and 10 and
50 fig/kg for soil samples.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/8318a.pdf
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4.2.36 EPA Method 8321B (SW-846): Solvent-Extractable Nonvolatile Compounds by
High Performance Liquid Chromatography/Thermospray/Mass Spectrometry
(HPLC/TS/MS) or Ultraviolet (UV) Detection
This method should be used for analysis of the contaminants identified below and listed in Appendix A.
Contaminant
Bromadiolone
Diisopropyl methylphosphonate (DIMP)
Dimethylphosphoramidic acid
EA2192
Ethylmethyl phosphonate (EMPA)
Isopropyl methylphosphonic acid (IMPA)
Methylphosphonic acid (MPA)
Tetramethylenedisulfotetramine
CASRN
28772-56-7
1445-75-6
33876-51-6
73207-98-4
1 832-53-7
1832-54-8
993-13-5
80-12-6
This method provides reversed-phase high performance liquid chromatographic (RP/HPLC), thermospray
(TS) mass spectrometric (MS), and ultraviolet (UV) conditions for detection of the target analytes.
Sample extracts can be analyzed by direct injection into the thermospray or onto a liquid
chromatographic-thermospray interface. A gradient elution program is used to separate the compounds.
Primary analysis may be performed by UV detection; however, positive results should be confirmed by
TS/MS. Quantitative analysis may be performed by either TS/MS or UV detection, using either an
external or internal standard approach. TS/MS detection may be performed in either a negative
ionization (discharge electrode) mode or a positive ionization mode, with a single quadrupole mass
spectrometer. The use of MS/MS techniques is an option. The analytical range and detection limits vary
depending on the target analyte and instrument used.
Source: http://www.epa.gov/epaoswer/hazwaste/test/pdfs/8321b.pdf
4.2.37 ASTM Method D5755-03: Standard Test Method for Microvacuum Sampling and
Indirect Analysis of Dust by Transmission Electron Microscopy (TEM) for
Asbestos Structure Number Surface Loading
This method should be used for preparation and analysis of solid samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Asbestos
CASRN
1332-21-4
This method describes procedures to (a) identify asbestos in dust and (b) provide an estimate of the
surface loading of asbestos reported as the number of asbestos structures per unit area of sampled
surface. The sample is collected by vacuuming a known surface area with a standard 25 or 37 mm air
sampling cassette using a plastic tube that is attached to the inlet orifice, which acts as a nozzle. The
sample is transferred from inside the cassette to an aqueous suspension of known volume. Aliquots of
the suspension are then filtered through a membrane. A section of the membrane is prepared and
transferred to a TEM grid using a direct transfer method. The asbestiform structures are identified, sized,
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and counted by TEM, using select area electron diffraction (SAED) and energy dispersive X-ray analysis
(EDXA) at a magnification of 15,000 to 20,OOOX.
Source:
http://www.astm.org/cgi-bin/SoftCart.exe/STORE/filtrexx40.cgi ?U+mvstore+tavs3076+-L+D5755:03+/u
sr6/htdocs/astm.org/DATABASE.CART/REDLINE PAGES/D5755.htm
4.2.38 ASTM Method D6480-99: Standard Test Method for Wipe Sampling of Surfaces,
Indirect Preparation, and Analysis for Asbestos Structure Number Concentration
by Transmission Electron Microscopy
This method should be used for preparation and analysis of solid samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Asbestos
CASRN
1332-21-4
This test method describes a procedure to identify asbestos in samples wiped from surfaces and to
provide an estimate of the concentration of asbestos reported as the number of asbestos structures per
unit area of sampled surface. A sample is collected by wiping a surface of known area with a wipe
material. The sample is transferred from the wipe material to an aqueous suspension of known volume.
Aliquots of the suspension are then filtered through a membrane filter. A section of the membrane filter
is prepared and transferred to a TEM grid, using the direct transfer method. The asbestiform structures
are identified, sized, and counted by TEM, using electron diffraction (ED) and EDXA at a magnification
from 15,000 to 20,OOOX.
Source:
http://www.astm.org/cgi-bin/SoftCart.exe/STORE/filtrexx40.cgi?U+mvstore+tavs3076+-L+D6480:99+/u
sr6/htdocs/astm.org/DATABASE.CART/REDLINE PAGES/D6480.htm
4.2.39 ISO Method -10312: Ambient Air - Determination of Asbestos Fibres -
Direct-transfer Transmission Electron Microscopy Method (TEM)
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Asbestos
CASRN
1332-21-4
This method determines the type(s) of asbestos fibers present but cannot discriminate between individual
fibers of the asbestos and non-asbestos analogues of the same amphibole mineral. The method is defined
for polycarbonate capillan/pore filters or cellulose ester (either mixed esters of cellulose or cellulose
nitrate) filters through which a known volume of air has been drawn. The method is suitable for
determination of asbestos in both exterior and building atmospheres. The range of concentrations that
can be determined is 50 structures/mm2 to 7,000 structures/mm2 on the filter. In a 4000-L air sample with
approximately 10 pg/m3 (typical of clean or rural atmospheres), an analytical sensitivity of 0.5
structure/L can be obtained. This is equivalent to a detection limit of 1.8 structure/L when an area of
0.195 mm of the TEM specimen is examined.
Source:
http://www.iso.org/iso/en/CatalogueDetailPage. CatalogueDetail?CSNUMBER=18358&ICSl=13&ICS2
=40&ICS3=20
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4.2.40 ISO Method -12884: Ambient Air- Determination of Total (Gas and Particle-
phase) Polycyclic Aromatic Hydrocarbons -Collection on Sorbent-backed Filters
with Gas Chromatographic/Mass Spectrometric Analysis
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Carbofuran (Furadan)
Dichlorvos
Dicrotophos
Dimethylphosphite
Fenamiphos
Methyl parathion
Mevinphos
Phencyclidine
Phenol
Phorate
Polychlorinated biphenyls (PCBs)
Semivolatile Organic Compounds, NOS *
Tear gas (CS) [chlorobenzylidene malonitrile]
Tetraethyl pyrophosphate
Tetramethylenedisulfotetramine
Trimethyl phosphite
VE
VG
VM
VX [O-ethyl-S-(2-diisopropylaminoethyl)methyl
phosphonothiolate]
CASRN
1563-66-2
62-73-7
141-66-2
868-85-9
22224-92-6
298-00-0
7786-34-7
77-10-1
108-95-2
298-02-2
1336-36-3
NA
2698-41-1
107-49-3
80-12-6
121-45-9
21738-25-0
78-53-5
21770-86-5
50782-69-9
* NOS = Not otherwise specified
This standard specifies sample collection, cleanup, and analysis procedures for determination of
polycyclic aromatic hydrocarbons (PAHs) in air. It is designed to collect both gas-phase and particulate-
phase compounds. It is a high-volume (100 to 250 L/min) method capable of detecting 0.05 ng/m3 or less
concentrations in 350-m3 samples. An air sample is collected by pulling air at a maximum flow rate of
225 L/min through a fine-particle filter followed by a vapor trap containing polyurethane foam (PUF) or
styrene/divinylbenzene polymer resin (XAD-2). The particle filter and sorbent cartridge are extracted
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together in a Soxhlet extractor, and the sample extract is concentrated using a Kuderna-Danish
concentrator (or other verified method), followed by further concentration under a nitrogen stream. An
aliquot of sample is analyzed using GC/MS.
Source:
http://www.iso.org/iso/en/CatalogueDetailPage.CatalogueDetail?CSNUMBER=1343&ICSl=13&ICS2=
40&ICS3=20
4.2.41 ISO Method -16000-3: Indoor Air- Part 3: Determination of Formaldehyde and
Other Carbonyl Compounds -Active Sampling Method
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Formaldehyde
CASRN
50-00-0
Samples are collected by passing air through a cartridge containing silica gel coated with acidified 2,4-
dinitrophenylhydrazine (DNPH) reagent. The carbonyl group reacts with DNPH in the presence of an
acid to form stable derivatives that are analyzed for parent aldehydes and ketones using high performance
liquid chromatography (HPLC) with UV detection. Interferences are caused by certain isomeric
aldehydes or ketones that may be unresolved by the HPLC. Interferences from organic compounds that
have the same retention times and significant absorbance at 360 nm can be overcome by altering
separation conditions (e.g., use of alternative columns or mobile gas phase compositions).
Source:
http://www.iso.org/iso/en/CatalogueDetailPage.CatalogueDetail?CSNUMBER=29049&ICSl=13&ICS2
=40&ICS3=20
4.2.42 NIOSH Method 1402: Alcohols III
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Allyl alcohol
CASRN
107-18-6
A sample tube containing coconut shell charcoal is used for sample collection with a flow rate of 0.01 to
0.2 L/min. One milliliter of eluent is added to a sampling vial, which is crimped and then allowed to sit
for 30 minutes with occasional agitation. High humidity reduces the sampling capacity. Volatile
compounds can be replaced on the sorbent by less volatile substances. The working range is dependant
on the size of the compound. For a 10-L sample, compounds with a lower molecular weight have a
working range from 45 to 140 mg/m3 and compounds with a higher molecular weight have a working
range between 175 to 680 mg/m3.
Source: http://www.cdc.gov/niosh/nmam/pdfs/1402.pdf
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4.2.43 NIOSH Method 1612: Propylene Oxide
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Propylene oxide
CASRN
75-56-9
A sample tube containing coconut shell charcoal is used for sample collection with a flow rate of 0.01 to
0.2 L/min. One milliliter of carbon disulfide (CS2) is added to the vial and allowed to sit for 30 minutes
prior to analysis with occasional agitation. No interferences have been found in this method. The
working range is between 8 to 295 ppm for air samples of 5 L.
Source: http://www.cdc.gov/niosh/nmam/pdfs/1612.pdf
4.2.44 NIOSH Method 2010: Amines, Aliphatic
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Methylamine
CASRN
74-89-5
A silica gel sorbenttube is used for sample collection with a flow rate of 0.01 to 1 L/min. An aliquot of
0.1 M H2SO4 in aqueous methanol is added to sample vials, and the vials are agitated in a sonic water
bath. Samples are neutralized using 0.3 M KOH prior to analysis by GC. Methylamine can be collected
on a sampling tube containing XAD-7 resin coated with 10%NBD chloride (7-chloro4-nitrobenzo-2-
oxa-l,3-diazole) by weight. A stable derivative is formed on the coated resin. The derivative is extracted
with 5% (w/v) NBD chloride in tetrahydrofuran (THF) and analyzed by high-performance liquid
chromatography (http://www.osha-slc.gov/dts/sltc/methods/organic/org040/org040.html). A methanol
peak can interfere with low-level analysis, and high humidity can cause reduced capacity of sample
adsorption. The working range is between 8 to 183 ppm for diethylamine and 4 to 71 ppm for
dimethylamine in air samples of 20 L.
Source: http://www.cdc.gov/niosh/nmam/pdfs/2010.pdf
4.2.45 NIOSH Method 2513: Ethylene Chlorohydrin
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
2-Chloroethanol
CASRN
1 07-07-3
Samples are drawn into a tube containing petroleum charcoal at a rate of 0.01 to 0.2 L/min and
transferred into vials containing eluent (carbon disulfide, 2-propanol, and n-pentadiene as an internal
standard). Vials must sit for 30 minutes prior to analysis. No interferences have been identified.
Humidity may decrease the breakthrough volume during sample collection. The working range of the
method is 0.5 to 15 ppm for a 20-L air sample.
Source: http://www.cdc.gov/niosh/nmam/pdfs/2513 .pdf
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4.2.46 NIOSH Method 3510: Monomethylhydrazine
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A:
Contaminant
Methyl hydrazine
CASRN
60-34-4
Samples are collected into a bubbler containing HC1 using a flow rate of 0.5 to 1.5 L/min. Samples are
then mixed with phosphomolybdic acid solution and transferred to a large test tube for analysis. Positive
interferences that have been noted include stannous ion, ferrous ion, zinc, sulfur dioxide, and hydrogen
sulfide. Negative interferences may occur by oxidation of the monomethylhydrazine by halogens,
oxygen (especially in the presence of copper (I) ions) and hydrogen dioxide. The working range of the
method is 0.027 to 2.7 ppm for a 20-L air sample.
Source: http://www.cdc.gov/niosh/nmam/pdfs/3510.pdf
4.2.47 NIOSH Method 6001: Arsine
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Arsine
CASRN
7784-42-1
In this method, arsine is determined as arsenic. A volume of 0.1 to 10 L of air is drawn through a sorbent
tube containing activated charcoal. The sorbent is extracted with a nitric acid solution. The arsine is
determined by graphite furnace atomic absorption. The working range of the method is 0.001 to 0.2
mg/m3 for a 10-L sample. The method is subject to interferences from other arsenic compounds.
Source: http://www.cdc.gov/niosh/nmam/pdfs/6001 .pdf
4.2.48 NIOSH Method 6002: Phosphine
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Phosphine
CASRN
7803-51-2
In this method, phosphine is determined as phosphate. One to 16 liters of air are drawn through a sorbent
tube containing silica gel coated with Hg(CN)2. The sorbent is extracted with a potassium permanganate/
sulfuric acid solution and washed with reagent water. Following treatment with the color agent and
extraction into organic solvent, the phosphate is determined by visible spectrometry. The working range
of the method is 0.02 to 0.9 mg/m3 for a 16-L sample. The method is subject to interferences from
phosphorus trichloride, phosphorus pentachloride, and organic phosphorus compounds.
Source: http ://www .cdc .gov/niosh/nmam/pdfs/6002 .pdf
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4.2.49 NIOSH Method 6004: Sulfur Dioxide
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Sulfur dioxide
CASRN
7446-09-5
In this method, sulfur dioxide is determined as sulfite plus sulfate. A volume of 40 to 200 liters of air is
drawn through a sodium carbonate-treated filter that is preceded by a 0.8 (im filter to remove particulates
and sulfuric acid. The treated filter is extracted with a carbonate/bicarbonate solution and the extract
analyzed by ion chromatography for sulfite and sulfate. The sulfur dioxide is present as sulfite on the
filter; however, because sulfite oxidizes to sulfate, both ions must be determined and the results summed.
The working range of the method is 0.5 to 20 mg/m3 for a 100-L sample. The method is subject to
interference from sulfur trioxide in dry conditions.
Source: http://www.cdc.gov/niosh/nmam/pdfs/6004.pdf
4.2.50 NIOSH Method 6010: Hydrogen Cyanide
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Hydrogen cyanide
CASRN
74-90-8
Hydrogen cyanide is determined as a cyanide ion complex by this method. A volume of 2 to 90 liters of
air is drawn through a soda lime sorbent tube. A glass-fiber filter is used to remove particulate cyanides
prior to the sorbent tube. Cyanide is extracted from the sorbent with reagent water. The extract is pH
adjusted and treated with the coupling-color agent. The cyanide ion is determined by visible
spectrophotometry. The working range of the method is 3 to 260 mg/m3 for a 3-L sample. The method is
subject to interference from high concentrations of hydrogen sulfide.
Source: http://www.cdc.gov/niosh/nmam/pdfs/6010.pdf
4.2.51 NIOSH Method 6011: Bromine and Chlorine
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Chlorine
CASRN
7782-50-5
In this method, chlorine is determined as chloride. A volume of 2 to 90 liters of air is drawn through a
silver membrane filter. A prefilter is used to remove particulate chlorides. The filter is extracted with
sodium hyposulfate solution, and the extract analyzed for chloride by ion chromatography. The working
range of the method is 0.02 to 1.5 mg/m3 for a 90-L sample. The method is subject to positive
interference by HC1 and negative interference by hydrogen sulfide.
Source: http://www.cdc.gov/niosh/nmam/pdfs/6011 .pdf
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4.2.52 NIOSH Method 6013: Hydrogen Sulfide
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Hydrogen sulfide
CASRN
7783-06-4
Hydrogen sulfide is determined as sulfate by this method. A volume of 1.2 to 40 liters of air is drawn
through charcoal sorbent. A prefilter is used to remove particulates. The sorbent portions are extracted
with an ammonium hydroxide/hydrogen peroxide solution and the extract is analyzed for sulfate by ion
chromatography. The working range of the method is 0.9 to 20 mg/m3 for a 20-L sample. The method is
subject to interference from sulfur dioxide.
Source: http://www.cdc.go v/niosh/nmam/pdfs/6013.pdf
4.2.53 NIOSH Method 6015: Ammonia
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Ammonia
CASRN
7664-41-7
Ammonia is determined as indophenol blue by this method. A volume of 0.1 to 96 liters of air is drawn
through a sulfuric acid-treated silca gel sorbent. A prefilter is used to remove particulates. The sorbent
is extracted with reagent water, the pH adjusted, and reagents are added to generate the indophenol blue
compound in the presence of ammonium. The extract is analyzed by visible spectrophotometry. The
working range of the method is 0.15 to 300 mg/m3 for a 10-L sample. No interferences have been
identified.
Source: http://www.cdc.gov/niosh/nmam/pdfs/6015.pdf
4.2.54 NIOSH Method 6402: Phosphorus Trichloride
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Phosphorus trichloride
CASRN
7719-12-2
In this method, phosphorus trichloride is determined as phosphate. A volume of 11 to 100 liters of air is
drawn through a bubbler containing reagent water. The resulting H3PO3 solution is oxidized to H3PO4
and color agents are added. The solution is analyzed by visible spectrophotometry. The working range
of the method is 1.2 to 80 mg/m3 for a 25-L sample. Phosphorus (V) compounds do not interfere. The
sample solutions are stable to oxidation by air during sampling.
Source: http://www.cdc.gov/niosh/nmam/pdfs/6402.pdf
SAM Revision 2.0 47 September 29, 2005
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4.2.55 NIOSH Method 7903: Acids, Inorganic
This method should be used for preparation and analysis of air samples for the contaminants identified
below and listed in Appendix A.
Contaminant
Hydrogen bromide
Hydrogen chloride
Hydrogen fluoride
CASRN
10035-10-6
7647-01-0
7664-39-3
Acids are analyzed as bromide, chloride, and fluoride, respectively, by this method. A volume of 3 to
100 liters of air is drawn through a silica gel sorbent. The sorbent portions are extracted with a buffered
carbonate/bicarbonate solution and the extract is analyzed by ion chromatography. The working range of
this method is 0.01 to 5 mg/m3 for a 50-L sample. Particulate salts of the acids are an interference
(trapped on the glass wool filter plug in the sorbent tube). Chlorine and bromine are also interferences.
Acetate, formate, and propionate interferences may be reduced by use of a weaker eluent.
Source: http://www.cdc.gov/niosh/nmam/pdfs/7903.pdf
4.2.56 NIOSH Method 7904: Cyanides, Aerosol and Gas
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Cyanide
CASRN
57-12-5
In this method, cyanide(s) are determined as cyanide ion. A volume of 10 to 180 liters of air is drawn
through a 0.8-(im PVC membrane filter and a bubbler containing 0.1N KOH solution. The filter collects
aerosols of cyanide solutions and the bubbler collects HCN. The filters are extracted with the KOH
solution. Sulfide must be removed from the solutions prior to analysis. Analyze the solutions by cyanide
ion specific electrode (ISE). The working range of the method is 0.5 to 15 mg/m3 for a 90-L sample.
Sulfide, chloride, iodide, bromide, cadmium, zinc, silver, nickel, cuprous iron, and mercury are
interferences.
Source: http://www.cdc.gov/niosh/nmam/pdfs/7904.pdf
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4.2.57 NIOSH Method 7906: Fluorides, Aerosol and Gas
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Hydrogen fluoride
CASRN
7664-39-3
Hydrogen fluoride is determined as fluoride ion by this method. A volume of 1 to 800 liters of air is
drawn through a 0.8-(im cellulose ester membrane (to trap particulate fluorides) and a cellulose pad
treated with sodium carbonate (to trap gaseous fluoride). The pad is extracted with reagent water and the
extract is analyzed for fluoride by ion chromatography. The working range of the method is 0.04 to 8
mg/m3 for 250-L samples. If other aerosols are present, gaseous fluoride may be slightly underestimated
owing to adsorption onto or reaction with particles; with concurrent overestimation of
particulate/gaseous fluoride ratio.
Source: http://www.cdc.gov/niosh/nmam/pdfs/7906.pdf
4.2.58 NIOSH Method S301-1: Fluoroacetate Anion
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Fluoroacetate salts
CASRN
NA
This method was developed specifically for sodium fluoroacetate, but also may be applicable to other
fluoroacetate salts. A known volume of air (e.g., 480 L was used in validation of this method), is drawn
through a cellulose ester membrane filter to collect sodium fluoroacetate. Sodium fluoroacetate is
extracted from the filter with 5 mL of deionized water, and the resulting sample is analyzed by ion
chromatography using electrolytic conductivity detection. The analytical range of this method is
estimated to be 0.01 to 0.16 mg/m3. The detection limit of the analytical method is estimated to be 20 ng
of sodium fluoroacetate per injection, corresponding to a 100-u.L aliquot of a 0.2-u.g/mL standard.
Source: http://www.cdc.gov/niosh/pdfs/s301 .pdf
4.2.59 OSHA Method ID-188: Ammonia in Workplace Atmospheres - Solid Sorbent
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Ammonia
CASRN
7664-41-7
In this method, ammonia is determined as ammonium ion. A volume of 7.5 to 24 liters of air is drawn
through a sulfuric acid-treated carbon bead sorbent. The sorbent is extracted with reagent water and the
extract analyzed for ammonium by ion chromatography. The detection limit for the method is 0.60 ppm
for 24-L samples and the quantitation limit is 1.5 ppm for 24-L samples. Volatile amines,
monethanolamine, isopropanolamine, and propanolamine may be interferences. Particulate ammonium
salts can be a positive interference (trapped on the glass wool filter plug in the sorbent tube).
Source: http://www.osha-slc.gov/dts/sltc/methods/inorganic/idl88/idl88.html
SAM Revision 2.0 49 September 29, 2005
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4.2.60 OSHA Method ID-216SG: Boron Trifluoride (BF3)
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Boron trifluoride
CASRN
7637-07-2
Boron trifluoride is determined as fluoroborate by this method. A volume of 30 to 480 liters of air is
drawn through a bubbler containing 0.1-M ammonium fluoride. The solution is diluted and analyzed
with a fluoroborate ion specific electrode (ISE). The detection limit is 10 (ig in a 30-L sample.
Source: http://www.osha-slc.gov/dts/sltc/methods/partial/id216sg/id216sg.html
4.2.61 Standard Method 4110 B: Ion Chromatography with Chemical Suppression of
Eluent Conductivity
This method should be used for preparation and analysis of aqueous/liquid and drinking water samples
for the contaminants identified below and listed in Appendix A.
Contaminant
Hydrogen bromide
Hydrogen chloride
CASRN
10035-10-6
7647-01-0
The contaminants are determined as bromide and chloride respectively by this method. Aqueous/liquid
samples are pre-filtered and injected onto the ion chromatograph. The anions are identified on the basis
of retention time and quantified by measurement of peak area or height. The method can detect bromide
and chloride at 0.1 mg/L. Lower values can be achieved using a higher scale setting and an electronic
integrator. Other salts of the anions are a positive interference. Low molecular weight organic acids may
interfere with chloride.
Source: American Public Health Association, American Waterworks Association, and Water
Environment Federation. 1998. Standard Methods for the Examination of Water and Wastewater. 20th
Edition, (http://www.standardmethods.org/')
4.2.62 Standard Method 4500-NH3 B: Preliminary Distillation Step
This method should be used for preparation of aqueous/liquid samples for the contaminant identified
below and listed in Appendix A. Note: Method 4500-NH3 G should be used for sample analysis.
Contaminant
Ammonia
CASRN
7664-41-7
A 0.5-L to 1-L water sample is dechlorinated, buffered, adjusted to pH 9.5, and distilled into a sulfuric
acid solution. The distillate is brought up to volume and neutralized with sodium hydroxide. The
distillate is analyzed by Method 4500-NH3 G.
Source: American Public Health Association, American Water Works Association, and Water
Environment Federation. 1998. Standard Methods for the Examination of Water and Wastewater. 20th
Edition, (http://www.standardmethods.org/')
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4.2.63 Standard Method 4500-NH, G: Automated Phenate Method
This method should be used for analysis of aqueous/liquid samples for the contaminant identified below
and listed in Appendix A.
Contaminant
Ammonia
CASRN
7664-41-7
Ammonia is determined as indophenol blue by this method. A portion of the neutralized distillate from
procedure 4500-NH3 B is run through the manifold decribed in the method. The ammonium in the
distillate reacts with solutions of disodium EDTA, sodium phenate, sodium hypochlorite, and sodium
nitroprusside. The resulting indophenol blue is detected by colorimetry in a flow cell. The range of the
method is 0.02 to 2.0 mg/L.
Source: American Public Health Association, American Water Works Association, and Water
Environment Federation. 1998. Standard Methods for the Examination of Water and Wastewater. 20th
Edition, (http://www.standardmethods.org/)
4.2.64 Standard Method 4500-CI G: DPD Colorimetric Method
This method should be used for preparation and analysis of aqueous/liquid and drinking water samples
for the contaminant identified below and listed in Appendix A.
Contaminant
Chlorine
CASRN
7782-50-5
A portion of aqueous/liquid sample is buffered and reacted with N,N-diethyl-p-phenylenediamine (DPD)
color agent. The resulting free chlorine is determined by colorimetry. If total chlorine (including
chloroamines and nitrogen trichloride) is to be determined, KI crystals are added. Results for chromate
and manganese are blank corrected using thioacetamide solution. The method can detect 10 (ig/L
chlorine. Organic contaminants and strong oxidizers may cause interference.
Source: American Public Health Association, American Waterworks Association, and Water
Environment Federation. 1998. Standard Methods for the Examination of Water and Wastewater. 20th
Edition, (http://www.standardmethods.org/)
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4.2.65 IO Compendium Method IO-3.1: Selection, Preparation, and Extraction of Filter
Material
This method should be used for preparation and analysis of air samples for the contaminants identified
below and listed in Appendix A.
Contaminant
Arsenic (III) compounds
Arsenic trichloride
Cadmium
CASRN
22569-72-8
7784-34-1
7440-43-9
This method will determine arsenic (IE) compounds and arsenic trichloride as arsenic. A subsample
(one-ninth of the overall filter) is obtained by cutting a strip from the filter used to collect the sample.
The filter strip is extracted using hydrochloric/nitric acid mix and microwave or hotplate heating. The
extract is filtered and worked up to 20 mL. The extract is analyzed by compendium methods IO-3.4 or
IO-3.5.
Source: http://www.epa.gov/ttn/amtic/files/ambient/inorganic/mthd-3-l.pdf
4.2.66 IO Compendium Method IO-3.4: Determination of Metals in Ambient Particulate
Matter Using Inductively Coupled Plasma (ICP) Spectroscopy
This method should be used for preparation and analysis of air samples for the contaminants
identified below and listed in Appendix A.
Contaminant
Arsenic (III) compounds
Arsenic trichloride
Cadmium
Osmium tetraoxide
CASRN
22569-72-8
7784-34-1
7440-43-9
20816-12-0
All analytes are determined as the metal by this method. Ambient air is sampled by high-volume filters
using compendium method IO-2.1 (a sampling method). The filters are extracted by compendium
method IO-3.1 and the extracts analyzed by Inductively Coupled Plasma -Atomic Emission Spectroscopy
(ICP-AES). Detection limits, ranges, and interference corrections are dependent on the analyte and the
instrument used.
Source: http://www.epa.gov/ttn/amtic/files/ambient/inorganic/mthd-3-4.pdf
http://www.epa.gov/ttn/amtic/files/ambient/inorganic/mthd-2-l.pdf
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4.2.67 IO Compendium Method IO-3.5: Determination of Metals in Ambient Participate
Matter Using Inductively Coupled Plasma/Mass Spectrometry (ICP/MS)
This method should be used for preparation and analysis of air samples for the contaminants identified
below and listed in Appendix A.
Contaminant
Arsenic (III) compounds
Arsenic trichloride
Cadmium
CASRN
22569-72-8
7784-34-1
7440-43-9
All analytes are determined as the metal by this method. Ambient air is sampled by high-volume filters
using compendium method IO-2.1 (a sampling method). The filters are extracted by compendium
method IO-3.1 and the extracts analyzed by Inductively Coupled Plasma/Mass Spectrometry (ICP/MS).
Detection limits, ranges, and interference corrections are dependent on the analyte and the instrument
used.
Source: http://www.epa.gov/ttn/amtic/files/ambient/inorganic/mthd-3-5.pdf
http: //www. epa. go v/ttn/amtic/file s/ambient/inorganic/mthd-2-1 .pdf
4.2.68 IO Compendium Method IO-5: Sampling and Analysis for Vapor and Particle
Phase Mercury in Ambient Air Utilizing Cold Vapor Atomic Fluorescence
Spectrometry (CVAFS)
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Mercury
CASRN
7439-97-6
Vapor phase mercury is collected using gold-coated glass bead traps at a flow rate of 0.3 L/min. The
traps are directly desorbed onto a second (analytical) trap. The mercury desorbed from the analytical
trap is determined by Atomic Fluorescence Spectrometry. Particulate mercury is sampled on glass-fiber
filters at a flow rate of 30 L/min. The filters are extracted with nitric acid and microwave heating. The
extract is oxidized with BrCl, then reduced with stannous chloride and purged from solution onto a gold-
coated glass bead trap. This trap is desorbed onto a second trap, the second trap is desorbed, and the
mercury is determined by Atomic Fluorescence Spectrometry. The detection limits are 30 pg/m3 for
particulate mercury and 45 pg/m3 for vapor mercury. Detection limits, analytical range, and interferences
are dependent on the instrument used. There are no known positive interferences at 253.7 nm
wavelength. Water vapor will cause a negative interference.
Source: http://www.epa.gov/ttn/amtic/files/ambient/inorganic/mthd-5.pdf
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4.2.69 EPA Air Method, Toxic Organics - 6 (TO-6): Method for the Determination of
Phosgene in Ambient Air Using High Performance Liquid Chromatography
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Phosgene
CASRN
75-44-5
This method can be used to detect phosgene in air at the 0.1 ppbv level. Ambient air is drawn through a
midget impinger containing 10 mL of 2/98 aniline/toluene (by volume). Phosgene readily reacts with
aniline to form carbanilide (1,3-diphenylurea), which is stable indefinitely. After sampling, the impinger
contents are transferred to a screw capped vial having a Teflon-lined cap and returned to the laboratory
for analysis. The solution is heated to dryness and the residue is dissolved in acetonitrile. Carbanilide is
determined in the acetonitrile solution using reverse-phase HPLC with an ultraviolet (UV) absorbance
detector operating at 254 nm. Precision for phosgene spiked into a clean air stream is ±15 to 20%
relative standard deviation. Recovery is quantitative within that precision, down to less than 3 ppbv.
Source: http://www.epa.gov/ttn/amtic/files/ambient/airtox/to-6.pdf
4.2.70 EPA Air Method, Toxic Organics - 10A (TO-10A): Determination of Pesticides and
Polychlorinated Biphenyls in Ambient Air Using Low Volume Polyurethane Foam
(PUF) Sampling Followed by Gas Chromatographic/Multi-Detector Detection (GC/
MD)
This method should be used for sampling and analysis of ambient air samples for the contaminants
identified below and listed in Appendix A.
Contaminant
Carbofuran (Furadan)
Dichlorvos
Dicrotophos
Dimethylphosphite
Fenamiphos
Methyl parathion
Mevinphos
Phencyclidine
Phenol
Phorate
Polychlorinated biphenyls (PCBs)
Semivolatile Organic Compounds, NOS *
Tear gas (CS) [chlorobenzylidene malonitrile]
Tetraethyl pyrophosphate
CASRN
1 563-66-2
62-73-7
141-66-2
868-85-9
22224-92-6
298-00-0
7786-34-7
77-10-1
108-95-2
298-02-2
1336-36-3
NA
2698-41-1
107-49-3
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Contaminant
Tetramethylenedisulfotetramine
Trimethyl phosphite
VE
VG
VM
VX [O-ethyl-S-(2-di isopro pylami noethyl )methyl
phosphonothiolate]
CASRN
80-12-6
121-45-9
21738-25-0
78-53-5
21770-86-5
50782-69-9
* NOS = Not otherwise specified
A low-volume (1 to 5 L/minute) sample is used to collect vapors on a sorbent cartridge containing PUF
or PUF in combination with another solid sorbent. Airborne particles may also be collected, but the
sampling efficiency is not known. Pesticides and other chemicals are extracted from the sorbent
cartridge with 5% diethyl ether in hexane and determined by gas chromatography coupled with an
electron capture detector (BCD). Nitrogen-phosphorous detector (NPD), flame photometric detector
(FPD), Hall electrolytic conductivity detector (HECD), or mass spectrometer (MS) also maybe used.
This method is applicable to multicomponent atmospheres, 0.001 to 50 (ig/m3 concentrations, and 4 to
24-hour sampling periods. The limit of detection will depend on the specific compounds measured, the
concentration level, and the degree of specificity required.
Source: http://www.epa.gov/ttnamti 1 /files/ambient/airtox/to-1 Oar.pdf
4.2.71 EPA Air Method, Toxic Organics -15 (TO-15): Determination of Volatile Organic
Compounds (VOCs) in Air Collected in Specially-Prepared Canisters and Analyzed
by Gas Chromatography/Mass Spectrometry (GC/MS)
This method should be used for preparation and analysis of air samples for the contaminants identified
below and listed in Appendix A.
Contaminant
Carbon disulfide
3-Chloro-1 ,2-propanediol
Chloropicrin
Chlorosarin
Chlorosoman
2-Chlorovinylarsonous acid (CVAA)
Cyanogen chloride
Cyclohexyl sarin (GF)
1,2-Dichloroethane
Diisopropyl methylphosphonate (DIMP)
Dimethylphosphoramidic acid
CASRN
75-15-0
96-24-2
76-06-2
1445-76-7
7040-57-5
85090-33-1
506-77-4
329-99-7
107-06-2
1445-75-6
33876-51-6
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Contaminant
1,4-Dithiane
EA2192
Ethyldichloroarsine (ED)
Ethylene oxide
Ethylmethyl phosphonate (EMPA)
GE (1-methylethyl ester ethyl-phosphonofluoridic acid)
Isopropyl methylphosphonic acid (IMPA)
Lewisite 1 (L-1) [2-chlorovinyldichloroarsine]
Lewisite 2 (L-2) [bis(2-chlorovinyl)-chloroarsine]
Lewisite 3 (L-3) [tris(2-chlorovinyl)-arsine]
Lewisite oxide
Methylphosphonic acid (MPA)
Mustard, nitrogen (HN-2) [unstable compound]
Mustard, sulfur (HD) / Mustard gas (H)
Oxamyl
Perfluoroisobutylene (PFIB)
Phosgene
Sarin (GB)
Soman (GD)
Tabun (GA)
Thiodiglycol (TDG)
1,4-Thioxane
Volatile Organic Compounds, NOS *
CASRN
505-29-3
73207-98-4
598-14-1
75-21-8
1 832-53-7
1189-87-3
1 832-54-8
541-25-3
40334-69-8
40334-70-1
1306-02-1
993-13-5
51-75-2
505-60-2
23135-22-0
382-21-8
75-44-5
107-44-8
96-64-0
77-81-6
111-48-8
15980-15-1
NA
* NOS = Not otherwise specified
The atmosphere is sampled by introduction of air into a specially prepared stainless steel canister
(specially electropolished or silica-coated). A sample of air is drawn through a sampling train
comprising components that regulate the rate and duration of sampling into the pre-evacuated and
passivated canister. Grab samples also may be collected. After the air sample is collected, the canister
valve is closed, an identification tag is attached to the canister, and the canister is transported to the
laboratory for analysis. To analyze the sample, a known volume of sample is directed from the canister
through a solid multisorbent concentrator. After the concentration and drying steps are completed, the
VOCs are thermally desorbed, entrained in a carrier gas stream, and then focused in a small volume by
trapping on a cryo-focusing (ultra-low temperature) trap or small volume multisorbent trap. The sample
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is then released by thermal desorption and analyzed by GC/MS. This method applies to ambient
concentrations of VOCs above 0.5 ppbv and typically requires VOC enrichment by concentrating up to 1
L of a sample volume.
Source: http://www.epa. gov/ttn/amtic/files/ambient/airtox/to-15r.pdf
4.2.72 Journal of Analytical Atomic Spectrometry, 2000, 15, pp. 277-279: Boron
Trichloride Analysis
This method should be used for preparation and analysis of air samples for the contaminant identified
below and listed in Appendix A.
Contaminant
Boron trichloride
CASRN
10294-34-5
An analytical procedure is described for the determination of boron trichloride by ICP-AES. A modified
sampling and gas introduction system allows on-line monitoring of the investigated gas. The air sample
is introduced into an aqueous mannitol solution, and the boron trichloride hydrolyzed to boric acid.
Since this method is designed for measuring boron in trichlorosilane, the detection limit was found to be
0.63 |ig of boron/g dichlorosilane.
Source: Eschwey, M., Pulvermacher E., Benninghoff, C., and Telgheder, U., "On-line monitoring of
boron in dichlorosilane by means of inductively coupled plasma atomic emission spectrometry,'" Royal
Society of Chemistry. Journal of Analytical Atomic Spectrometry, 2000, 15, pp. 277-279.
http://pubs.rsc.org/ei/JA/2000/a908634i.pdf
4.2.73 Analytical Letters, 1994, 27 (14), pp. 2703-2718: Screening-Procedure for Sodium
Fluoroacetate (Compound 1080) at Sub-Microgram/Gram Concentrations in Soils
This method should be used for preparation and analysis of solid and oily solid samples for the
contaminant identified below and listed in Appendix A.
Contaminant
Fluoroacetate salts
CASRN
NA
Sodium fluoroacetate is readily quantitated at sub-microgram per gram concentrations in small (ca. 1-g)
soil samples. Samples are ultrasonically extracted with water, which is then partitioned with hexane, and
acidified prior to re-extraction with ethyl acetate. The latter is taken to dryness in the presence of
triethanolamine "keeper," and the resulting acid is derivatized with pentafluorobenzyl bromide.
Quantitation is performed using a gas chromatograph equipped with an electron-capture detector. A
standardized statistical protocol is used to verify a screening level of 0.2 u,g sodium fluoroacetate/g soil.
Difluoroacetic, trifluoroacetic, and naturally occurring formic acids do not interfere with the
determination. The recovery for sodium fluoroacetate was 40% from soil fortified to 0.2 (ig/g soil.
Source: Tomkins, B.A., "Screening-Procedure for Sodium Fluoroacetate (Compound 1080) at Sub-
Microgram/Gram Concentrations in Soils," Analytical Letters. 27(14), 2703-2718 (1994).
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Section 5.0: Biological Methods
The purpose of this section is to provide analytical methods for the analysis of environmental samples for
biological agents in response to a homeland security event.
Protocols from peer-reviewed journal articles have been identified for analyte-matrix pairs where
standardized methods are not available. It should be noted that the limitations of these protocols are not
the same as the limitations of the standardized methods that have been identified. Future steps include
the development of standardized methods based on journal protocols. The literature references will be
replaced with standardized, verified protocols as they become available.
Although culture-based methods have been selected for the bacterial pathogens, PCR techniques will be
used for viruses because of the difficulty and time required to propagate these agents in host cell cultures.
It should be noted that PCR techniques have inherent limitations with regard to the determination of
viability or infectivity of the analyte.
Sample collection and handling protocols are not available for all analyte-matrix combinations included
in this document. Future research will include the development and validation of sampling protocols and
sample preparation procedures to support the specified analytical methods.
A list of analytical methods to be used in analyzing environmental samples for biological contaminants
during homeland security events is provided in Appendix B. Methods are listed for each analyte and for
each sample matrix that potentially may need to be measured and analyzed when responding to an
environmental emergency. The methods tables in Appendix B-l, B-2, and B-3 are sorted alphabetically
by analyte under each agent category (i.e., bacteria, biotoxins, viruses, and protozoa). Appendix B-l lists
methods to be used for waterborne analytes (both wastewater and drinking water). Appendix B-2 lists
methods to be used for dustborne analytes and Appendix B-3 lists methods to be used for aerosolized
analytes. Each appendix includes the following information:
• Analyte(s). The contaminant or contaminant(s) of interest.
Determinative technique. An analytical instrument or technique used to determine the identity,
quantity, and/or viability of a biological agent.
• Determinative method identifier. The unique identifier or number assigned to an analytical
method by the method publisher.
Sample preparation procedure and/or sampling method. The recommended sample preparation
procedure and/or sample collection procedure for the analyte-matrix combination.
• Identification Procedure. A procedure used to establish the identity of a specific biological agent
or a group of similar biological agents.
Viability Procedure. For the purposes of this document, a procedure used to directly or indirectly
evaluate the growth potential and/or replication of an organism under permissive conditions. For
example, the proliferation of bacteria in culture is a direct indication of viability whereas the ability
of some organisms (viruses and protozoa particularly) to infect, replicate, and cause a detectable
alteration in a suitable host system (cell culture, animal or human) is an indirect measurement of
viability.
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5.1 General Guidance
The guidance summarized in this section provides a general overview of how to identify the appropriate
biological method(s) for a given analyte-matrix combination as well as recommendations for quality
control procedures.
For additional information on the properties of the biological agents listed in Appendix B, TOXNET
(http://toxnet.nlm.nih.gov/index.html'). a cluster of databases on toxicology, hazardous chemicals, and
related areas maintained by the National Library of Medicine is an excellent resource. Additional
information also can be found on CDC's Emergency Preparedness and Response Web site
(http://www.bt.cdc.gov/'). Further research on biological agents is ongoing within EPA and databases to
manage this information are currently under development.
5.1.1 Standard Operating Procedures for Identifying Biological Methods
To determine the appropriate method and sample preparation procedure and/or sampling method that is
to be used on the environmental samples, determine the matrix of interest and locate the appropriate
biological appendix (B-l, B-2, or B-3).
After locating the correct appendix, find the analyte of interest and continue across the table to identify
the appropriate identification determinative technique, viability determinative technique, determinative
method, and sample preparation procedure and/or sampling method for the analyte of interest.
Sections 5.2.1 through 5.2.19 below provide summaries of the analytical methods listed in Appendix B.
Where available, a direct link to the full text of the selected method is provided in the method summary.
For additional information on preparation procedures and methods available through consensus standards
organizations, please use the contact information provided in Table 2.
Table 2. Sources of Biological Methods
Name
National Environmental Methods Index
(NEMI)
U.S. EPA Microbiology Methods
USDA/FSIS Microbiology Laboratory
Guidebook
ICR Microbial Laboratory Manual
Occupational Safety and Health
Administration Methods
National Institutes for Occupational
Safety and Health Methods
Publisher
EPA, USGS
EPA
USDA Food Safety and
Inspection Service
EPA Office of Research and
Development
OSHA
NIOSH
Reference
http://vwwv.nemi.gov
http://www.epa.qov/microbes/
http://www.fsis.usda.qov/OPHS/microla
b/mlqbook.htm
http://www.epa.qov/nerlcwww/icrmicro.
2df
http://www.osha-slc.qov/dts/sltc/method
s/toc.html
http://www.cdc.qov/niosh/nmam/
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Name
Standard Methods for the Examination
of Water and Wastewater, 20th Edition,
1998*
Annual Book of ASTM Standards*
Applied and Environmental
Microbiology*
Journal of Clinical Microbiology*
Publisher
American Public Health
Association (APHA),
American Water Works
Association (AWWA), and
Water Environment
Federation (WEF)
ASTM International
American Society for
Microbiology
American Society for
Microbiology
Reference
http://wvwv.standardmethods.orq
http://www.astm.orq
http://www.asm.orq
http://www.asm.org
Subscription and/or purchase required.
5.1.2 General Quality Control (QC) Guidance for Biological Methods
As with analysis of chemical analytes, the level or amount of quality control (QC) needed during sample
analysis and reporting to address biological analytes depends on the intended purpose of the data. The
specific decisions that will be made should be identified, and quality goals (including QC requirements)
for data generation should be derived based on those decisions. Analytical data of known and
documented quality is a critical factor in the accurate assessment of and appropriate response to
emergency situations. The generation of data of sufficient quality requires that analytical laboratories:
(1) conduct the appropriate QC procedures to ensure that all measurement systems are in control and
operating properly, (2) properly document all analytical results, and (3) properly document analytical QC
procedures and corrective actions.
The specific level and amount of QC procedures required during sample analysis and data reporting
depends on the intended purpose of the data. Individual methods, sampling and analytical protocols, or
contractual statements of work should be consulted to determine if additional QC procedures are
required. Method-specific QC requirements are described in many of the individual methods cited in this
manual and will be included in protocols developed to address specific analyte-matrix combinations of
concern. In general, analytical QC requirements for biological methods include an initial demonstration
of measurement system capability as well as ongoing analysis of control samples to ensure the continued
reliability of the analytical results. At a minimum, the following QC analyses should be conducted on an
ongoing basis for biological analytes:
• Media and reagent sterility checks
• Positive and negative controls
Method blanks
• Matrix spikes to evaluate method performance in the matrix of interest
• Matrix spike duplicates (MSB) and/or sample replicates to assess method precision
QC procedures should be performed as frequently as necessary to ensure the reliability of analytical
results. As with the identification of needed QC samples, frequency should be established based on an
evaluation of data quality objectives.
Please note: The appropriate point of contact identified in Section 3 should be consulted regarding
appropriate quality assurance and quality control (QA/QC) procedures prior to sample analysis. These
contacts will consult with their respective QA/QC managers regarding QA/QC issues.
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5.1.3 Safety and Waste Management
It is imperative that safety precautions are used during collection, processing, and analysis of
environmental samples, particularly in emergency response situations that may include unknown hazards.
Many of the methods summarized or cited in Section 5.2 contain specific requirements, guidance, or
information regarding safety precautions that should be followed when handling or processing
environmental samples and reagents. These methods also provide information regarding waste
management. Additional resources that can be consulted for additional information include the
following:
• Environmental Protection Agency's standards regulating hazardous waste (40 CFR parts 260 - 270)
Biosafety in Microbiological and Biomedical Laboratories, 4th Edition, found at
www.cdc.gov/od/ohs/biosfty/bmbl4toc.htm
Laboratory Security and Emergency Response Guidance for Laboratories Working with Select
Agents, December 6, 2002 / 51 (RR19); 1-8, found at
www.cdc.gov/mmwr/preview/mmwrhtml/rr5119al .htm.
5.2 Method Summaries
Method summaries for the analytical methods listed in Appendix B are provided in Sections 5.2.1
through 5.2.19. Each method summary contains atable identifying the contaminants in Appendix B to
which the method applies, provides a brief description of the analytical method, and includes a link (if
available) to the full version of the method or source for obtaining a full version of the method.
Please note: Not all methods have been verified for the analyte/matrix combination listed in Appendix B.
Please refer to the specified method to identify analyte/matrix combinations that have been verified. Any
questions regarding information discussed in this section should be addressed to the appropriate
contact(s) listed in Section 3.
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5.2.1 Laboratory Response Network (LRN)
The agents identified below and listed in Appendix B should be analyzed in accordance with the
appropriate LRN protocols.
Analyte(s)
Bacillus anthracis (Anthrax)
Brucella spp. (Brucellosis)
Burkholderia mallei (Glanders)
Burkholderia pseudomallei (Melioidosis)
Coxiella burnetti (Q-fever)
Francisella tularensis (Tularemia)
Rickettsia prowazekii (Epidemic Typhus)
Yersinia pestis (Plague)
Agent Category
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
These agents will be analyzed using restricted procedures available only through the Laboratory
Response Network (LRN). These procedures are not available to the general laboratory community and
thus are not discussed within this document. For additional information on the LRN, please use the
contact information provided below or visit http://www.bt.cdc.gov/lrn/.
Centers for Disease Control and Prevention
Laboratory Response Branch
Bioterrorism Preparedness and Response Program
National Center for Infectious Diseases
1600 Clifton Road NE, Mailstop C-18
Atlanta, GA 30333
Telephone: (404) 639-2790
E-mail: lrn@cdc.gov
Local public health laboratories, private laboratories, and commercial laboratories with questions about
the LRN should contact their State public health laboratory director or the Association of Public Health
Laboratories (contact information provided below).
Association of Public Health Laboratories
2025 M Street NW, Suite 550
Washington, DC 2003 6
Telephone: (202) 822-5227
Fax: (202) 887-5098
Web site: www.aphl.org
E-mail: info@aphl.org
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5.2.2 Biosafety Level 4 Viruses
Samples to be analyzed for the viruses identified below and listed in Appendix B should be analyzed
under biosafety level (BSL) 4 conditions at the Centers for Disease Control and Prevention (CDC).
Analyte(s)
Arenaviruses (Hemorrhagic fever)
Bunyaviruses (Hemorrhagic fever)
Filoviruses (Hemorrhagic fever)
Flaviviruses (Hemorrhagic fever)
Orthopoxvirus: Monkey pox
Orthopoxvirus: Variola major (Smallpox)
Agent Cateory
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
For additional information on the BSL 4 laboratories, please use the contact information provided below
or visit http://www.bt.cdc.gov/lrn/.
Centers for Disease Control and Prevention
Laboratory Response Branch
Bioterrorism Preparedness and Response Program
National Center for Infectious Diseases
1600 Clifton Road NE, Mailstop C-18
Atlanta, GA 30333
Telephone: (404) 639-2790
E-mail: lrn@cdc.gov
5.2.3 Standard Methods 9260 B: Salmonella typhi
This method should be used for the identification and viability assessment of Salmonella typhi in water,
dust, and aerosol samples.
Analyte(s)
Salmonella typhi (Typhoid fever)
Agent Category
Bacteria
Concentrated samples are enriched in either selenite cystine, selenite-F, or tetrathionate broths and
incubated at 35°C - 37°C for up to five days. An aliquot from each turbid tube is streaked onto bismuth
sulfite (BS) plates and incubated at 35°C - 37°C for 24 - 48 hours. Presumptive positive colonies are
then subjected to biochemical characterization and serological confirmation using polyvalent O and Vi
antiserum.
Please note: This procedure has not been fully verified. At a minimum, the following sample processing
quality control checks should be performed and evaluated before using this protocol: positive control,
negative control, and blank. This method was originally developed for water matrices; further research
will be required to develop and standardize sample processing protocols for other matrices.
Source: American Public Health Association, American Water Works Association, and Water
Environment Federation. 1998. Standard Methods for the Examination of Water and Wastewater. 20th
Edition, (http://www.standardmethods.org/)
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5.2.4 Standard Methods 9260 E: Shigella species
This method should be used for the identification and viability assessment of Shigella species in water,
dust, and aerosol samples.
Analyte(s)
Shigella species (Shigellosis)
Agent Category
Bacteria
This method contains two options for sample concentration: membrane filtration (liquid matrices) and
centrifugation (liquid and solid matrices) for analyses. Both options include inoculation of an
enrichment medium (Selenite F broth). Isolation of the target analyte is achieved by plating onto XLD
and/or MacConkey agar. Biochemical identification consists of inoculating TSI and LIA slants.
Serological grouping is done by slide agglutination tests using polyvalent antisera. Serotyping for S.
dysenteriae, S.flexneri, and S. boydii may be performed at State Health laboratories or CDC.
Please note: This procedure has not been fully verified. At a minimum, the following sample processing
quality control checks should be performed and evaluated before using this protocol: positive control,
negative control, and blank. This method was originally developed for water matrices; further research
will be required to develop and standardize sample processing protocols for other matrices.
Source: American Public Health Association, American Waterworks Association, and Water
Environment Federation. 1998. Standard Methods for the Examination of Water and Wastewater. 20th
Edition, (http://www.standardmethods.org/)
5.2.5 Standard Methods 9260 F: Pathogenic Escherichia coli
This method should be used for the identification and viability assessment of Escherichia coli in water,
dust, and aerosol samples.
Analyte(s)
Escherichia coli (E. coli) O157:H7
Agent Category
Bacteria
This method allows for two options, one being a modification of SM 9221 B followed by plating and
biochemical identification. The second option, modification of a food method, allows for the analysis of
large sample volumes. A 200-mL water sample is centrifuged, resuspended in E. coli enrichment broth
(EEB) and incubated for 6 hours. Tellurite Cefixime SMAC (TC SMAC) plates are inoculated with the
enriched EEB culture. The TC SMAC plates are incubated for up to 24 hours. Colorless colonies on TC
SMAC are tested for indole production. Additional biochemical tests and serotyping are also done to
confirm identification.
Please note: This procedure has not been fully verified. At a minimum, the following sample processing
quality control checks should be performed and evaluated before using this protocol: positive control,
negative control, and blank. This method was originally developed for liquid matrices; further research
will be conducted to develop and standardize sample processing protocols for other matrices.
Source: American Public Health Association, American Water Works Association, and Water
Environment Federation. 1998. Standard Methods for the Examination of Water and Wastewater. 20th
Edition, (http://www.standardmethods.org/')
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5.2.6 Standard Methods 9260 G: Campylobacterjejuni
This method should be used for the identification and viability assessment of Campylobacterjejuni in
water, dust, and aerosol samples.
Analyte(s)
Campylobacterjejuni
Agent Category
Bacteria
Water samples (1 to several liter volumes) are filtered using a cellulose nitrate membrane filter. Filters
are placed face down on either Skirrow's medium or Campy-BAP and incubated for 24 hours at 42°C.
Filters are then transferred to another selective medium face-down and incubated for a total of 5 days at
42°C under microaerophilic conditions. Identification is made by culture examination, microscopy,
motility test, and biochemical testing. Biochemical tests include oxidase, catalase, nitrite and nitrate
reduction, H2S production, and hippurate hydrolysis. Serotyping is done using commercially available
rapid test kits. Skirrow's and other selective media containing antibiotics may prevent the growth of
injured organisms.
Please note: This procedure has not been fully verified. At a minimum, the following sample processing
quality control checks should be performed and evaluated before using this protocol: positive control,
negative control, and blank. This method was originally developed for water matrices; further research
will be conducted to develop and standardize sample processing protocols for other matrices.
Source: American Public Health Association, American Waterworks Association, and Water
Environment Federation. 1998. Standard Methods for the Examination of Water and Wastewater. 20th
Edition, (http://www.standardmethods.org/')
5.2.7 Standard Methods 9260 H: Vibrio cholerae
This method should be used for the identification and viability assessment of Vibrio cholerae in water,
dust, and aerosol samples.
Analyte(s)
Vibrio cholerae (Cholera)
Agent Category
Bacteria
Samples are enriched in alkaline peptone broth and incubated for up to 8 hours. Thiosulfate-citrate-bile
salts-sucrose TCBS agar plates are inoculated with the incubated broth and incubated for 24 hours.
Vibrio cholerae isolates are plated on tryptic soy agar with 0.5% NaCl. Biochemical confirmation is
done using multiple tests including but not limited to ONPG, Indole, and Voges-Proskauer. Slide
agglutination assays are used for serological identification.
Please note: This procedure has not been fully verified. At a minimum, the following sample processing
quality control checks should be performed and evaluated before using this protocol: positive control,
negative control, and blank. This method was originally developed for water matrices, further research
will be conducted to develop and standardize sample processing protocols for other matrices.
Source: American Public Health Association, American Waterworks Association, and Water
Environment Federation. 1998. Standard Methods for the Examination of Water and Wastewater. 20th
Edition, (http://www.standardmethods.org/')
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5.2.8 Literature Reference for Enteric Viruses (Applied and Environmental
Microbiology. 69(6): 3158-3164)
This method should be used for the identification of Enteroviruses, Hepatitis A virus, and Rotavirus
(Group A) in water, dust, and aerosol samples.
Analyte(s)
Picornaviruses: Enteroviruses
Picornaviruses: Hepatitis A virus (HAV)
Reoviruses: Rotavirus (Group A)
Agent Category
Viruses
Viruses
Viruses
This method is used to detect human enteric viruses (enteroviruses, HAV, rotavirus) in groundwater
samples. It is a multiplex reverse-transcription PCR (RT-PCR) procedure optimized for the simultaneous
detection of enteroviruses, hepatitis A virus (HAV), reoviruses, and rotaviruses. Water samples are
collected by filtration (1 MDS filter) and viruses are eluted using a beef extract solution (1.5%, pH 9.5).
Viruses are concentrated using celite adsorption (pH 4.0), filtration, and celite-elution with sodium
phosphate (0.15 M, pH 9.0), followed by further concentration and processing to remove inhibitors
(ultracentrifugation, solvent extraction, and MW-exclusion filtration). Concentrated samples are
analyzed by a two-step multiplex RT-PCR (RT followed by PCR) using virus-specific primer sets.
Detection of amplicons is by gel electrophoresis with subsequent confirmation by hybridization (dot-blot)
using digoxigenin-labeled internal (nested) probes.
Please note: This procedure has not been fully verified. At a minimum, the following sample processing
quality control checks should be performed and evaluated before using this protocol: positive control,
negative control, and blank. PCR quality control checks should be performed according to EPA Draft
Quality Assurance/Quality Control Guidance for Laboratories Performing PCR Analyses on
Environmental Samples document (www.epa.gov/nerlcwww/qa qc_pcr 10 04.pdf) or call the point of
contact identified in Section 3. This method was originally developed for water matrices; further
research will be conducted to develop and standardize sample processing protocols for other matrices.
Source: Fout, G. S., Martinson, B. C., Moyer, M. W. N, and Dahling, D. R. 2003. "A Multiplex Reverse
Transcription-PCR Method for Detection of Human Enteric Viruses in Groundwater." Applied and
Environmental Microbiology. 69(6): 3158-3164. (http://aem.asm.Org/cgi/reprint/69/6/3158.pdf)
5.2.9 Literature Reference for Noroviruses (Applied and Environmental Microbiology.
69(9): 5263-5268)
This method should be used for the identification of noroviruses in water, dust, and aerosol samples.
Analyte(s)
Caliciviruses: Noroviruses
Agent Category
Viruses
This method is for the detection of human noroviruses (Genogroups I and II) in groundwater samples.
Water samples are collected by filtration using a 1 MDS filter and subsequently eluted using a beef
extract solution (1.5%, pH 9.0). Viruses are further concentrated using celite adsorption (pH 4.0),
filtration, and celite-elution with sodium phosphate (0.15 M, pH 9.0). The concentrated material is
processed to remove PCR inhibitors (density sedimentation, solvent extraction, and MW-exclusion
filtration). RNA is extracted from concentrated samples and subjected to reverse-transcription (RT) using
one or both genogroup-specific cDNA-sense primer sets and the resulting cDNA is then amplified using
one or both genogroup-specific RNA-sense primer sets. The end-point RT-PCR products are analyzed by
agarose gel electrophoresis and SYBR Green I staining. Amplicons can also be verified by cloning and
sequencing.
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Please note: This procedure has not been fully verified. At a minimum, the following sample processing
quality control checks should be performed and evaluated: positive control, negative control, and blank
reactions. PCR quality control checks should be performed according to EPA Draft Quality
Assurance/Quality Control Guidance for Laboratories Performing PCR Analyses on Environmental
Samples document (www.epa.gov/nerlcwww/qa qc_pcr 1004 .pdf) or call the point of contact identified
in Section 3. This method was originally developed for ground water matrices; further research should
be conducted to develop and standardize sample processing protocols for other matrices.
Source: Parshionaker, S. U., Willian-True, S., Fout, G. S., Robbins, D. E., Seys, S. A., Cassady, J. D.,
and Harris, R. 2003. "Waterborne Outbreak of Gastroenteritis Associated with aNomvinis" Applied and
Environmental Microbiology. 69(9): 5263-5268.
5.2.10 Literature Reference for Hepatitis E virus (Journal of Virological Methods. 101:
175-188)
This method should be used for the identification of Hepatitis E virus in water, dust, and aerosol
samples.
Analyte(s)
Hepatitis E virus (HEV)
Agent Category
Viruses
This molecular detection method is used for the detection of several hepatitis E virus (HEV) classes
(Asian/African, Mexico, and US clusters) in environmental water samples using a reverse transcription-
polymerase chain reaction (RT-PCR) approach. Water samples are collected by filtration using a 1 MDS
filter; and viruses are eluted using a beef extract solution (1.5%, pH 9.5). Viruses are concentrated using
celite adsorption (pH 4.0), filtration, and celite-elution with sodium phosphate (0.15 M, pH 9.0),
followed by further concentration and processing to remove inhibitors (ultracentrirugation, solvent
extraction, and MW-exclusion filtration). Concentrated samples are analyzed by target-specific, two-step
RT-PCR (RT followed by PCR) assays using single- and multiplexed virus-specific primer sets. End
point detection of amplicons is by gel electrophoresis and subsequent confirmation by hybridization
analysis (Southern or dot-blot) using digoxigenin-labeled internal (nested) probes.
Please note: This procedure has not been fully verified. At a minimum, the following sample processing
quality control checks should be performed and evaluated before using this protocol: positive control,
negative control, and blank. PCR quality control checks should be performed according to EPA Draft
Quality Assurance/Quality Control Guidance for Laboratories Performing PCR Analyses on
Environmental Samples document (www.epa.gov/nerlcwww/qa qc_pcrlO 04.pdf) or call the point of
contact identified in Section 3. This method was originally developed for water matrices; further
research will be conducted to develop and standardize sample processing protocols for other matrices.
Source: Grimm, A. C. and G. S. Fout, 2002. "Development of a Molecular Method to Identify Hepatitis
E Virus in Water." Journal of Virological Methods, Vol. 101: 175-188.
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5.2.11 Literature Reference for Astroviruses (Canadian Journal of Microbiology. 50: 269-
278)
This method should be used for the identification of Astroviruses in water, dust, and aerosol samples.
Analyte(s)
Astroviruses
Agent Category
Viruses
This method is used to detect all eight astrovirus serotypes in clinical specimens (stool) and water
samples. It is a reverse transcription-polymerase chain reaction (RT-PCR) procedure optimized for use
in a real-time PCR assay and can be integrated with sample-cell culture (CaCo-2 cells) to enhance
sensitivity (ICC/RT-PCR). Water samples are collected by filtration (1 MDS filter), and viruses are
eluted using a beef extract solution (1.5%, pH 9.5). Viruses are concentrated using celite adsorption (pH
4.0), filtration, and celite-elution with sodium phosphate (0.15 M, pH 9.0), followed by further
concentration and processing to remove inhibitors (ultracentrifugation, solvent extraction, and MW-
exclusion filtration). Concentrated samples are analyzed directly or indirectly (following cell culture) by
a two-step RT-PCR (RT followed by PCR) assay using astrovirus-specific primer sets. Detection of
amplicons is by gel electrophoresis with subsequent confirmation by hybridization (dot-blot) using
digoxigenin-labeled internal (nested) probes or by real-time detection using fluorogenic probes.
Please note: This procedure has not been fully verified. At a minimum, the following sample processing
quality control checks should be performed and evaluated before using this protocol: positive control,
negative control, and blank. PCR quality control checks should be performed according to EPA Draft
Quality Assurance/Quality Control Guidance for Laboratories Performing PCR Analyses on
Environmental Samples document (www.epa.gov/nerlcwww/qa qc_pcr 10 04.pdf) or call the point of
contact identified in Section 3. This method was originally developed for water matrices; further
research will be conducted to develop and standardize sample processing protocols for other matrices.
Source: Grimm, A. C., Cashdollar, J. L., Williams, F. P., and Fout, G. S. 2004. "Development of an
Astrovirus RT-PCR Detection Assay for use with Conventional, Real-Time, and Integrated Cell
Culture/RT-PCR." Canadian Journal of Microbiology. 50(4): 269-268.
5.2.12 Literature Reference for Togaviruses (Journal of Clinical Microbiology. 38(4):
1527-1535)
This method should be used for the identification of Venezeulan Equine Encephalitis Virus in water,
dust, and aerosol samples.
Analyte(s)
Togaviruses: Venezuelan Equine Encephalitis Virus
(VEEV)
Agent Category
Viruses
The VEEV-specific RT-PCR assay is applied to human sera viruses that are isolated in either Vero cells,
C6/36 cells, or newborn mice. VEEV is identified using an indirect immunofluorescence assay. QIAmp
viral RNA kit (Qiagen) is used to extract RNA without the use of TaqExtender and amplification is done
using gene-specific RT-PCR-seminested PCR. Annealing temperature is 55°C in the thermocycler.
Please note: This procedure has not been fully verified for matrices other than human sera. At a
minimum, the following sample processing quality control checks should be performed and evaluated
before using this protocol: positive control, negative control, and blank. PCR quality control checks
should be performed according to EPA Draft Quality Assurance/Quality Control Guidance for
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Laboratories Performing PCR Analyses on Environmental Samples document
(www.epa.gov/nerlcwww/qa_qc_pcrl 0_04.pdf) or call the point of contact identified in Section 3. This
method was originally developed for clinical matrices; further research will be conducted to develop and
standardize sample processing protocols for other matrices.
Source: Linssen, B., Kinney, R. M., Aguilar, P., Russell, K. L., Watts, D. M., Kaaden, O., and Pfeffer
M. 2000. "Development of Reverse Transcription-PCR Assays Specific for Detection of Equine
Encephalitis Viruses." Journal of Clinical Microbiology. 38(4): 1527-1535.
(http://jcm.asm.Org/cgi/reprint/38/4/1527.pdf)
5.2.13 Literature Reference for Adenoviruses (Applied and Environmental Microbiology.
71 (6): 3131-3136)
This method should be used for the identification of Adenoviruses: enteric and non-enteric (A-F) in
water, dust, and aerosol samples.
Analyte(s)
Adenoviruses: enteric and non-enteric (A-F)
Agent Category
Viruses
This method uses a broadly reactive fluorogenic 5' nuclease (TaqMan) quantitative real-time polymerase
chain reaction (PCR) assay for the detection of all six species (A-F) of human adenoviruses (HadV).
Sensitive detection and discrimination of adenovirus F species (AdV40 and AdV41) can be achieved by
using a real-time fluorescence resonance energy transfer (FRET)-based PCR assay.
Please note: This procedure has not been fully verified for matrices other than human sera. At a
minimum, the following sample processing quality control checks should be performed and evaluated
before using this protocol: positive control, negative control, and blank. PCR quality control checks
should be performed according to EPA Draft Quality Assurance/Quality Control Guidance for
Laboratories Performing PCR Analyses on Environmental Samples document
(www.epa.gov/nerlcwww/qa qc_pcrlO 04.pdf) or call the point of contact identified in Section 3. This
method was originally developed for clinical matrices, further research will be conducted to develop and
standardize sample processing protocols for other matrices.
Source: Jothikumar, N., Cromeans, T. L., Hill, V. R., Lu, X., Sobsey, M., and Erdman, D. D. 2005.
"Quantitative Real-Time PCR Assays for Detection of Human Adenoviruses and Identification of
Serotypes 40 and4l". Applied and Environmental Microbiology. 71 (6): 3131-3136.
5.2.14 Literature Reference for Coronaviruses (SARS) (Journal of Virological Methods.
122: 29-36)
This method should be used for the identification of SARS-associated human coronavirus in water, dust,
and aerosol samples.
Analyte(s)
Coronaviruses: SARS-associated human coronavirus
Agent Category
Viruses
This method uses a conventional single-tube reverse transcription-polymerase chain reaction (RT-PCR)
procedure based on consensus primer sequences targeting conserved regions of coronavirus genome
sequences. End-point amplicon analysis is by electrophoresis and subsequent visualization. The assay
can detect the severe acute respiratory syndrome (SARS) - associated human coronavirus (SARS-HCoV)
as well as several other human respiratory coronaviruses (HCo-OC43 and HcoV-229E). Species
identification is provided by amplicon sequencing or by rapid restriction enzyme analysis.
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Please note: This procedure has not been fully verified for matrices other than human sera. At a
minimum, the following sample processing quality control checks should be performed and evaluated
before using this protocol: positive control, negative control, and blank. PCR quality control checks
should be performed according to EPA Draft Quality Assurance/Quality Control Guidance for
Laboratories Performing PCR Analyses on Environmental Samples document
(www.epa.gov/nerlcwww/qa qc_pcr 10 04.pdf) or call the point of contact identified in Section 3. This
method was originally developed for clinical matrices, further research will be conducted to develop and
standardize sample processing protocols for other matrices.
Source: Adachi, D., Johnson. G., Draker, R., Ayers, M., Mazzulli, T., Talbot, P. J., and Tellier, R. 2004.
"Comprehensive detection and identification of human coronaviruses, including the SARS-associated
coronavirus, with a single RT-PCR assay. "Journal of Virological Methods. 122: 29-36.
5.2.15 EPA Method 1622: Cryptosporidium in Water by Filtration/IMS/FA
This method should be used for the identification of Cryptosporidium species in drinking water (source
and finished), dust, and aerosol samples.
Analyte(s)
Cryptosporidium species (Cryptosporidiosis)
Agent Category
Protozoa
A water sample is filtered and the oocysts and extraneous materials are retained on the filter. Materials
on the filter are eluted, the eluate is centrifuged to pellet the oocysts, and the supernatant fluid is
aspirated. The oocysts are magnetized by attachment of magnetic beads conjugated to
anti-Cryptosporidium antibodies. The magnetized oocysts are separated from the extraneous materials
using a magnet, and the extraneous materials are discarded. The magnetic bead complex is then detached
from the oocysts. The oocysts are stained on well slides with fluorescently labeled monoclonal
antibodies and 4',6-diamidino-2-phenylindole (DAPI). The stained sample is examined using
fluorescence and differential interference contrast (DIC) microscopy. Qualitative analysis is performed
by scanning each slide well for objects that meet the size, shape, and fluorescence characteristics of
Cryptosporidium oocysts. Quantitative analysis is performed by counting the total number of objects on
the slide confirmed as oocysts. This method is not intended to determine viability of the oocysts.
Please note: This method was originally developed for water matrices; further research will be
conducted to develop and standardize sample processing protocols for other matrices.
Source: USEPA. 2003. Cryptosporidium in Water by Filtration/IMS/FA (document is currently on Web
site as draft for comment). United States Environmental Protection Agency, Washington, B.C.
(http://www.epa.gov/safewater/lt2/pdfs/guide It2 mlmanual appendix-b method-1622-
June-2003.pdf)
5.2.16 Draft EPA Method 1693: Cryptosporidium and Giardia in Disinfected Wastewater
and Combined Sewer Overflows (CSOs) by Concentration/IMS/IFA
This method should be used for the identification of Cryptosporidium species in wastewater samples.
Analyte(s)
Cryptosporidium species (Cryptosporidiosis)
Agent Category
Protozoa
A disinfected wastewater or CSO sample is concentrated either by filtration using the Envirochek™ F£V
capsule or by direct centrifugation. The filtration option of Draft Method 1693 is a modification of the
filter elution procedures used in EPA Method 1623 and includes a rinse of the filtered sample with
sodium hexametaphosphate and reagent water prior to filter elution. The second concentration option
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concentrates highly turbid or "unfilterable" matrices using direct centrifugation. The concentrated
oocysts and cysts are recovered by immunomagnetic separation (IMS) using magnetic beads conjugated
to anti-Cryptosporidium and anti-Giardia antibodies. The magnetic bead-sample complexes are
separated from the extraneous materials using a magnet, and the extraneous materials are discarded. For
samples concentrated by direct centrifugation, this separation step includes the addition of kaolin.
Kaolin is included to adsorb fats, oils, organics, and heavy particulates which may be present in a sample
deemed to be unfilterable. The magnetic bead-sample complex is then rinsed prior to dissociation and
recovery of the oocysts and cysts. The magnetic bead complex is then detached from the oocysts. The
oocysts are stained on well slides with fluorescently labeled monoclonal antibodies and
4',6-diamidino-2-phenylindole (DAPI). The stained sample is examined using fluorescence and
differential interference contrast (DIG) microscopy. Qualitative analysis is performed by scanning each
slide well for objects that meet the size, shape, and fluorescence characteristics of Cryptosporidium
oocysts. Quantitative analysis is performed by counting the total number of objects on the slide
confirmed as oocysts. This method is not intended to determine viability of the oocysts.
Please note: This method was originally developed for wastewater matrices; further research will be
conducted to develop and standardize sample processing protocols for other matrices.
Source: USEPA. 2005. Draft Method 1693: Cryptosporidium and Giardia in Disinfected Wastewater
and Combined Sewer Overflows (CSOs) by Concentration/IMS/IFA. United States Environmental
Protection Agency, Washington, D.C.
5.2.17 Literature References for Toxoplasma gondii (Applied and Environmental
Microbiology. 70(7): 4035-4039)
This method should be used for the identification and viability assessment of Toxoplasma gondii in
water, dust, and aerosol samples.
Analyte(s)
Toxoplasma gondii (Toxoplasmosis)
Agent Category
Protozoa
This method uses a fluorogenic 5' nuclease (TaqMan) real-time polymerase chain reaction (PCR) assay
for the detection of T. gondii oocyst DNA using gene-specific (Bl gene) primers and probe. Water
samples (10 -100 L) are filtered (Envirochek™) to concentrate oocysts. Filters are elutedand recovered
oocysts are further purified and concentrated by differential flotation and centrifugation. Final sample
pellets are split and subjected to PCR detection and mouse bioassay.
Please note: This procedure has not been fully verified. At a minimum, the following sample processing
quality control checks should be performed and evaluated before using this protocol: positive control,
negative control, and blank. PCR quality control checks should be performed according to EPA Draft
Quality Assurance/Quality Control Guidance for Laboratories Performing PCR Analyses on
Environmental Samples (www.epa.gov/nerlcwww/qa qc pcrlO 04.pdf) document or call the point of
contact identified in Section 3. This method was originally developed for water matrices; further
research will be required to develop and standardize sample processing protocols for other matrices.
Source: Villena, I., Aubert, D., Gomis, P., Ferte, H., Inglard, J-C., Denise-Bisiaux, H., Dondon, J-M.,
Pisano, E., Ortis, N., and Pinon, J-M. 2004. "Evaluation of a Strategy for Toxoplasma gondii Oocyst
Detection in Water". Applied and Environmental Microbiology. 70(7): 4035-4039.
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5.2.18 Entamoeba histolytica: PCR
This method should be used for the identification of Entamoeba histolytica in water, dust, and aerosol
samples.
Analyte(s)
Entamoeba histolytica
Agent Category
Protozoa
A standardized method/protocol for the analysis of Entamoeba histolytica has not been identified.
However, a real-time PCR assay has recently been developed by CDC and is expected to be
published during 2006. In the interim, PCR test kits may be obtained for analysis of this organism.
Please contact the appropriate point of contact identified in Section 3 if the need to analyze samples for
Entamoeba histolytica arises.
5.2.19 Literature Reference for Shiga Toxin Gene (Journal of Clinical Microbiology.
39(1): 370-374)
This method should be used to detect Shiga toxin genes from isolated bacterial colonies derived from
water, dust, and aerosol samples.
Analyte(s)
Shiga toxin
Agent Category
Biotoxin
This method is used to detect bacterial genes (stx; and stx2) encoding the two major classes of Shiga
toxins, Shiga toxin 1 and Shiga toxin 2. Detection of stx genes (stxl5 stx2, and stx2e) is performed using a
multiplexed polymerase chain reaction (PCR) assay and fluorescence-based melting curve analysis of
amplicons in a single capillary tube format (LightCycler).
Please note: This procedure has not been fully verified. At a minimum, the following sample processing
quality control checks should be performed and evaluated before using this protocol: positive control,
negative control, and blank. PCR quality control checks should be performed according to EPA Draft
Quality Assurance/Quality Control Guidance for Laboratories Performing PCR Analyses on
Environmental Samples document or call the point of contact identified in Section 3.
Source: Bellin, T., Pulz, M., Matussek, A., Hempen, H-G., and Gunzer, F. 2001. "Rapid Detection of
Enterohemorrhagic Escherichia coll by Real-Time PCR with Fluorescent Hybridization Probes."
Journal of Clinical Microbiology. 39(1): 370-374.
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Section 6.0: Radiochemical Methods
A list of analytical methods to be used in analyzing environmental samples for radiochemical
contaminants during homeland security events is provided in Appendix C. Methods are listed for each
isotope and for each sample matrix that potentially may need to be measured and analyzed when
responding to an emergency. The methods table in Appendix C is sorted alphabetically by analyte and
includes the following information:
• Analyte(s). The compound or compound(s) of interest.
Chemical Abstract Survey Registration Number (CAS RN). A unique identifier for chemical
substances that provides an unambiguous way to identify a chemical or molecular structure when
there are many possible systematic, generic, or trivial names. In this section (Section 6.0) and
Appendix C, the CAS RNs correspond to the specific radionuclide identified.
• Determinative technique. An analytical instrument or technique used for qualitative and
quantitative determination of compounds or components in a sample.
Drinking water sample analysis procedure. The recommended method/procedure for sample
preparation and analysis to measure the analyte of interest in drinking water samples. Methods have
been identified for gross determination and confirmation of specific isotopes.
Aqueous and liquid phase sample analysis procedure. The recommended method/procedure for
sample preparation and analysis to measure the analyte of interest in aqueous and/or non-aqueous
liquid phase samples. Methods have been identified for gross determination and confirmation of
specific isotopes.
• Soil and sediment phase sample analysis procedure. The recommended method/procedure for
sample preparation and analysis to measure the analyte of interest in soil and sediment samples.
Methods have been identified for gross determination and confirmation of specific isotopes.
Surface wipe sample analysis procedure. The recommended method/procedure for sample
preparation and analysis to measure the analyte of interest in surface wipe samples. Methods have
been identified for gross determination and confirmation of specific isotopes.
Air filter sample analysis procedure. The recommended method/procedure for sample preparation
and analysis to measure the analyte of interest in air filter samples. Methods have been identified for
gross determination and confirmation of specific isotopes.
• Gross determination method identifier. A unique identifier or number assigned to an analytical
method by the method publisher. The identified method is for measurement of the specific activity
(i.e., gamma, alpha or beta) from all radioisotopes of the targeted radiological element.
Confirmatory method identifier. A unique identifier or number assigned to an analytical method
by the method publisher. The identified method is for measurement of the specific activity (i.e.,
gamma, alpha or beta) from a particular target radioisotope of a radiological element.
6.1 General Guidance
The guidance summarized in this section provides a general overview of how to identify the appropriate
radiochemical method(s) for a given analyte-matrix combination as well as recommendations for quality
control procedures.
For additional information on the properties of the radionuclides listed in Appendix C, TOXNET
(http://toxnet.nlm.nih.gov/index.html). a cluster of databases on toxicology, hazardous chemicals, and
related areas maintained by the National Library of Medicine, is an excellent resource. EPA's Radiation
Information (http://www.epa.gov/radiation/radionuclides/index.html) and the Multi-Agency Radiological
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Laboratory Analytical Protocols Manual (littp://www.epa.gov/radiation/marlap/manual.htm) Web sites
provide some additional information pertaining to radionuclides of interest and radiochemical methods.
6.1.1 Standard Operating Procedures for Identifying Radiochemical Methods
To determine the appropriate method that is to be used on the environmental samples, locate the analyte
of concern in Appendix C: Radiochemical Methods under the "Analyte(s)" column. After locating the
analyte of concern, continue across the table to identify the appropriate determinative technique and
determinative (gross and/or confirmatory) method applicable to the matrix of interest (drinking water,
aqueous and liquid phase, soil and sediment, surface wipes, and air filters) for the particular analyte.
Sections 6.2.1 through 6.2.20 below provide summaries of the gross and confirmatory determinative
methods listed in Appendix C. Where available, a direct link to the full text of the selected analytical
method is provided in the method summary. For additional information on sample preparation and
analysis procedures and on methods available through consensus standards organizations, please use the
contact information provided in Table 3.
Table 3. Sources of Radiochemical Methods
Name
Publisher
Reference
National Environmental Methods Index
(NEMI)
U.S. Environmental
Protection Agency
(USEPA), United States
Geological Survey (USGS)
http://wvwv.nemi.gov
Prescribed Procedures for
Measurement of Radioactivity in
Drinking Water (EPA-600 4-80-032
August 1980)
U.S. Environmental
Protection Agency
(USEPA), Office of
Research and Development
(ORD), Environmental
Monitoring and Support
Laboratory (EMSL)
Available from National Technical
Information Service (NTIS). NTIS, U.S.
Department of Commerce, 5285 Port
Royal Road, Springfield, VA22161
(703) 605-6000.
Annual Book of ASTM Standards, Vol.
11.02*
American Society for
Testing and Materials
(ASTM) International
http://www.astm.org
EML Procedures Manual, HASL-300,
28th Edition, February, 1997
U.S. Department of Energy
(DOE), Environmental
Measurements Laboratory
(EML)/Now, U.S.
Department of Homeland
Security (DHS),
http://www.eml.doe.gov/publications/pr
ocman/
Also available from National Technical
Information Service (NTIS). NTIS, U.S.
Department of Commerce, 5285 Port
Royal Road, Springfield, VA22161
(703) 605-6000
Radiochemical Analytical Procedures
for Analysis of Environmental Samples,
March 1978. EMSL-LV-0539-17
United States
Environmental Protection
Agency (U.S. EPA),
Environmental Monitoring
and Support Laboratory
(EMSL)
Available from National Technical
Information Service (NTIS). NTIS, U.S.
Department of Commerce, 5285 Port
Royal Road, Springfield, VA 22161.
(703) 605-6000
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Name
Publisher
Reference
Standard Methods for the Examination
of Water and Wastewater, 20th Edition,
1998*
American Public Health
Association (APHA),
American Water Works
Association (AWWA), and
Water Environment
Federation (WEF)
http://wvwv.standardmethods.org
Subscription and/or purchase required.
6.1.2 General Quality Control (QC) Guidance for Radiochemical Methods
Having data of known and documented quality is critical in order for public officials to accurately assess
the activities that may be needed in responding to emergency situations. Having such data requires that
laboratories: (1) conduct the necessary QC to ensure that measurement systems are in control and
operating correctly, (2) properly document results of the analyses, and (3) properly document
measurement system evaluation of the analysis-specific QC. Ensuring data quality also requires that
laboratory results are properly evaluated and the results of the data quality evaluation are transmitted to
decision makers.
The level or amount of QC needed often depends on the intended purpose of the data that are generated.
Various levels of QC may be required if the data are generated during contaminant presence/absence
screening determinations versus quantitative analytical analyses. The specific needs for data generation
should be identified. Quality control requirements and data quality objectives should be derived based
on those needs. For example, during rapid sample screening analyses, minimal QC samples (e.g., blanks,
duplicates) and documentation might be required to ensure data quality. Implementation of the analytical
methods for risk assessment and site release, such as those identified in this document, might require
increased QC requirements (demonstrations of method sensitivity, precision, and accuracy).
Some method-specific QC requirements are described in many of the individual methods that are cited in
this manual, and will be referenced in any standardized analytical protocols developed to address specific
analytes and matrices of concern. Individual methods, sampling and analysis protocols, or contractual
statements of work also should be consulted to determine any additional QC that may be needed.
QC samples are required to assess the precision, accuracy, and independence of sample results. All QC
results are tracked on control charts for prescribed parameters of their results and reviewed for
acceptability and trends in analysis or instrument operation. These quality assurance (QA) parameters
are measured as required per method at the prescribed frequency. QA of laboratory analyses using
radiochemical methods includes an initial demonstration of proficiency or capability as well as ongoing
analysis of standards and other samples to ensure continued reliability of the analytical results.
• Method blank
• Lab fortified blank recovery for samples that are chemically prepared
Calibration check
• Sample and sample duplicate
• Laboratory control sample recovery for samples that are not chemically prepared, OR
Matrix spike and matrix spike duplicate for samples that are chemically prepared
• Tracer recovery
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Please note: The appropriate point of contact identified in Section 3 should be consulted regarding
appropriate quality assurance and quality control (QA/QC) procedures prior to sample analysis. These
contacts will consult with their respective QA/QC managers regarding QA/QC issues.
6.1.3 Safety and Waste Management
It is imperative that safety precautions are used during collection, processing, and analysis of
environmental samples, particularly in emergency response situations that may include unknown hazards.
Many of the methods summarized or cited in Section 6.2 contain specific requirements, guidance, or
information regarding safety precautions that should be followed when handling or processing
environmental samples and reagents. These methods also provide information regarding waste
management. Other resources that can be consulted for additional information include the following:
Occupational Health and Safety Administration's standard for Occupational Exposure to Hazardous
Chemicals in Laboratories (29 CFR 1910.1450)
• Environmental Protection Agency's standards regulating hazardous waste (40 CFR parts 260 - 270)
Standards for protection against radiation (10 CFR part 20)
U.S. Department of Energy (DOE). Order O 435.1: Radioactive Waste Management. July 1, 1999.
Available at: www.directives.doe.gov/pdfs/doe/doetext/neword/435/o4351 .html
• U.S. Department of Energy (DOE). M 435.1-1. Radioactive Waste Management Manual. Office of
Environmental Management. July 9, 1999. Available at:
http://www.directives.doe.gov/pdfs/doe/doetext/neword/435/m4351-l.html
• U.S. Department of Energy (DOE). Compendium ofEPA-Approved Analytical Methods for
Measuring Radionuclides in Drinking Water. Prepared by the Office of Environmental Policy and
Assistance Air, Water and Radiation Division (EH-412). June 1998
• U.S. Environmental Protection Agency (EPA). 1996. Profile and Management Options for EPA
Laboratory Generated Mixed Waste. Office of Radiation and Indoor Air, Washington, DC
• EPA 402-R-96-015. August. Available at: http://www.epa.gov/radiation/mixed-
waste/mw_pg7 .htm#lab mix
• U.S. Environmental Protection Agency (EPA). 2001. Changes to 40 CFR 266 (Storage, Treatment,
Transportation, and Disposal of Mixed Waste), Federal Register 66:27217-27266, May 16
• U.S. Environmental Protection Agency (EPA). 2002. RCRA Orientation Manual. Office of Solid
Waste, Washington, DC. EPA530-R-02-016. 259 pp. Available at:
http://www.epa.gov/epaoswer/general/orientat/
Waste Management in a Radioanalytical Laboratory 17-18 Multi-Agency Radiological Laboratory
Analytical Protocols (MARLAP) Manual, July 2004
• National Research Council. 1995. Prudent Practices in the Laboratory; Handling and Disposal of
Chemicals, National Academy Press, Washington, DC
• National Council on Radiation Protection and Measurements (NCRP). 2002. Risk-Based
Classification of Radioactive and Hazardous Chemical Wastes, 7910 Woodmont Avenue, Suite 400,
Bethesda, MD 20814-3095
• U.S. Nuclear Regulatory Commission/U.S. Environmental Protection Agency (NRC/EPA). 1995.
Low-Level Mixed Waste Storage Guidance, Federal Register 60:40204-40211, August 7
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6.2 Method Summaries
Summaries for the analytical methods listed in Appendix C are provided in Sections 6.2.1 through 6.2.20.
These summaries contain information that has been extracted from the selected methods. Each method
summary contains a table identifying the contaminants in Appendix C to which the method applies, a
brief description of the analytical method, and a link to the full version of the method or a source for
obtaining a full version of the method. The full version of the method should be consulted prior to
sample analysis.
Please note: Not all methods have been verified for the analyte/matrix combination listed in Appendix C.
Please refer to the specified method to identify analyte/matrix combinations that have been verified. Any
questions regarding information discussed in this section should be addressed to the appropriate
contact(s) listed in Section 3.
6.2.1 EPA Method 901.1: Gamma Emitting Radionuclides in Drinking Water
This method should be used for gross determination and confirmatory analysis of drinking water
samples for the contaminants identified below and listed in Appendix C.
Contaminant
Cesium-137 *
Cobalt-60
Europium-154
lridium-192
Ruthenium-103
Ruthenium-106 *
CASRN
10045-97-3
10198-40-0
15585-10-1
14694-69-0
13968-53-1
13967-48-1
* The identified method will measure decay products of these isotopes
This method is applicable for analysis of water samples that contain radionuclides that emit gamma
photons with energies ranging from approximately 60 to 2000 keV. The method uses gamma
spectroscopy for measurement of gamma photons emitted from radionuclides without separating them
from the sample matrix. A homogeneous aliquot of water is placed into a standard geometry (normally a
Marinelli beaker) for gamma counting, using a Ge(Li) detector (preferred) or a Nal(Tl) detector. Sample
aliquots are counted long enough to meet the required sensitivity of measurement. To reduce adsorbance
of radionuclides on the walls of the counting container, the sample is acidified at collection time.
Significant interference can occur using the Nal(Tl) detector when counting a sample containing
radionuclides that emit gamma photons of nearly identical energies. Detection limits for this method are
dependent on sample volume, geometry (physical shape), and counting time.
Source: "Prescribed Procedures for Measurement of Radioactivity in Drinking Water," National
Exposure Risk Laboratory-Cincinnati (NERL-CI), EPA/600/4/80/032, August 1980, available from
National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161. Phone:
800-553-6847.
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6.2.2 EPA Method 903.0: Alpha-Emitting Radium Isotopes in Drinking Water
This method should be used for gross determination analysis of drinking water samples for the
contaminant identified below and listed in Appendix C.
Contaminant
Radium-226
CASRN
13982-63-3
This method covers measurement of the total soluble alpha emitting radioisotopes of radium, namely
radium-223, radium-224 and radium-226 in drinking water. The method does not give an accurate
measurement of radium-226 content in the sample when other alpha emitters are present. If radium-223
and radium-224 are present, the results can be used to provide a gross determination of radium-226.
When the total radium alpha activity of a drinking water sample is greater than 5 pCi/L, use of Method
903.1 (Radium-226 in Drinking Water) is preferred. Radium in the water sample is collected by co-
precipitation with barium and lead sulfate, and purified by re-precipitation from EDTA solution. Citric
acid is added to ensure that complete interchange occurs before the first precipitation step. The final
barium sulfate precipitate is alpha counted to determine the total disintegration rate of the radium
isotopes. By making a correction for the ingrowth of alpha activity in radium-226 for the elapsed time
after separation, one can determine radium activity in the sample. Presence of significant natural barium
in the sample can result in a falsely high yield. Based on a 1000-mL sample and 100-minute counting
time, the minimum detectable levels for this method is 0.5 pCi/L.
Source: "Prescribed Procedures for Measurement of Radioactivity in Drinking Water," National
Exposure Risk Laboratory-Cincinnati (NERL-CI), EPA/600/4/80/032, August 1980, available from
National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161. Phone:
800-553-6847.
6.2.3 EPA Method 903.1: Radium-226 in Drinking Water - Radon Emanation Technique
This method should be used for confirmatory analysis of drinking water samples for the contaminant
identified below and listed in Appendix C.
Contaminant
Radium-226
CASRN
13982-63-3
This method is specific for radium-226, and is based on the emanation and scintillation counting of
radon-222, a daughter product of radium-226. Radium-226 is concentrated and separated from the water
sample by co-precipitation on barium sulfate. The precipitate is dissolved in EDTA reagent, placed in a
sealed bubbler and stored for ingrowth of radon-222. After ingrowth, the gas is purged into a
scintillation cell. When the short-lived radon-222 daughters are in equilibrium with the parent (after
~4h), the scintillation cell is counted for activity. The absolute measurement of radium-226 is effected
by calibrating the scintillation cell system with a standard solution of the nuclide. There are no
radioactive interferences in this method. Based on a 1000-mL sample and 100-minute counting time, the
minimum detectable level for this method is 0.5 pCi/L.
Source: "Prescribed Procedures for Measurement of Radioactivity in Drinking Water," National
Exposure Risk Laboratory-Cincinnati (NERL-CI), EPA/600/4/80/032, August 1980, available from
National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161. Phone:
800-553-6847. Also at http://webl.er.usgs.gov/nemi/method summary.jsp?param method id=4732
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6.2.4 EPA Method 905.0: Radioactive Strontium in Drinking Water
This method should be used for gross determination and confirmatory analysis of drinking water
samples for the contaminant identified below and listed in Appendix C.
Contaminant
Strontium-90
CASRN
10098-97-2
This method measures total strontium and soluble strontium-89 and strontium-90 in drinking water
samples. Some naturally insoluble (and probably suspended) forms of strontium-89 and strontium-90
would also be measured by this method when samples are acid preserved before analysis. Stable
strontium carrier is added to the sample and strontium-89 and strontium-90 are precipitated from solution
as insoluble carbonates. The yttrium-90 daughter of strontium-90 is removed by a hydroxide
precipitation step and the separated combined strontium-89 and strontium-90 are counted for beta particle
activity. The counting result, immediately ascertained, represents total strontium activity (strontium-90 +
strontium-89). To determine the amount of strontium-90, the yttrium-90 daughter is allowed to grow for
two weeks as the strontium-90 decays. Yttrium-90 is then separated with stable yttrium carrier as
hydroxide and finally precipitated as oxalate and beta counted. The strontium-90 concentration is equal
to the yttrium-90 activity. Strontium-89 activity is determined by subtracting the yttrium-90 activity from
the strontium-89 and strontium-90 total activity. Interferences from calcium and some radionuclides are
removed by one or more precipitations of the strontium carrier as strontium nitrate. Barium and radium
are removed as chromate. Based on a 1000-mL sample and 100-minute counting time, the minimum
detectable level for this method is 0.5 pCi/L.
Source: "Prescribed Procedures for Measurement of Radioactivity in Drinking Water," National
Exposure Risk Laboratory-Cincinnati (NERL-CI), EPA/600/4/80/032, August 1980, available from
National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161. Phone:
800-553-6847.
6.2.5 EPA Method 908.0: Uranium in Drinking Water - Radiochemical Method
This method should be used for gross determination analysis of drinking water samples for the
contaminant identified below and listed in Appendix C.
Contaminant
Uranium-238
CASRN
7440-61-1
This method measures total uranium alpha activity of a sample, without doing an isotopic uranium
analysis. The sample is acidified with hydrochloric acid and boiled to eliminate carbonate and
bicarbonate ions. Uranium is co-precipitated with ferric hydroxide and separated from the sample. The
uranium is then separated from other radionuclides that were carried down with the ferric hydroxide by
dissolving the hydroxide precipitate in hydrochloric acid, putting the solution through an anion exchange
column, washing the column with hydrochloric acid, and finally eluting the uranium with hydrochloric
acid. The uranium eluate is evaporated and the uranium chemical form is converted to nitrate. The
residue is transferred to a stainless steel planchet, dried, flamed, and counted for alpha particle activity.
Since uranium is a naturally occurring radionuclide, reagents must be checked for uranium contamination
by analyzing a complete reagent blank by the same procedure as used for the samples. Based on a 1000-
mL sample and 100-minute counting time in a single laboratory study, the minimum detectable level for
this method is 1.0 pCi/L.
Source: "Prescribed Procedures for Measurement of Radioactivity in Drinking Water," National
Exposure Risk Laboratory-Cincinnati (NERL-CI), EPA/600/4/80/032, August 1980, available from
National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield, VA 22161. Phone:
800-553-6847.
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6.2.6 EPA Method EMSL-19: Determination of Radium-226 and Radium-228 in Water,
Soil, Air and Biological Tissue
This method should be used for confirmatory analysis of soil/sediment, surface wipe, and air filter
samples for the contaminant identified below and listed in Appendix C.
Contaminant
Radium-226 *
CASRN
13982-63-3
* The identified method will measure decay products of this isotope
Following acid digestion and filtration of soil, sediment, surface wipe, or air filter samples, radium is
precipitated with barium sulfate. Barium-radium-sulfate is dissolved in a pentasodium
diethylenetriamine-pentaacetate solution and transferred to an emanation tube. The radon is allowed to
come to equilibrium for approximately 30 days. Radium-226 decays by alpha emission to radon-222.
Radon-222 is separated and collected from the liquid by a de-emanation technique. The radon is counted
by alpha scintillation 4.5 hours after de-emanation, at which time the short-lived progeny have reached
97% of equilibrium. An applicable measurement range has not been determined, however, samples that
contain 0.1 pCi of radium-226 have been analyzed.
Source: "Radiochemical Analytical Procedures for Analysis of Environmental Samples," United States
Environmental Protection Agency, Environmental Monitoring and Support Laboratory (EMSL), March
1979, available from National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield,
VA 22161. Phone:800-553-6847.
6.2.7 EPA Method EMSL-33: Isotopic Determination of Plutonium, Uranium, and
Thorium in Water, Soil, Air, and Biological Tissue
This method should be used for confirmatory analysis of drinking water, aqueous/liquid, soil/sediment,
surface wipe, and/or air filter samples for the contaminants identified below and listed in Appendix C.
Contaminant
Plutonium-238
Uranium-238
CASRN
13981-16-3
7440-61-1
This method is appropriate for the analysis of isotopic plutonium, uranium, and thorium, together or
individually, by alpha spectrometry. Plutonium-236, uranium-232, and thorium-234 tracer standards are
added for the determination of chemical yields. Samples are decomposed by nitric-hydrofluoric acid
digestion or ignition to assure that all of the plutonium is dissolved and chemically separated from the
sample by co-precipitation with sodium and ammonium hydroxide, anion exchange, and
electrodeposition. The residues are dissolved in dilute nitric acid and successive sodium and ammonium
hydroxide precipitations are performed in the presence of boric acid to remove fluoride and soluble salts.
The hydroxide precipitate is dissolved, the solution is pH-adjusted with hydrochloric acid, and plutonium
and uranium are adsorbed on an anion exchange column, separating them from thorium. Plutonium is
eluted with hydrobromic acid. The actinides are electrodeposited on stainless steel discs from an
ammonium sulfate solution and subsequently counted by alpha spectrometry. This method is designed to
detect environmental levels of activity as low as 0.02 picocuries per sample. To avoid possible cross-
contamination, sample activities should be limited to 25 picocuries or less.
Source: "Radiochemical Analytical Procedures for Analysis of Environmental Samples," United States
Environmental Protection Agency, Environmental Monitoring and Support Laboratory (EMSL), March
1979, available from National Technical Information Service (NTIS), 5285 Port Royal Road, Springfield,
VA 22161. Phone:800-553-6847.
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6.2.8 ASTM Method D3084: Standard Practice for Alpha Spectrometry in Water
This method should be used for gross determination analysis of drinking water and aqueous/liquid
samples for the contaminants identified below and listed in Appendix C.
Contaminant
Americium-241
Californium-252
Plutonium-238
CASRN
14596-10-2
13981-17-4
13981-16-3
This standard practice covers the process that is required to obtain well-resolved alpha spectra from
water samples and discusses the associated problems. This practice is typically followed with specific
chemical separations and mounting techniques, that are included in referenced methods. A chemical
procedure is required to isolate and purify the radionuclides (see ASTM Methods D3865 and D3972) and
a radioactive tracer is added to determine yield. A source is prepared by employing electrodeposition,
microprecipitation, or evaporation (depositing the solution onto a stainless steel or platinum disk).
Electrodeposition and microprecipitation are preferred. The source's radioactivity is then measured in an
alpha spectrometer according to manufacturer's operating instructions. The counting period chosen
depends on the sensitivity required of the measurement and the degree of uncertainty in the result that is
acceptable.
Source: "Annual Book of ASTM Standards, Vol. 11.02," American Society for Testing and Materials
(ASTM), 1996, ASTM International, 100 Barr Harbor Drive West, Conshohocken, PA 19428. Phone:
610-832-9500. Web: http://www.astm.org. Use Method number when ordering.
6.2.9 ASTM Method D3972: Standard Test Method for Isotopic Uranium in Water by
Radiochemistry
This method should be used for confirmatory analysis of drinking water samples for the contaminant
identified below and listed in Appendix C.
Contaminant
Uranium-238
CASRN
7440-61-1
This method covers the determination of uranium isotopes in water by means of chemical separations and
alpha pulse height analysis. Uranium is chemically separated from a water sample by co-precipitation
with ferrous hydroxide, anion exchange, and electrodeposition. When suspended matter is present, an
acid dissolution step is added to ensure that all of the uranium dissolves. The sample is acidified, and
uranium-232 is added as an isotopic tracer to determine chemical yield. Uranium is co-precipitated from
the sample with ferrous hydroxide. This precipitate is dissolved in concentrated hydrochloric acid, or is
subjected to acid dissolution with concentrated nitric and hydrofluoric acids, if the hydrochloric acid fails
to dissolve the precipitate. Uranium is separated from other radionuclides by adsorption on anion
exchange resins, followed by elution with hydrochloric acid. The uranium is finally electrodeposited
onto a stainless steel disk for alpha pulse analysis with a silicon-surface barrier detector.
Source: "Annual Book of ASTM Standards, Vol. 11.02," American Society for Testing and Materials
(ASTM), 2002, ASTM International, 100 Barr Harbor Drive West, Conshohocken, PA 19428. Phone:
610-832-9500. Web: http://www.astm.org. Use Method number when ordering.
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6.2.10 U.S. DHS EML Method Am-01-RC: Americium in Soil
This method should be used for confirmatory analysis of soil/sediment samples for the contaminants
identified below and listed in Appendix C.
Contaminant
Americium-241
Californium-252
CASRN
14596-10-2
13981-17-4
This method uses alpha spectrometry for determination of americium-241 in soil, and also can be applied
for determination of californium. Americium is leached from soil with nitric acid and hydrochloric acid.
Americium-243 is added as a tracer to determine chemical yield. The soil is processed through the
plutonium separation steps using ion exchange resin according to Procedure Pu-11-RC. Americium is
collected with a calcium oxalate precipitation and finally isolated and purified by ion exchange.
Californium is expected to be eluted at a point after americium is stripped off the column. After source
preparation by microprecipitation, americium-241 and californium-25 2 are determined by separate alpha
spectrometry analysis. The lower limit of detection (LLD) for americium-241 is 0.3 mBq when counted
for 5000 minutes.
Source: AM-01-RC and Pu-11-RC. "EML Procedures Manual, HASL-3000," 28th Edition,
Environmental Measurements Laboratory (EML), Department of Energy (EML is currently part of the
U.S. Department of Homeland Security), February 1997. Web:
http://www.eml .doe. gov/publications/procman/
6.2.11 U.S. DHS EML Method Am-02-RC: Americium-241 in Soil-Gamma Spectrometry
This method should be used for gross determination analysis of soil/sediment samples for the
contaminant identified below and listed in Appendix C.
Contaminant
Americium-241
CASRN
14596-10-2
This method uses gamma spectrometry for determination of americium-241 in soil. Americium-241
decays with the emission of a gamma ray at 59.5 keV with a decay frequency (abundance or yield) of
35.9%. The sample is placed into an appropriately sized standard geometry (normally a Marinelli
beaker) after drying and grinding the sample forhomogenization. Gamma-ray attenuation corrections are
required if the calibration source and the sample are in a different matrix or are of different densities.
The lower limit of detection (LLD) for 600 to 800 g of soil in a Martinelli beaker is 0.74 mBq for a 1000-
minute count.
Source: "EML Procedures Manual, HASL-3000," 28th Edition, Environmental Measurements Laboratory
(EML), Department of Energy (EML is currently part of the U.S. Department of Homeland Security),
February 1997. Web: http://www.eml.doe.gov/publications/procman/
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6.2.12 U.S. DHS EML Method Am-04-RC: Americium in QAP Water and Air Filters -
Eichrom's TRU Resin
This method should be used for confirmatory analysis of drinking water and aqueous/liquid samples for
the contaminants identified below and listed in Appendix C.
Contaminant
Americium-241
Californium-252
CASRN
14596-10-2
13981-17-4
This method is specific to measurement of americium isotopes in samples that do not contain
lanthanides, but also can be used for measurement of californium. The method uses microprecipitation
and determination by alpha spectrometry. Americium-243 is added to the sample to determine chemical
yield. The sample is processed through separation steps using ion exchange resins. The eluate from the
ion exchange column containing americium (and all other ions, except plutonium) is evaporated,
redissolved, and loaded onto a TRU Resin extraction column. Americium (and curium, if present) is
separated and purified on the column and finally stripped with dilute nitric acid stripping solution.
Californium is expected to be eluted at a point after americium is stripped off the column.
Microprecipitation is used to prepare for alpha-precipitation. The method involves sample preparation
steps from U.S. DHS EML Method Pu-10-RC for water samples. The lower limit of detection (LLD) for
total americium is 0.1 mBq when counted for 5000 minutes.
Source: "EML Procedures Manual, HASL-3000," 28th Edition, Environmental Measurements Laboratory
(EML), Department of Energy (EML is currently part of the U.S. Department of Homeland Security),
February 1997. Web: http://www.eml.doe.gov/publications/procman/
6.2.13 U.S. DHS EML Method Ga-01-R: Gamma Radioassay
This method should be used for gross determination and/or confirmatory analysis of soil/sediment,
surface wipes, and/or air filter samples for the contaminants identified below and listed in Appendix C.
Contaminant
Cesium-137 *
Cobalt-60
Europium-154
lridium-192
Radium-226 **
Ruthenium-103
Ruthenium-106 *
CASRN
10045-97-3
10198-40-0
15585-10-1
14694-69-0
13982-63-3
13968-53-1
13967-48-1
* The identified method will measure decay products of these isotopes
** Method selected for gross determination of radium-226 in soil and sediment samples only
This method uses gamma spectroscopy for the measurement of gamma photons emitted from
radionuclides without separating them from the sample matrix. The method is applicable for analysis of
samples that contain radionuclides emitting gamma photons with energies ranging from about >40 keV
for Ge(Li) and 100 keV for Nal(Tl) detector. The sample is placed into a standard geometry (physical
shape) for gamma counting. Soil samples and sludge are placed into an appropriately sized Martinelli
beaker after drying and grinding the sample for homogenization. Samples are counted long enough to
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meet the required sensitivity of measurement. For typical counting systems and sample types, activity
levels of approximately 40 Bq are measured and sensitivities as low as 0.002 Bq can be achieved for
many nuclides. Because of electronic limitations, count rates higher than 2000 counts per second (cps)
should be avoided. High activity samples may be diluted, reduced in size, or moved away from the
detector (a limited distance) to reduce the count rate and allow for analysis.
Source: "EML Procedures Manual, HASL-3000," 28th Edition, Environmental Measurements Laboratory
(EML), Department of Energy (EML is currently part of the U.S. Department of Homeland Security),
February, 1997. Web: http://www.eml.doe.gov/publications/procman/
6.2.14 U.S. DHS EML Method Sr-03-RC: Strontium-90 in Environmental Samples
This method should be used for gross determination and confirmatory analysis of soil/sediment,
surface wipes, and air filter samples for the contaminant identified below and listed in Appendix C.
Contaminant
Strontium-90 *
CASRN
10098-97-2
* The identified method will measure decay products of these isotopes
Strontium is separated from calcium, other fission products, and natural radioactive elements. Fuming
nitric acid separations remove the calcium and most other interfering ions. Radium, lead and barium are
removed with barium chromate. Traces of other fission products are scavenged with iron hydroxide.
After strontium-90 and yttrium-90 equilibrium has been attained, yttrium-90 is precipitated as the
hydroxide and converted to oxalate for counting on a low-background gas proportional beta counter.
Chemical yield is determined with strontium-85 tracer by counting in a gamma well detector.
Source: "EML Procedures Manual, HASL-3000," 28th Edition, Environmental Measurements Laboratory
(EML), Department of Energy (EML is currently part of the U.S. Department of Homeland Security),
February, 1997. Web: http://www.eml.doe.gov/publications/procman/
6.2.15 Standard Method 7120: Gamma-Emitting Radionuclides
This method should be used for gross determination and confirmatory analysis of aqueous/liquid
samples for the contaminants identified below and listed in Appendix C.
Contaminant
Cesium-137*
Cobalt-60
Europium-154
lridium-192
Ruthenium-103
Ruthenium-106 *
CASRN
10045-97-3
10198-40-0
15585-10-1
14694-69-0
13968-53-1
13967-48-1
* The identified method will measure decay products of these isotopes
The method uses gamma spectroscopy for measurement of gamma photons emitted from radionuclides in
water samples, using either germanium (Ge) diodes or thalium-activated sodium iodide (Nal(Tl))
crystals. The method is applicable to samples that contain radionuclides emitting gamma photons with
energies ranging from about 60 to 2000 KeV, and can be used for qualitative and quantitative
determinations (using Ge detectors) or for screening and semi-quantitative determinations (using Nal(Tl)
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detectors). Exact quantitation using Nal is possible for single nuclides or when the gamma emissions are
limited to a few well-separated energies. A homogeneous water sample is placed into a standard
geometry (normally a Marinelli beaker) for gamma counting. Sample portions are counted long enough
to meet the required sensitivity of measurement. A standard containing a mixture of gamma energies
from about 100 to 2000 KeV is used for energy calibration.
Source: "Standard Methods for Examination of Water and Wastewater," 20th Edition, American Public
Health Association (APHA), American Water Works Association (AWWA), and Water Environment
Federation (WEF), 1998. Web: http://www.standardmethods.org/
6.2.16 Standard Method 7500-Ra B: Radium: Precipitation Method
This method should be used for gross determination analysis of aqueous/liquid samples for the
contaminant identified below and listed in Appendix C.
Contaminant
Radium-226*
CASRN
13982-63-3
* The identified method will measure decay products of this isotope
This method is for determination of all alpha-emitting radium isotopes by alpha decay analysis. Lead and
barium carriers are added to the sample containing alkaline citrate, then sulfuric acid is added to
precipitate radium, barium, and lead as sulfates. The precipitate is purified by washing with nitric acid,
dissolving in alkaline EDTA, and reprecipitating as radium-barium sulfate after pH adjustment to 4.5.
This slightly acidic EDTA keeps other naturally occurring alpha-emitters and the lead carrier in solution.
Radium-223, -224, and -226 are identified by the rate of ingrowth of their daughter products in barium
sulfate precipitate. The results are corrected by the rate of ingrowth to determine radium activity. This
method involves alpha counting by a gas-flow internal proportional counter, scintillation counter, or thin
end-window gas-flow proportional counter.
Source: "Standard Methods for Examination of Water and Wastewater," 20th Edition, American Public
Health Association (APHA), American Water Works Association (AWWA), and Water Environment
Federation (WEF), 1998. Web: http://www.standardmethods.org/
6.2.17 Standard Method 7500-Ra C: Radium: Emanation Method
This method should be used for confirmatory analysis of aqueous/liquid samples for the contaminant
identified below and listed in Appendix C.
Contaminant
Radium-226 *
CASRN
13982-63-3
* The identified method will measure decay products of this isotope
This method is for determination of radium-226 by alpha counting. Radium in water is concentrated and
separated from sample solids by co-precipitation with a relatively large amount of barium as the sulfate.
The precipitate is treated to remove silicates, if present, and to decompose insoluble radium compounds,
fumed with phosphoric acid to remove sulfite, and dissolved in hydrochloric acid. The completely
dissolved radium is placed in a bubbler, which is then closed and stored for a period of several days to
four weeks for ingrowth of radon. The bubbler is connected to an evacuation system and the radon gas is
removed from the liquid by aeration and helium, dried with a desiccant, and collected in a counting cell.
Four hours after radon collection, the cell is counted. The activity of the radon is equal to the radium
concentration. The minimum detectable concentration depends on counter characteristics, background-
counting rate of scintillation cell, cell efficiency, length of counting period, and contamination of
apparatus and environment by radium-226. Without reagent purification, the overall reagent blank
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(excluding background) should be between 0.03 and 0.05 pCi radium-226, which may be considered the
minimum detectable amount under routine conditions.
Source: "Standard Methods for Examination of Water and Wastewater," 20th Edition, American Public
Health Association (APHA), American Water Works Association (AWWA), and Water Environment
Federation (WEF), 1998. Web: http://www.standardmethods.org/
6.2.18 Standard Method 7500-Sr B: Total Radioactive Strontium and Strontium-90:
Precipitation Method
This method should be used for gross determination and confirmatory analysis of aqueous/liquid
samples for the contaminant identified below and listed in Appendix C.
Contaminant
Strontium-90 *
CASRN
10098-97-2
* The identified method will measure decay products of this isotope
A known amount of inactive strontium ions, in the form of strontium nitrate, is added as a "carrier." The
carrier, alkaline earths, and rare earths are precipitated as the carbonate to concentrate the radiostrontium.
The carrier, along with the radionuclides of strontium, is separated from other radioactive elements and
inactive sample solids by precipitation as strontium nitrate using fuming nitric acid solution. The carrier
and radionuclides of strontium are precipitated as strontium carbonate, which is dried, weighed to
determine recovery of carrier, and measured for radioactivity. The activity of the final precipitate is due
to radioactive strontium only, because all other radioactive elements have been removed. Because it is
impossible to separate the isotopes of strontium-89 and strontium-90 by any chemical procedure, the
amount of strontium-90 is determined by separating and measuring the activity of yttrium-90, its daughter
product. This method involves beta counting by a gas-flow internal proportional counter or thin end-
window low-background proportional counter. A correction is applied to compensate for loss of carriers
and activity during the various purification steps.
Source: "Standard Methods for Examination of Water and Wastewater," 20th Edition, American Public
Health Association (APHA), American Water Works Association (AWWA), and Water Environment
Federation (WEF), 1998. Web: http://www.standardmethods.org/
6.2.19 Standard Method 7500-U B: Uranium: Radiochemical Method
This method should be used for gross determination analysis of aqueous/liquid samples for the
contaminant identified below and listed in Appendix C.
Contaminant
Uranium-238
CASRN
7440-61-1
The sample is acidified with hydrochloric or nitric acid and boiled to eliminate carbonate and bicarbonate
ions. Uranium is co-precipitated with ferric hydroxide and subsequently separated. The ferric hydroxide
is dissolved, passed through an anion-exchange column, and washed with acid, and the uranium is eluted
with dilute hydrochloric acid. The acid eluate is evaporated to near dryness, the residual salt is converted
to nitrate, and the alpha activity is counted by a gas-flow proportional counter or alpha scintillation
counter.
Source: "Standard Methods for Examination of Water and Wastewater," 20th Edition, American Public
Health Association (APHA), American Water Works Association (AWWA), and Water Environment
Federation (WEF), 1998. Web: http://www.standardmethods.org/
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6.2.20 Standard Method 7500-U C: Uranium: Isotopic Method
This method should be used for confirmatory analysis of aqueous/liquid samples for the contaminant
identified below and listed in Appendix C.
Contaminant
Uranium-238
CASRN
7440-61-1
This method is a radiochemical procedure for determination of the isotopic content of uranium alpha
activity; it is consistent with determining the differences among naturally occurring, depleted, and
enriched uranium. The sample is acidified with hydrochloric or nitric acid, and uranium-232 is added as
an isotopic tracer. Uranium is co-precipitated with ferric hydroxide and subsequently separated. The
ferric hydroxide is dissolved, passed through an anion-exchange column, and washed with acid, and the
uranium is eluted with dilute hydrochloric acid. The acid eluate is evaporated to near dryness, and the
residual salt is converted to nitrate and electrodeposited onto a stainless steel disk for counting by alpha
pulse height analysis using a silicon surface barrier detector.
Source: "Standard Methods for Examination of Water and Wastewater," 20th Edition, American Public
Health Association (APHA), American Water Works Association (AWWA), and Water Environment
Federation (WEF), 1998. Web: http://www.standardmethods.org/
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Section 7.0: Biotoxin Methods
A list of analytical methods to be used in analyzing environmental samples for biotoxin contaminants
during homeland security events is provided in Appendix D. Methods are listed for each analyte and for
each sample matrix that potentially may need to be measured and analyzed when responding to an
emergency. The methods table in Appendix D is sorted alphabetically by analyte and includes the
following information:
• Analyte(s). The compound or compound(s) of interest.
• Chemical Abstract Survey Registration Number (CAS RN). A unique identifier for chemical
substances that provides an unambiguous way to identify a chemical or molecular structure when
there are many possible systematic, generic, or trivial names.
• Determinative technique. An analytical instrument or technique used to determine the quantity and
identification of compounds or components in a sample.
Determinative method identifier. The unique identifier or number assigned to an analytical
method by the method publisher.
• Solid sample preparation procedure. The recommended method/procedure for sample preparation
to measure the analyte of interest in solid phase samples.
Oily solid sample preparation procedure. The recommended method/procedure for sample
preparation to measure the analyte of interest in oily phase samples.
Aqueous/Liquid sample preparation procedure. The recommended method/procedure for sample
preparation to measure the analyte of interest in aqueous and/or liquid phase samples.
• Drinking water sample preparation procedure. The recommended method/procedure for sample
preparation to measure the analyte of interest in drinking water samples.
Air sample preparation procedure. The recommended method/procedure for sample preparation
and analysis to measure the analyte of interest in air samples.
7.1 General Guidance
The guidance summarized in this section provides a general overview of how to identify the appropriate
biotoxin method(s) for a given analyte-matrix combination as well as recommendations for quality
control procedures.
For additional information on the properties of the biotoxins listed in Appendix D, TOXNET
(http://toxnet.nlm.nih.gov/index.html'). a cluster of databases on toxicology, hazardous chemicals, and
related areas maintained by the National Library of Medicine, is an excellent resource.
Additional resources include:
A U.S. Army Medical Research Institute of Infectious Diseases' document at
http://www.usamriid.armv.mil/education/defensetox/toxdefbook.pdfcontains information regarding
sample collection, toxin analysis and identification, as well as decontamination and water treatment.
• The U.S. Centers for Disease Control has information regarding biotoxins, including 42 CFRPart
1003 regulations for possession, use, and transfer of select agents and toxins, on the following Web
site: http://www.cdc.gov/od/sap/toxinamt.htm
Syracuse Research Corporation's Physprop and Chemfate, part of the Environmental Fate Database
supported by EPA. http://www.syrres.com/esc/databases.htm
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• INCHEM at http://www.inchem.org/ contains both chemical and toxicity information.
• The RTECS database can be accessed via the NIOSH Web site at
http://www.cdc.gov/niosh/rtecs/vz72d288.htmltfJWIDAW for toxicity information.
EPA's Integrated Risk Information System (IRIS): http://www.epa.gov/iris/ contains toxicity
information.
• The Forensic Science and Communications Journal published by the Laboratory Division of the
Federal Bureau of Investigation, http://www.fbi.gov/hq/lab/fsc/current/backissu.htm.
Additional research on biotoxin contaminants is ongoing within EPA.
7.1.1 Standard Operating Procedures for Identifying Biotoxin Methods
To determine the appropriate method and sample preparation technique that is to be used on the
environmental samples, locate analyte of concern in Appendix D: Biotoxin Methods under the "Analyte"
column. After locating the analyte of concern, continue across the table to identify the determinative
technique and determinative method for that particular compound. To determine the sample preparation
technique select the appropriate matrix column (Solid, Oily Solid, Aqueous/Liquid, Drinking Water, or
Air) for that particular analyte.
Sections 7.2.1 through 7.2.4 below provide summaries of the determinative and sample preparation
methods listed in Appendix D. Where available, a direct link to the full text of the selected analytical
method is provided in the method summary. For additional information on preparation procedures and
methods available through consensus standards organizations, please use the contact information
provided in Table 4.
Table 4. Sources of Biotoxin Methods
Name
National Environmental Methods Index
(NEMI)
U.S. EPA Office of Water (OW)
Methods
U.S. EPA SW-846 Methods
U.S. EPA Office of Research and
Development Methods
U.S. EPA Air Toxics Methods
Occupational Safety and Health
Administration Methods
National Institutes for Occupational
Safety and Health Methods
Publisher
EPA, USGS
EPA Office of Water
EPA Office of Solid Waste
EPA Office of Research and
Development
EPA Office of Air and
Radiation
OSHA
NIOSH
Reference
http://vwwv.nemi.qov
http://www.epa.qov/safewater/methods/
sourcalt.html
http://www.epa.qov/epaoswer/hazwaste
/test/main, htm
http://www.epa.qov/nerlcwww/ordmeth.
htm
http://www.epa.qov/ttn/amtic/airtox.html
http://www.osha-slc.qov/dts/sltc/method
s/toc.html
http://www.cdc.qov/niosh/nmam/
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Name
Standard Methods for the Examination
of Water and Wastewater, 20th Edition,
1998*
Annual Book of ASTM Standards*
International Organization for
Standardization Methods*
Official Methods of Analysis of AOAC
International*
Journal of Clinical Microbiology*
Publisher
American Public Health
Association (APHA),
American Water Works
Association (AWWA), and
Water Environment
Federation (WEF)
ASTM International
ISO
AOAC International
American Society for
Microbiology
Reference
http://wvwv.standardmethods.orq
http://www.astm.orq
http://www.iso.orq
http://www.aoac.org
http://aem.asm.orq
Subscription and/or purchase required.
7.1.2 General Quality Control (QC) Guidance for Biotoxin Methods
Having data of known and documented quality is critical in order for public officials to accurately assess
the activities that may be needed in responding to emergency situations. Having such data requires that
laboratories: (1) conduct the necessary QC to ensure that measurement systems are in control and
operating properly, (2) properly document results of the analyses, and (3) properly document
measurement system evaluation of the analysis-specific QC. Ensuring data quality also requires that
laboratory results are properly evaluated and the results of the data quality evaluation are transmitted to
decision makers.
The level or amount of QC needed often depends on the intended purpose of the data that are generated.
Various levels of QC may be required if the data are generated during contaminant presence/absence
screening determinations versus quantitative analytical analyses. The specific needs for data generation
should be identified. Quality control requirements and data quality objectives should be derived based
on those needs. For example, during rapid sample screening analyses, minimal QC samples (e.g., blanks,
duplicates) and documentation might be required to ensure data quality. Implementation of the analytical
methods for risk assessment and site release, such as those identified in this document, might require
increased QC requirements (demonstrations of method sensitivity, precision, and accuracy).
While method-specific QC requirements are described in many of the individual methods that are cited in
this manual, and will be referenced in any standardized analytical protocols developed to address specific
analytes and matrices of concern, the following describes a minimum set of QC procedures that shall be
conducted for all chemical testing. Individual methods, sampling and analysis protocols, or contractual
statements of work also should be consulted to determine any additional QC that may be needed. These
QC requirements generally consist of analysis of laboratory control samples and or matrix spikes to
identify and quantify measurement system accuracy at the levels of concern, blanks as a measure of
freedom from contamination, and matrix spike duplicates (MSB) or sample replicates to assess data
precision. QC tests should be run as frequently as necessary to ensure the reliability of analytical results.
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In general, sufficient QC includes an initial demonstration of measurement system capability as well as
ongoing analysis of standards and other samples to ensure the continued reliability of the analytical
results. Examples of sufficient quality control includes:
• Demonstration that measurement system is operating properly
*• Initial calibration
•• Method blanks
Demonstration of measurement system suitability for intended use
•• Precision and recovery (verify measurement system has adequate accuracy)
•• Analyte/matrix/level of concern-specific QC samples (verify that measurement system has
adequate sensitivity at levels of concern)
• Demonstration of continued measurement system reliability
•• Matrix spike/matrix spike duplicates (recovery and precision)
•• QC samples (system accuracy and sensitivity at levels of concern)
•• Continuing calibration verification
»• Method blanks
Please note: The appropriate point of contact identified in Section 3 should be consulted regarding
appropriate quality assurance and quality control (QA/QC) procedures prior to sample analysis. These
contacts will consult with their respective QA/QC managers regarding QA/QC issues.
7.1.3 Safety and Waste Management
It is imperative that safety precautions are used during collection, processing, and analysis of
environmental samples, particularly in emergency response situations that may include unknown hazards.
Laboratories should have a documented health and safety plan for handling samples that may contain the
target chemical, biological, or radiological contaminants, and laboratory staff should be trained in and
implement the safety procedures included in the plan. In addition, many of the methods summarized or
cited in Section 4.2 contain some specific requirements, guidance, or information regarding safety
precautions that should be followed when handling or processing environmental samples and reagents.
These methods also provide information regarding waste management.
Other resources that can be consulted for additional information include the following:
• Occupational Health and Safety Administration's (OSHA) standard for Occupational Exposure to
Hazardous Chemicals in Laboratories (29 CFR 1910.1450)
• OSHA regulations for hazardous waste operations and emergency response (29 CFR Part 1910)
• Environmental Protection Agency's standards regulating hazardous waste (40 CFR Parts 260 - 270)
• U.S. Department of Transportation (DOT) regulations for transporting hazardous materials (49 CFR
Part 172)
• U.S. Department of Health and Human Services, Centers for Disease Control and Prevention's
requirements for possession, use, and transfer of select agents and toxins (42 CFR Part 1003)
7.2 Method Summaries
Method summaries for the analytical methods listed in Appendix D, including methods for sample
preparation and determinative techniques, are provided in Section 7.2.1 through 7.2.4. Information
provided in these sections contains summary information only, extracted from the selected methods. The
full version of the method should be consulted prior to sample analysis.
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Each method summary contains a table identifying the contaminants in Appendix D to which the method
applies, a brief description of the analytical method, and a link to the full version of the method or source
for obtaining a full version of the method.
Please note: Not all methods have been verified for the analyte/matrix combination listed in Appendix D.
Please refer to the specified method to identify analyte/matrix combinations that have been verified. Any
questions regarding information discussed in this section should be addressed to the appropriate
contact(s) listed in Section 3.
7.2.1 Laboratory Response Network (LRN)
The agents identified below and listed in Appendix D should be analyzed in accordance with the
appropriate LRN protocols.
Contaminants
Alpha amanitin
Botulinum toxin
Microcystin
Ricin
Tetanus toxin
CASRN
NA
NA
NA
9009-86-3
NA
These agents will be analyzed using restricted procedures available only through the Laboratory
Response Network (LRN). These procedures are not available to the general laboratory community and
thus are not discussed within this document. For additional information on the LRN, please see the
contact information listed below or visit http://www .bt.cdc.gov/lrn/.
Centers for Disease Control and Prevention
Laboratory Response Branch
Bioterrorism Preparedness and Response Program
National Center for Infectious Diseases
1600 Clifton Road NE, Mailstop C-18
Atlanta, GA 30333
Telephone: (404) 639-2790
E-mail: lrn@,cdc.gov
Local public health laboratories, private, and commercial laboratories with questions about the LRN
should contact their State public health laboratory director or the Association of Public Health
Laboratories (contact information provided below).
Association of Public Health Laboratories
2025 M Street NW, Suite 550
Washington, DC 20036
Telephone: (202) 822-5227
Fax: (202) 887-5098
Website: www.aphl.org
E-mail: info@,aphl.org
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7.2.2 AOAC Official Method 994.08: Aflatoxin in Corn, Almonds, Brazil Nuts, Peanuts,
and Pistachio Nuts
This method should be used for preparation and analysis of solid, oily solid, aqueous/liquid, and
drinking water samples for the contaminants identified below and listed in Appendix D.
Contaminant
Aflatoxin
B revet oxin *
Picrotoxin **
Saxitoxin *
T-2 Mycotoxin *
CASRN
1402-68-2
NA
124-87-8
35523-89-8
NA
* Alternative derivitization chemistries, chromatographic conditions, and fluorometric calibration of standards may
be required
** The U.S. Department of Agriculture (USDA) is currently developing an HPLC procedure specifically for detection
of this toxin
Samples are extracted using an acetonitrile-water (9 + 1) solution. Sample extracts are then run through
a multifunctional cleanup column. The purified extract and standards are derivatized with trifluoracetic
acid, and then analyzed using a high performance liquid chromatography (HPLC) system with a
fluorescence detector. Specific aflatoxins can be identified by their retention time and quantified using
standard curves. Method performance was characterized using various commodities (e.g., corn) at
aflatoxin levels over a range of 5 to 30 ng/g. This method was originally designed for the analysis of
aflatoxins (B1; B2, G1; and G2) in commodities where cleanup was necessary to remove other food
components, such as fats and proteins; the cleanup procedure may not be necessary with water analyses.
Coupling the procedures, or a modification of the procedures, included in this method with an
immunoassay and/or viability test (where available) will provide more information regarding the
specificity and toxicity of each target biotoxin.
Source: AOAC International. 1998. Official Methods of Analysis of AOAC International. 16th Edition, 4th
Revision; Vol II.
7.2.3 Shiga Toxin Genes (Six, Stx2)
Contaminant
Shiga toxin
CASRN
NA
Bacterial genes encoding Shiga toxin 1 and Shiga toxin 2 are detected using a real-time polymerase chain
reaction (PCR) assay. Please see Section 5 for method summary.
7.2.4 Staphyloccocal Enterotoxin (Method to be determined)
Contaminant
Staphylococcal enterotoxin
CASRN
NA
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Section 8.0: Conclusions
Methods listed in Appendix A (chemical methods), Appendix B (biological methods), Appendix C
(radiochemical methods), and Appendix D (biotoxin methods) are recommended for use in assessment of
the extent of contamination and the effectiveness of decontamination in response to a homeland security
event.
As stated in the introduction, the primary objective of this document is not necessarily to identify the
"best" method for use during homeland security events, but rather to provide a balanced approach
between leveraging existing and available determinative procedures and providing consistent analytical
results. The method selected for each analyte/matrix pair was deemed the most general, appropriate, and
broadly applicable of available methods. This is a living document and recommended methods are
subject to change based on advances in technology.
Any questions concerning the information in this document should be directed to the appropriate point(s)
of contact listed in Section 3.
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Appendix A:
Chemical Methods
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Appendix A: Chemical Methods
Analyte(s)
Aldicarb (Temik)
Allyl alcohol
Ammonia
Arsenic III compound
Arsenic trichloride
(analyze for Arsenic)
Arsine
Asbestos
Boron trichloride
Boron trifluoride
Bromadiolone
CASRN
116-06-3
107-18-6
7664-41-7
22569-72-8
7784-34-1
7784-42-1
1332-21-4
10294-34-5
7637-07-2
28772-56-7
Determinative
Technique
HPLC
GC/MS
Spectrophotometry /
ISE
ICP-MS/ICP-AES
ICP-MS/ICP-AES
GFAA/ICP-MS
TEM
ICP-AES
ISE
HPLC-UV
Determinative
Method Identifier
8318A(SW-846)
8260B
(SW-846)
4500-NH3 G (SM)
6020A/6010C
(SW-846)
6020A/6010C
(SW-846)
7010 (SW-846)
ASTM(dust) /
ISO-10312(air)
Journal Article: J.
Anal. At. Spectrom.,
2000, 15,277-279
ID-216SG (OSHA)
832 1B (SW-846)
Solid Sample
Prep / Procedure
831 8A (SW-846)
5035A (SW-846)
Not of concern in this
matrix
3050B (SW-846)
3050B (SW-846)
3050B (SW-846)
ASTM D5755-03 (soft
surfaces-microvac) or
D6480-99 (hard surfaces
wipes)
Not of concern in this
matrix
Not of concern in this
matrix
3545A/3541
(SW-846)
Oily Solid Sample
Prep / Procedure
831 8A (SW-846)
3585 (SW-846)
Not of concern in this
matrix
3031/3050B
(SW-846)
3031/3050B
(SW-846)
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
3545A/3541/3580A
(SW-846)
Aqueous/Liquid Sample
Prep / Procedure
831 8A (SW-846)
5030C (SW-846)
4500-NH3 B (SM)
200.8 (OW)
200.8 (OW)
200.8 (OW)
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
3520C/3535A
(SW-846)
Drinking Water Sample
Prep / Procedure
531 .2 (OW)
5030C (SW-846)
350.3 (OW)
200.8 (OW)
200.8 (OW)
200.8 (OW)
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
3520C/3535A
(SW-846)
Air Sample Prep /
Procedure
Not of concern in
this matrix
1402(NIOSH)
6015(NIOSH)/
ID-188(OSHA)
IO-3.1/IO-3.4/IO-3.5
(ORD)
10-3.1/1 0-3.4/10-3.5
(ORD)
6001 (NIOSH)
ISO-10312 (filter)
Journal Article:
J. Anal. At.
Spectrom., 2000,
15,277-279
ID-216SG(OSHA)
Not of concern in
this matrix
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Appendix A: Chemical Methods
Analyte(s)
Cadmium
Carbofuran (Furadan)
Carbon disulfide
Chlorine
2-Chloroethanol
3-Chloro-1 ,2-propanediol
Chloropicrin
Chlorosarin
Chlorosoman
2-Chlorovinylarsonous acid
(CVAA) (degradation product of
Lewisite)
CASRN
7440-43-9
1563-66-2
75-15-0
7782-50-5
107-07-3
96-24-2
76-06-2
1445-76-7
7040-57-5
85090-33-1
Determinative
Technique
ICP-MS/ICP-AES
HPLC / GC/MS
GC/MS
1C
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
ICP-MS / GC/MS
Determinative
Method Identifier
6020A/6010C
(SW-846)
8318A(SW-846)
8260B (SW-846)
601 1 (NIOSH) /
4500-CI G (SM)
8260B (SW-846)
8260B (SW-846)
8270D (SW-846)
8270D (SW-846)
8270D (SW-846)
6020A
(SW-846)
Solid Sample
Prep / Procedure
3050B (SW-846)
831 8A (SW-846)
5035A (SW-846)
Not of concern in this
matrix
5035A (SW-846)
5035A (SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
Oily Solid Sample
Prep / Procedure
3031/3050B
(SW-846)
831 8A (SW-846)
3585 (SW-846)
Not of concern in this
matrix
3585 (SW-846)
3585 (SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
Aqueous/Liquid Sample
Prep / Procedure
200.8 (OW)
831 8A (SW-846)
5030C (SW-846)
4500-CI G (SM)
5030C (SW-846)
5030C (SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Drinking Water Sample
Prep / Procedure
200.8 (OW)
531 .2 (OW)
524.2 (OW)
4500-CI G (SM)
5030C (SW-846)
5030C (SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Air Sample Prep /
Procedure
IO-3.1/IO-3.4/IO-3.5
(ORD)
TO-10A/
ISO-12884
TO-15
601 1 (NIOSH)
251 3 (NIOSH)
TO-15
TO-15
TO-15
TO-15
TO-15
SAM Revision 2.0, Appendix A
A-2
September 29, 2005
-------
Appendix A: Chemical Methods
Analyte(s)
Cyanide
Cyanogen chloride
Cyclohexyl sarin (GF)
1 ,2-Dichloroethane
(degradation product of HD)
Dichlorvos
Dicrotophos
Diesel Range Organics
Diisopropyl methylphosphonate
(DIMP)
(degradation product of GB)
Dimethylphosphite
CASRN
57-12-5
506-77-4
329-99-7
107-06-2
62-73-7
141-66-2
NA
1445.75-6
868-85-9
Determinative
Technique
Spectrophotometry
(colorimetric)
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC-FID
HPLC-MS / GC/MS
GC/MS
Determinative
Method Identifier
CLPILM05.3CN
8260B (SW-846)
8270D (SW-846)
8260B (SW-846)
8270D (SW-846)
8270D (SW-846)
801 5C (SW-846)
832 1B (SW-846)
8270D (SW-846)
Solid Sample
Prep / Procedure
CLP ILM05.3 CN
5035A (SW-846)
3545A/3541
(SW-846)
5035A (SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
Oily Solid Sample
Prep / Procedure
Not of concern in this
matrix
3585 (SW-846)
3545A/3541/3580A
(SW-846)
3585 (SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
Aqueous/Liquid Sample
Prep / Procedure
CLPILM05.3CN
5030C (SW-846)
3520C/3535A
(SW-846)
5030C (SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Drinking Water Sample
Prep / Procedure
335.4 (OW)
5030C (SW-846)
3520C/3535A
(SW-846)
524.2 (OW)
525.2 (OW)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Air Sample Prep /
Procedure
7904 (NIOSH)
TO-15
TO-15
TO-15
TO-10A/
ISO-12884
TO-10A/
ISO-12884
Not of concern in
this matrix
TO-15
TO-10A/
ISO-12884
SAM Revision 2.0, Appendix A
A-3
September 29, 2005
-------
Appendix A: Chemical Methods
Analyte(s)
Dimethylphosphoramidic acid
(degradation product of GA)
1 ,4-Dithiane
(degradation product of HD)
EA2192
(hydrolysis product of VX)
Ethyldichloroarsine (ED)
Ethylene oxide
Ethylmethyl phosphonate
(EMPA)
(degradation product of VX)
Fenamiphos
Fluoroacetate salts
Formaldehyde
CASRN
33876-51-6
505-29-3
73207-98-4
598-14-1
75-21-8
1832-53-7
22224-92-6
NA
50-00-0
Determinative
Technique
HPLC-MS / GC/MS
GC/MS
HPLC-MS / GC/MS
GC/MS
GC/MS
HPLC-MS / GC/MS
GC/MS
Ion Chromatography/
GC-ECD
HPLC
Determinative
Method Identifier
8321B(SW-846)
8260B (SW-846)
8321B(SW-846)
8270D (SW-846)
8260B (SW-846)
832 1B
(SW-846)
8270D (SW-846)
300.1 (OW)
831 5A (SW-846)
Solid Sample
Prep / Procedure
3545A/3541
(SW-846)
5035A (SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
5035A (SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
Journal Article:
Analytical Letters,
1994, 27(14), 2703-
2718
831 5A (SW-846)
Oily Solid Sample
Prep / Procedure
3545A/3541/3580A
(SW-846)
3585 (SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3585 (SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
Journal Article:
Analytical Letters,
1994, 27(14), 2703-
2718
Not of concern in this
matrix
Aqueous/Liquid Sample
Prep / Procedure
3520C/3535A
(SW-846)
5030C (SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Note: For liquid matrices
use 3520C (SW-846)
5030C (SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
300.1 (OW)
831 5A (SW-846)
Drinking Water Sample
Prep / Procedure
3520C/3535A
(SW-846)
5030C (SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Note: For liquid matrices
use 3520C (SW-846)
5030C (SW-846)
3520C/3535A
(SW-846)
525.2 (OW)
300.1 (OW)
831 5A (SW-846)
Air Sample Prep /
Procedure
TO-15
TO-15
TO-15
TO-15
TO-15
TO-15
TO-10A/
ISO-12884
S301-1 (NIOSH)
ISO-1 6000-3
SAM Revision 2.0, Appendix A
A-4
September 29, 2005
-------
Appendix A: Chemical Methods
Analyte(s)
Gasoline Range Organics
GE (1-methylethyl ester ethyl-
phosphonofluoridic acid)
Hydrogen bromide
Hydrogen chloride
Hydrogen cyanide
Hydrogen fluoride
Hydrogen sulfide
Isopropyl methylphosphonic
acid (IMPA) (degradation
product of GB)
Kerosene
CASRN
NA
1189-87-3
10035-10-6
7647-01-0
74-90-8
7664-39-3
7783-06-4
1832-54-8
64742-81-0
Determinative
Technique
GC-FID
GC/MS
1C
1C
Spectrophotometry /
ISE
1C
1C
HPLC-MS / GC/MS
GC-FID
Determinative
Method Identifier
8015C(SW-846)
8270D (SW-846)
4110 B(SM)/
7903 (NIOSH)
4110 B(SM)/
7903 (NIOSH)
6010 (NIOSH)
7906/7903
(NIOSH)
601 3 (NIOSH)
8321 B
(SW-846)
801 5C (SW-846)
Solid Sample
Prep / Procedure
5035A (SW-846)
3545A/3541
(SW-846)
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
3545A/3541
(SW-846)
5035A (SW-846)
Oily Solid Sample
Prep / Procedure
3585 (SW-846)
3545A/3541/3580A
(SW-846)
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
Aqueous/Liquid Sample
Prep / Procedure
5030C (SW-846)
3520C/3535A
(SW-846)
4110B(SM)
4110B(SM)
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
3520C/3535A
(SW-846)
5030C (SW-846)
Note: For liquid matrices
use 3520C/3535A
(SW-846)
Drinking Water Sample
Prep / Procedure
5030C (SW-846)
3520C/3535A
(SW-846)
4110B(SM)
4110B(SM)
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
3520C/3535A
(SW-846)
5030C (SW-846)
Air Sample Prep /
Procedure
Not of concern in
this matrix
TO-15
7903 (NIOSH)
7903 (NIOSH)
6010 (NIOSH)
7906/7903 (NIOSH)
601 3 (NIOSH)
TO-15
Not of concern in
this matrix
SAM Revision 2.0, Appendix A
A-5
September 29, 2005
-------
Appendix A: Chemical Methods
Analyte(s)
Lewisite 1 (L-1)
[2-chlorovinyldichloroarsine]
Lewisite 2 (L-2)
[bis(2-chlorovinyl)-chloroarsine]
Lewisite 3 (L-3)
[tris(2-chlorovinyl)-arsine]
Lewisite Oxide
(degradation product of
Lewisite)
Mercury
Metals, NOS
Methyl hydrazine
Methyl isocyanate
Methyl parathion
Methylamine
CASRN
541-25-3
40334-69-8
40334-70-1
1306-02-1
7439-97-6
NA
60-34-4
624-83-9
298-00-0
74-89-5
Determinative
Technique
GC/MS
GC/MS
GC/MS
ICP-MS
CVAA/CVAFS
ICP-MS/ICP-AES
GC/MS
HPLC
GC/MS
GC
Determinative
Method Identifier
8270D (SW-846)
8270D (SW-846)
8270D (SW-846)
6020A
(SW-846)
7471 B(s)/
7470A (aq)
(SW-846)
6020A/6010C
(SW-846)
8270D (SW-846)
207-2 (OAQPS)
8270D (SW-846)
2010(NIOSH)
Solid Sample
Prep / Procedure
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
7471 B (SW-846)
3050B (SW-846)
3545A/3541
(SW-846)
Not of concern in this
matrix
3545A/3541
(SW-846)
Not of concern in this
matrix
Oily Solid Sample
Prep / Procedure
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
Not of concern in this
matrix
3031/3050B
(SW-846)
3545A/3541/3580A
(SW-846)
Not of concern in this
matrix
3545A/3541/3580A
(SW-846)
Not of concern in this
matrix
Aqueous/Liquid Sample
Prep / Procedure
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
7470A (SW-846)
200.8 (OW)
3520C/3535A
(SW-846)
Not of concern in this
matrix
3520C/3535A
(SW-846)
Not of concern in this
matrix
Drinking Water Sample
Prep / Procedure
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
245.2 (OW)
200.8 (OW)
3520C/3535A
(SW-846)
Not of concern in this
matrix
3520C/3535A
(SW-846)
Not of concern in this
matrix
Air Sample Prep /
Procedure
TO-15
TO-15
TO-15
TO-15
IO-5 (ORD)
See specific metals
methods
3510(NIOSH)
207-2 (OAQPS)
TO-10A/
ISO-12884
2010(NIOSH)
SAM Revision 2.0, Appendix A
A-6
September 29, 2005
-------
Appendix A: Chemical Methods
Analyte(s)
Methylphosphonic acid (MPA)
(degradation product of VX,
GB, & GD)
Mevinphos
Mustard, nitrogen (HN-2)
[unstable compound]
Mustard, sulfur (HD) /
Mustard Gas (H)
Nicotine
Osmium tetraoxide (analyze for
Osmium)
Oxamyl
Paraquat
Perfluoroisobutylene (PFIB)
Phencyclidine
CASRN
993-13-5
7786-34-7
51-75-2
505-60-2
54-11-5
20816-12-0
23135-22-0
4685-14-7
382-21-8
77-10-1
Determinative
Technique
HPLC-MS / GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
ICP-AES / FAA
HPLC
HPLC-UV
GC/MS
GC/MS
Determinative
Method Identifier
832 1B
(SW-846)
8270D (SW-846)
8270D (SW-846)
8270D (SW-846)
8270D (SW-846)
601 OC (SW-846)
831 8A (SW-846)
549.2 (OW)
8270D (SW-846)
8270D (SW-846)
Solid Sample
Prep / Procedure
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3050B (SW-846)
831 8A (SW-846)
Problematic
3545A/3541
(SW-846)
3545A/3541
(SW-846)
Oily Solid Sample
Prep / Procedure
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
Not of concern in this
matrix
831 8A (SW-846)
Problematic
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
Aqueous/Liquid Sample
Prep / Procedure
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
252.2 (OW)
831 8A (SW-846)
549.2 (OW)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Drinking Water Sample
Prep / Procedure
3520C/3535A
(SW-846)
525.2 (OW)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
252.2 (OW)
531 .2 (OW)
549.2 (OW)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Air Sample Prep /
Procedure
TO-15
TO-10A/
ISO-12884
TO-15
TO-15
Not of concern in
this matrix
IO-3.4 (ORD)
TO-15
Not of concern in
this matrix
TO-15
TO-1QA/
ISO-12884
SAM Revision 2.0, Appendix A
A-7
September 29, 2005
-------
Appendix A: Chemical Methods
Analyte(s)
Phenol
Phorate
Phosgene
Phosphine
Phosphorus trichloride
Polychlorinated biphenyls
(PCBs)
Propylene oxide
Red Phosphorus (RP)
(analyze for total Phosphorus)
Sarin (GB)
Semivolatile Organic
Compounds, NOS
CASRN
108-95-2
298-02-2
75-44-5
7803-51-2
7719-12-2
1336-36-3
75-56-9
7723-14-0
107-44-8
NA
Determinative
Technique
GC/MS
GC/MS
GC/MS / HPLC
UV-VIS
Spectrophotometry
GC/MS / GC-ECD /
GC
GC/MS
Spectrophotometry
(colorimetric)
GC/MS
GC/MS
Determinative
Method Identifier
8270D (SW-846)
8270D (SW-846)
8260B (SW-846)
6002 (NIOSH)
6402 (NIOSH)
8082A (SW-846)
8260B (SW-846)
365.1 (NERL)
8270D (SW-846)
8270D (SW-846)
Solid Sample
Prep / Procedure
3545A/3541
(SW-846)
3545A/3541
(SW-846)
5035A (SW-846)
Not of concern in this
matrix
Not of concern in this
matrix
3545A/3541
(SW-846)
5035A (SW-846)
Not of concern in this
matrix
3545A/3541
(SW-846)
3545A/3541
(SW-846)
Oily Solid Sample
Prep / Procedure
3545A/3541/3580A
(SW-846)
3545A/3580A
(SW-846)
3585 (SW-846)
Not of concern in this
matrix
Not of concern in this
matrix
3545A/3541/3580A
(SW-846)
3585 (SW-846)
Not of concern in this
matrix
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
Aqueous/Liquid Sample
Prep / Procedure
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
3520C/3535A
(SW-846)
5030C (SW-846)
365.1 (NERL)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Drinking Water Sample
Prep / Procedure
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Not of concern in this
matrix
Not of concern in this
matrix
Not of concern in this
matrix
508 (OW)
5030C (SW-846)
365.1 (NERL)
3520C/3535A
(SW-846)
525.2 (OW)
Air Sample Prep /
Procedure
TO-10A/
ISO-12884
TO-1QA/
ISO-12884
TO-6/TO-15
6002 (NIOSH)
6402 (NIOSH)
TO-1QA/
ISO-12884
1612 (NIOSH)
Not of concern in
this matrix
TO-15
TO-1QA/
ISO-12884
SAM Revision 2.0, Appendix A
September 29, 2005
-------
Appendix A: Chemical Methods
Analyte(s)
Soman (GD)
Strychnine
Sulfur Dioxide
Tabun (GA)
Tear gas (CS)
[chlorobenzylidene malonitrile]
Tetraethyl pyrophosphate
Tetramethylene-
disulfotetramine
Thiodiglycol (TDG)
(degradation product of HD)
1 ,4-Thioxane
(degradation product of HD)
Titanium tetrachloride (analyze
for total Titanium)
CASRN
96-64-0
57-24-9
7446-09-5
77-81-6
2698-41-1
107-49-3
80-12-6
111-48-8
15980-15-1
7550-45-0
Determinative
Technique
GC/MS
GC/MS
1C
GC/MS
GC/MS
GC/MS
HPLC-UV / GC/MS
GC/MS
GC/MS
ICP-MS/ICP-AES
Determinative
Method Identifier
8270D (SW-846)
8270D (SW-846)
6004 (NIOSH)
8270D (SW-846)
8270D (SW-846)
8270D (SW-846)
832 1B (SW-846)
8270D (SW-846)
8260B (SW-846)
6020A/6010C
(SW-846)
Solid Sample
Prep / Procedure
3545A/3541
(SW-846)
3545A/3541
(SW-846)
Not of concern in this
matrix
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
5035A (SW-846)
3050B (SW-846)
Oily Solid Sample
Prep / Procedure
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
Not of concern in this
matrix
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3585 (SW-846)
Not of concern in this
matrix
Aqueous/Liquid Sample
Prep / Procedure
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Not of concern in this
matrix
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
5030C (SW-846)
Not of concern in this
matrix
Drinking Water Sample
Prep / Procedure
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
Not of concern in this
matrix
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
5030C (SW-846)
Not of concern in this
matrix
Air Sample Prep /
Procedure
TO-15
Not of concern in
this matrix
6004 (NIOSH)
TO-15
TO-1QA/
ISO-12884
TO-1QA/
ISO-12884
TO-1QA/
ISO-12884
TO-15
TO-15
Not of concern in
this matrix
SAM Revision 2.0, Appendix A
A-9
September 29, 2005
-------
Appendix A: Chemical Methods
Analyte(s)
Trimethyl phosphite
VE
VG
VM
Volatile Organic Compounds,
NOS
VX [0-ethyl-S-(2-
diisopropylaminoethyl)
methyl phosphonothiolate]
CASRN
121-45-9
21738-25-0
78-53-5
21770-86-5
NA
50782-69-9
Determinative
Technique
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
GC/MS
Determinative
Method Identifier
8270D (SW-846)
8270D (SW-846)
8270D (SW-846)
8270D (SW-846)
8260B (SW-846)
8270D (SW-846)
Solid Sample
Prep / Procedure
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
3545A/3541
(SW-846)
5035A (SW-846)
3545A/3541
(SW-846)
Oily Solid Sample
Prep / Procedure
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3545A/3541/3580A
(SW-846)
3585 (SW-846)
3545A/3541/3580A
(SW-846)
Aqueous/Liquid Sample
Prep / Procedure
3520C/3535A
(SW-846)
Note: For liquid matrices
use 3520C (SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
5030C (SW-846)
3520C/3535A
(SW-846)
Drinking Water Sample
Prep / Procedure
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
3520C/3535A
(SW-846)
524.2 (OW)
3520C/3535A
(SW-846)
Air Sample Prep /
Procedure
TO-10A/
ISO-12884
TO-10A/
ISO-12884
TO-10A/
ISO-12884
TO-10A/
ISO-12884
TO-15
TO-10A/
ISO-12884
SAM Revision 2.0, Appendix A
A-10
September 29, 2005
-------
Appendix B:
Biological Methods
SAM Revision 2.0 September 29, 2005
-------
SAM Revision 2.0 September 29, 2005
-------
Appendix B-1: Waterborne Biological Methods
Waterborne
Agent
Category
Analyte(s)
Identification Procedures
Identification
determinative
technique
Determinative
method identifier
Wastewater sample
preparation1
procedure and/or
sampling method
Drinking water sample
preparation1 procedure
and/or sampling
method
Viability Procedures
Viability
determinative
technique
Determinative
method identifier
Wastewater sample
preparation1 procedure
and/or sampling
method
Drinking water sample
preparation1 procedure
and/or sampling
method
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacillus anthracis
(Anthrax)
Brucella spp. (Brucellosis)
Burkholderia mallei
(Glanders)
Burkholderia pseudomallei
(Melioidosis)
Campylobacter jejuni
Coxiella burnetii
(Q-fever)
Escherichia coli (E. coli)
O157:H7
Francisella tularensis
(Tularemia)
Rickettsia prowazekii
(Epidemic Typhus)
Salmonella typhi (Typhoid
fever)
Shigella spp. (Shigellosis)
Vibrio cholerae (Cholera)
Yersinia pestis (Plague)
Culture / PCR / TRF
Culture / PCR / TRF
Culture / PCR / TRF
Culture / PCR / TRF
Culture
Culture / PCR / TRF
Culture
Culture / PCR / TRF
Culture
Culture
Culture
Culture
Culture / PCR / TRF
LRN
LRN
LRN
LRN
SM 9260 G
LRN
SM 9260 F
LRN
LRN
SM 9260 B
SM 9260 E
SM 9260 H
LRN
As specified by LRN
protocol
As specified by LRN
protocol
As specified by LRN
protocol
As specified by LRN
protocol
Filtration of large
volumes of water using
0.45 or 0.22 micron filter
As specified by LRN
protocol
Collect 100 mL sample
in sterile container
As specified by LRN
protocol
As specified by LRN
protocol
As specified by SM
protocol
Filtration of large
volumes of water using
0.45 or 0.22 micron filter
Concentration by placing
Moore swabs in flowing
wastewater for 1 week
As specified by LRN
protocol
As specified by LRN
protocol
As specified by LRN
protocol
As specified by LRN
protocol
As specified by LRN
protocol
Ultrafiltration device
As specified by LRN
protocol
Ultrafiltration device
As specified by LRN
protocol
As specified by LRN
protocol
As specified by SM
protocol
Ultrafiltration device
Ultrafiltration device
As specified by LRN
protocol
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
LRN
LRN
LRN
LRN
SM 9260 G
LRN
SM 9260 F
LRN
LRN
SM 9260 B
SM 9260 E
SM 9260 H
LRN
As specified by LRN
protocol
As specified by LRN
protocol
As specified by LRN
protocol
As specified by LRN
protocol
Filtration of large
volumes of water using
0.45 or 0.22 micron filter
As specified by LRN
protocol
Collect 1 00 mL sample
in sterile container
As specified by LRN
protocol
As specified by LRN
protocol
As specified by SM
protocol
Filtration of large
volumes of water using
0.45 or 0.22 micron filter
Concentration by placing
Moore swabs in flowing
wastewater for 1 week
As specified by LRN
protocol
As specified by LRN
protocol
As specified by LRN
protocol
As specified by LRN
protocol
As specified by LRN
protocol
Ultrafiltration device
As specified by LRN
protocol
Ultrafiltration device
As specified by LRN
protocol
As specified by LRN
protocol
As specified by SM
protocol
Ultrafiltration device
Ultrafiltration device
As specified by LRN
protocol
SAM Revision 2.0, Appendix B-1
B-1 - 1
September 29, 2005
-------
Waterborne
Agent
Category
Analyte(s)
Identification Procedures
Identification
determinative
technique
Determinative
method identifier
Wastewater sample
preparation1
procedure and/or
sampling method
Drinking water sample
preparation1 procedure
and/or sampling
method
Viability Procedures
Viability
determinative
technique
Determinative
method identifier
Wastewater sample
preparation1 procedure
and/or sampling
method
Drinking water sample
preparation1 procedure
and/or sampling
method
Biotoxin
Biotoxin
Shiga toxin
PCR
Journal of Clinical
Microbiology Vol. 39
No. 1 : 370-374
Analysis conducted on
isolated bacteria
Analysis conducted on
isolated bacteria
NA
NA
NA
NA
Hemorrhagic Fever Viruses
Viruses
Viruses
Viruses
Viruses
Arenavi ruses
Bunyavi ruses
Filovi ruses
Flaviviruses
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
CDC
CDC
CDC
CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
CDC
CDC
CDC
CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
Encephalomyelitis / Encephalitis Viruses
Viruses
Togaviruses: Venezuelan
Equine Encephalitis
Virus (VEEV)
RT-PCR
Journal of Clinical
Microbiology Vol. 38
No. 4: 1527-1535
TBD
Filtration (1 MDS filter)
Tissue Culture
TBD
TBD
Filtration (1 MDS filter)
Poxviruses
Viruses
Viruses
Orthopoxvirus:
Monkeypox virus
Orthopoxvirus:
Variola major (Smallpox)
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
CDC
CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
CDC
CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
SAM Revision 2.0, Appendix B-1
B-1 -2
September 29, 2005
-------
Waterborne
Agent
Category
Analyte(s)
Identification Procedures
Identification
determinative
technique
Determinative
method identifier
Wastewater sample
preparation1
procedure and/or
sampling method
Drinking water sample
preparation1 procedure
and/or sampling
method
Viability Procedures
Viability
determinative
technique
Determinative
method identifier
Wastewater sample
preparation1 procedure
and/or sampling
method
Drinking water sample
preparation1 procedure
and/or sampling
method
Enteric viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Adenovi ruses:
enteric and non-enteric
(A-F)
Astroviruses
Caliciviruses: Noroviruses
Caliciviruses: Sapovirus
Coronavi ruses:
SARS-associated human
coronavirus
Hepatitis E virus (HEV)
Picornaviruses:
Enterovi ruses
Picornaviruses:
Hepatitis A virus (HAV)
Reovi ruses:
Rotavirus (Group A)
Real-time PCR
RT-PCR
ICC/RT-PCR
RT-PCR
RT-PCR
RT-PCR
RT-PCR
RT-PCR
RT-PCR
RT-PCR
AEMVol. 71 No. 6:
3131-3136
Canadian Journal of
Microbiology Vol. 50:
269-278
AEM Vol. 69 No. 9:
5263-5268
TBD
Journal of Virological
Methods Vol. 122:
29-36
Journal of Virological
Methods Vol. 101:
175-188
AEM Vol. 69 No. 6:
3158-3164
AEM Vol. 69 No. 6:
3158-3164
AEM Vol. 69 No. 6:
3158-3164
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
TBD
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
TBD
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
Tissue Culture
Tissue Culture
TBD
TBD
Tissue Culture
TBD
Tissue Culture
Tissue Culture
Tissue Culture
TBD
TBD
TBD
TBD
TBD
TBD
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
TBD
TBD
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
TBD
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
TBD
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
Protozoa
Protozoa
Protozoa
Protozoa
Cryptosporidium species
(Cryptosporidiosis)
Entamoeba histolytica
Toxoplasma gondii
(Toxoplasmosis)
FA / IFA
PCR
PCR
Method 16227
Method 1693
TBD
AEMVol. 70 No. 7:
4035-4039
Filtration/Centrifugation
per Method 1693
TBD
TBD
Filtration
per Method 1622
TBD
TBD
TBD
Mouse
Bioassay/Tissue
culture
Mouse Bioassay
TBD
TBD
AEM Vol. 70 No. 7:
4035-4039
Filtration/centrifugation
TBD
TBD
Filtration
TBD
TBD
1A dechlorinating agent (Sodium thiosulfate) should be added to treated water samples to remove any residual chlorine.
SAM Revision 2.0, Appendix B-1
B-1 -3
September 29, 2005
-------
SAM Revision 2.0, Appendix B-1 B-1 - 4 September 29, 2005
-------
Appendix B-2: Dustborne Biological Methods
Dustborne
Agent
Category
Analyte(s)
Identification Procedures
Identification
determinative
technique
Determinative method
identifier
Sample preparation
procedure and/or sampling
method
Viability Procedures
Viability
determinative
technique
Determinative method
identifier
Sample preparation
procedure and/or sampling
method
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacillus anthracis
(Anthrax)
Brucella spp. (Brucellosis)
Burkholderia mallei
(Glanders)
Burkholderia pseudomallei
(Melioidosis)
Campylobacterjejuni
Coxiella burnetii
(Q-fever)
Escherichia coli (E. coli)
O157:H7
Francisella tularensis
(Tularemia)
Rickettsia prowazekii
(Epidemic Typhus)
Salmonella typhi (Typhoid
fever)
Shigella spp. (Shigellosis)
Vibrio cholerae (Cholera)
Yersinia pestis (Plague)
Culture / PCR / TRF
Culture / PCR / TRF
Culture / PCR / TRF
Culture / PCR / TRF
Culture
Culture / PCR / TRF
Culture
Culture / PCR / TRF
Culture
Culture
Culture
Culture
Culture / PCR / TRF
LRN
LRN
LRN
LRN
SM 9260 G
LRN
SM 9260 F
LRN
LRN
SM 9260 B
SM 9260 E
SM 9260 H
LRN
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
LRN
LRN
LRN
LRN
SM 9260 G
LRN
SM 9260 F
LRN
LRN
SM 9260 B
SM 9260 E
SM 9260 H
LRN
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
Swabs, socks, swipes
CDC/NIOSH Sampling
techniques
SAM Revision 2.0, Appendix B-2
B-2-1
September 29, 2005
-------
Dustborne
Agent
Category
Analyte(s)
Identification Procedures
Identification
determinative
technique
Determinative method
identifier
Sample preparation
procedure and/or sampling
method
Viability Procedures
Viability
determinative
technique
Determinative method
identifier
Sample preparation
procedure and/or sampling
method
Biotoxin
Biotoxin
Shiga toxin
PCR
Journal of Clinical
Microbiology Vol. 39
No. 1:370-374
Analysis conducted on
isolated bacteria
NA
NA
NA
Hemorrhagic Fever Viruses
Viruses
Viruses
Viruses
Viruses
Arenaviruses
Bunyaviruses
Filoviruses
Flaviviruses
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
CDC
CDC
CDC
CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
CDC
CDC
CDC
CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
Encephalomyletis / Encephalitis Viruses
Viruses
Togaviruses: Venezuelan
Equine Encephalitis
Virus (VEEV)
RT-PCR
Journal of Clinical
Microbiology Vol. 38
No. 4: 1527-1535
TBD
Tissue Culture
TBD
TBD
Poxviruses
Viruses
Viruses
Orthopoxvirus:
Monkeypox virus
Orthopoxvirus:
Variola major (Smallpox)
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
CDC
CDC
As specified by CDC
As specified by CDC
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
CDC
CDC
As specified by CDC
As specified by CDC
SAM Revision 2.0, Appendix B-2
B-2-2
September 29, 2005
-------
Dustborne
Agent
Category
Analyte(s)
Identification Procedures
Identification
determinative
technique
Determinative method
identifier
Sample preparation
procedure and/or sampling
method
Viability Procedures
Viability
determinative
technique
Determinative method
identifier
Sample preparation
procedure and/or sampling
method
Enteric viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Adenoviruses:
enteric and non-enteric
(A-F)
Astroviruses
Caliciviruses: Noroviruses
Caliciviruses: Sapovirus
Coronaviruses:
SARS-associated human
coronavirus
Hepatitis E virus (HEV)
Pico rnavi ruses:
Enteroviruses
Pico rnavi ruses:
Hepatitis A virus (HAV)
Reoviruses:
Rotavirus (Group A)
Real-time PCR
RT-PCR
ICC/RT-PCR
RT-PCR
RT-PCR
RT-PCR
RT-PCR
RT-PCR
RT-PCR
RT-PCR
AEM Vol. 71 No. 6:
3131-3136
Canadian Journal of
Microbiology
Vol. 50: 269-278
AEM Vol. 69 No. 9:
5263-5268
TBD
Journal of Virological
Methods
Vol. 122:29-36
Journal of Virological
Methods
Vol. 101: 175-188
AEM Vol. 69 No. 6:
3158-3164
AEM Vol. 69 No. 6:
3158-3164
AEM Vol. 69 No. 6:
3158-3164
TBD
TBD
TBD
TBD
TBD
TBD
TBD
TBD
TBD
Tissue Culture
Tissue Culture
TBD
TBD
Tissue Culture
TBD
Tissue Culture
Tissue Culture
Tissue Culture
TBD
TBD
TBD
TBD
TBD
TBD
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
TBD
TBD
TBD
TBD
TBD
TBD
TBD
TBD
TBD
TBD
TBD
Protozoa
Protozoa
Protozoa
Protozoa
Cryptosporidium species
(Cryptosporidiosis )
Entamoeba histolytica
Toxoplasma gondii
(Toxoplasmosis)
FA
PCR
PCR
Method 1622
TBD
AEM Vol. 70 No. 7:
4035-4039
TBD
TBD
TBD
TBD
Mouse
Bioassay/Tissue
culture
Mouse Bioassay
TBD
TBD
AEM Vol. 70 No. 7:
4035-4039
TBD
TBD
TBD
SAM Revision 2.0, Appendix B-2
B-2-3
September 29, 2005
-------
SAM Revision 2.0, Appendix B-2 B-2 - 4 September 29, 2005
-------
Appendix B-3: Aerosol Biological Methods
Aerosol
Agent
Category
Analyte(s)
Identification Procedures
Identification
determinative
technique
Determinative method
identifier
Sample preparation
procedure and/or sampling
method
Viability Procedures
Viability
determinative
technique
Determinative method
identifier
Sample preparation
procedure and/or sampling
method
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacteria
Bacillus anthracis
(Anthrax)
Brucella spp. (Brucellosis)
Burkholderia mallei
(Glanders)
Burkholderia pseudomallei
(Melioidosis)
Campylobacterjejuni
Coxiella burnetii
(Q-fever)
Escherichia coli (E. coli)
O157:H7
Francisella tularensis
(Tularemia)
Rickettsia prowazekii
(Epidemic Typhus)
Salmonella typhi (Typhoid
fever)
Shigella spp. (Shigellosis)
Vibrio cholerae (Cholera)
Yersinia pestis (Plague)
Culture / PCR / TRF
Culture / PCR / TRF
Culture / PCR / TRF
Culture / PCR / TRF
Culture
Culture / PCR / TRF
Culture
Culture / PCR / TRF
Culture
Culture
Culture
Culture
Culture / PCR / TRF
LRN
LRN
LRN
LRN
SM 9260 G
LRN
SM 9260 F
LRN
LRN
SM 9260 B
SM 9260 E
SM 9260 H
LRN
XMZ/ Anderson Button
Sampler/ DFU
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
Culture
LRN
LRN
LRN
LRN
SM 9260 G
LRN
SM 9260 F
LRN
LRN
SM 9260 B
SM 9260 E
SM 9260 H
LRN
XMZ /Anderson Button
Sampler/ DFU
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
Wetted-wall cyclones,
CDC/NIOSH Sampling
techniques
SAM Revision 2.0, Appendix B-3
B-3-1
September 29, 2005
-------
Aerosol
Agent
Category
Analyte(s)
Identification Procedures
Identification
determinative
technique
Determinative method
identifier
Sample preparation
procedure and/or sampling
method
Viability Procedures
Viability
determinative
technique
Determinative method
identifier
Sample preparation
procedure and/or sampling
method
Biotoxin
Biotoxin
Shiga toxin
PCR
Journal of Clinical
Microbiology Vol. 39
No. 1:370-374
Analysis conducted on
isolated bacteria
NA
NA
NA
Hemorrhagic Fever Viruses
Viruses
Viruses
Viruses
Viruses
Arenaviruses
Bunyaviruses
Filoviruses
Flaviviruses
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
CDC
CDC
CDC
CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
CDC
CDC
CDC
CDC
As specified by CDC
As specified by CDC
As specified by CDC
As specified by CDC
Encephalomyletis / Encephalitis Viruses
Viruses
Togaviruses: Venezuelan
Equine Encephalitis
Virus (VEEV)
RT-PCR
Journal of Clinical
Microbiology Vol. 38
No. 4: 1527-1535
TBD
Tissue Culture
TBD
TBD
Poxviruses
Viruses
Viruses
Orthopoxvirus:
Monkeypox virus
Orthopoxvirus:
Variola major (Smallpox)
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
CDC
CDC
As specified by CDC
As specified by CDC
Biosafety Level 4 -
Ship directly to CDC
laboratory
Biosafety Level 4 -
Ship directly to CDC
laboratory
CDC
CDC
As specified by CDC
As specified by CDC
SAM Revision 2.0, Appendix B-3
B-3-2
September 29, 2005
-------
Aerosol
Agent
Category
Analyte(s)
Identification Procedures
Identification
determinative
technique
Determinative method
identifier
Sample preparation
procedure and/or sampling
method
Viability Procedures
Viability
determinative
technique
Determinative method
identifier
Sample preparation
procedure and/or sampling
method
Enteric viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Viruses
Adenoviruses: enteric and
non-enteric (A-F)
Astroviruses
Caliciviruses: Noroviruses
Caliciviruses: Sapovirus
Coronaviruses:
SARS-associated human
coronavirus
Hepatitis E virus (HEV)
Pico rnavi ruses:
Enteroviruses
Pico rnavi ruses:
Hepatitis A virus (HAV)
Reoviruses:
Rotavirus (Group A)
PCR
RT-PCR
ICC/RT-PCR
RT-PCR
RT-PCR
RT-PCR
RT-PCR
RT-PCR
RT-PCR
RT-PCR
AEM Vol. 71 No. 6:
3131-3136
Canadian Journal of
Microbiology
Vol. 50: 269-278.
AEM Vol. 69 No. 9:
5263-5268
TBD
Journal of Virological
Methods Vol. 122:
29-36
Journal of Virological
Methods Vol. 101:
175-188
AEM Vol. 69 No. 6:
3158-3164
AEM Vol. 69 No. 6:
3158-3164
AEM Vol. 69 No. 6:
3158-3164
TBD
TBD
TBD
TBD
TBD
TBD
TBD
TBD
TBD
Tissue Culture
Tissue Culture
TBD
TBD
Tissue Culture
TBD
Tissue Culture
Tissue Culture
Tissue Culture
TBD
TBD
TBD
TBD
TBD
TBD
As specified in USEPA
Manual of Methods for
Virology EPA/600/4-
84/013, April 2001
TBD
TBD
TBD
TBD
TBD
TBD
TBD
TBD
TBD
TBD
TBD
Protozoa
Protozoa
Protozoa
Protozoa
Cryptosporidium species
(Cryptosporidiosis )
Entamoeba histolytica
Toxoplasma gondii
(Toxoplasmosis)
FA
PCR
PCR
Method 1622
TBD
AEM Vol. 70 No. 7:
4035-4039
TBD
TBD
TBD
TBD
Mouse
Bioassay/Tissue
culture
Mouse Bioassay
TBD
TBD
AEM Vol. 70 No. 7:
4035-4039
TBD
TBD
TBD
SAM Revision 2.0, Appendix B-3
B-3-3
September 29, 2005
-------
SAM Revision 2.0, Appendix B-3 B-3 - 4 September 29, 2005
-------
Appendix C:
Radiochemical Methods
SAM Revision 2.0 September 29, 2005
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SAM Revision 2.0 September 29, 2005
-------
Appendix C: Radiochemical Methods
Analyte(s)
Americium-241
Californium-252
Cesium-137**
Cobalt-60
Europium-154
lridium-192
Plutonium-238
Radium-226
Ruthenium-103
Ruthenium-106 **
Strontium-90
Uranium-238
CASRN
14596-10-2
13981-17-4
10045-97-3
10198-40-0
15585-10-1
14694-69-0
13981-16-3
13982-63-3
13968-53-1
13967-48-1
10098-97-2
7440-61-1
Determinative
Technique
Alpha/Gamma
spectrometry
Alpha
spectrometry
Gamma
spectrometry
Gamma
spectrometry
Gamma
spectrometry
Gamma
spectrometry
Alpha
spectrometry
Alpha Counting
Gamma
spectrometry
Gamma
spectrometry
Beta counting by
low-background
gas flow
proportional
detector
Alpha Counting
Drinking Water Samples
Gross
Determination
D3084
(ASTM)
D3084
(ASTM)
901.1 (EPA)
901.1 (EPA)
901.1 (EPA)
901.1 (EPA)
D3084
(ASTM)
903.0 (EPA)
901.1 (EPA)
901.1 (EPA)
905.0 (EPA)
908.0 (EPA)
Confirmatory
Am-04-RC
(DHS)
Am-04-RC
(DHS)
901.1 (EPA)
901.1 (EPA)
901.1 (EPA)
901.1 (EPA)
EMSL-33
(EPA)
903.1 (EPA)
901.1 (EPA)
901.1 (EPA)
905.0 (EPA)
D3972
(ASTM)
Aqueous and Liquid Phase
Samples
Gross
Determination
D3084
(ASTM)
D3084
(ASTM)
7120 (SM)
7120 (SM)
7120 (SM)
7120 (SM)
D3084
(ASTM)
7500-Ra B
(SM)
7120 (SM)
7120 (SM)
7500-Sr B
(SM)
7500-U B
(SM)
Confirmatory
Am-04-RC
(DHS)
Am-04-RC
(DHS)
7120 (SM)
7120 (SM)
7120 (SM)
7120 (SM)
EMSL-33
(EPA)
7500-Ra C
(SM)
7120 (SM)
7120 (SM)
7500-Sr B
(SM)
7500-U C
(SM)
Soil and Sediment Samples
Gross
Determination
Am-02-RC
(DHS)
TBD
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
TBD
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Sr-03-RC
(DHS)
TBD
Confirmatory
Am-01-RC
(DHS)
Am-01-RC
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
EMSL-33
(EPA)
EMSL-19
(EPA)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Sr-03-RC
(DHS)
EMSL-33
(EPA)
Surface Wipes
Gross
Determination
TBD
TBD
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
TBD
TBD
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Sr-03-RC
(DHS)
TBD
Confirmatory
TBD
TBD
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
EMSL-33
(EPA)
EMSL-19
(EPA)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Sr-03-RC
(DHS)
EMSL-33
(EPA)
Air Filters
Gross
Determination
TBD
TBD
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
TBD
TBD
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Sr-03-RC
(DHS)
TBD
Confirmatory
TBD
TBD
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
EMSL-33
(EPA)
EMSL-19
(EPA)
Ga-01-R
(DHS)
Ga-01-R
(DHS)
Sr-03-RC
(DHS)
EMSL-33
(EPA)
" Methods identified will measure decay product of these isotopes
SAM Revision 2.0, Appendix C
C-1
September 29, 2005
-------
SAM Revision 2.0, Appendix C C-2 September 29, 2005
-------
Appendix D:
Biotoxin Methods
SAM Revision 2.0 September 29, 2005
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SAM Revision 2.0 September 29, 2005
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Appendix D: Biotoxins Methods
Analyte(s)
Aflatoxin
Alpha amanitin
Botulinum toxin
Brevetoxin
Microcystin
Picrotoxin
Ricin
Saxitoxin
T-2 Mycotoxin
Tetanus toxin
Shiga toxin
Staphylococcal
enterotoxin
CASRN
1402-68-2
NA
NA
NA
NA
124-87-8
9009-86-3
35523-89-8
NA
NA
NA
NA
Determinative
Technique
HPLC-FL
Immunoassay
Immunoassay
HPLC-FL
Immunoassay
HPLC-FL
Immunoassay
HPLC-FL
HPLC-FL
Immunoassay
PCR
Immunoassay
Determinative
Method Identifier
994.08 (AOAC)
LRN
LRN
994.08 (AOAC)
LRN
994.08 (AOAC)
LRN
994.08 (AOAC)
994.08 (AOAC)
LRN
Solid Sample
Prep / Procedure
994.08 (AOAC)
LRN
LRN
994.08 (AOAC)
LRN
994.08 (AOAC)
LRN
994.08 (AOAC)
994.08 (AOAC)
LRN
Oily Solid Sample
Prep / Procedure
994.08 (AOAC)
LRN
LRN
994.08 (AOAC)
LRN
994.08 (AOAC)
LRN
994.08 (AOAC)
994.08 (AOAC)
LRN
Aqueous/Liquid Sample
Prep / Procedure
994.08 (AOAC)
LRN
LRN
994.08 (AOAC)
LRN
994.08 (AOAC)
LRN
994.08 (AOAC)
994.08 (AOAC)
LRN
Drinking Water Sample
Prep / Procedure
994.08 (AOAC)
LRN
LRN
994.08 (AOAC)
LRN
994.08 (AOAC)
LRN
994.08 (AOAC)
994.08 (AOAC)
LRN
Air Sample Prep /
Procedure
Not of concern in
this matrix
LRN
LRN
Not of concern in
this matrix
LRN
Not of concern in
this matrix
LRN
Not of concern in
this matrix
Not of concern in
this matrix
LRN
Refer to Appendix B for appropriate methods
TBD
TBD
TBD
TBD
TBD
TBD
SAM Revision 2.0, Appendix D
D-1
September 29, 2005
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SAM Revision 2.0, Appendix D D - 2 September 29, 2005
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