&EPA
EPA/600/R-10/090 September 2010
United States
Environmental Protection
Agency
Rapid Screening and Preliminary
Identification Techniques and
Methods
Companion to Standardized Analytical Methods for
Environmental Restoration Following Homeland
Security Events (SAM) - Revision 5.0
Office of Research and Development
National Homeland Security Research Center
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Rapid Screening and Preliminary
Identification Techniques and
Methods
Companion to Standardized Analytical
Methods for Environmental Restoration
Following Homeland Security Events (SAM)
- Revision 5.0
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
Office of Research and Development, National Homeland Security Research Center,
Cincinnati, OH 45268
Office of Research and Development
National Homeland Security Research Center, Threat and Consequence Assessment Division
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SAM Companion - Rapid Screening and Preliminary Identification Techniques and Methods
Acknowledgements
This document was developed by the U.S. Environmental Protection Agency's (EPA) National Homeland
Security Research Center (NHSRC) within EPA's Office of Research and Development as a companion
to NHSRC's Standardized Analytical Methods for Environmental Restoration Follow ing Homeland
Security Events (SAM), Revision 5.0. We wish to acknowledge the external peer reviews conducted by
Zia Bukhari of American Water, Larry Burchfield of the Radiochemistry Society, Gary T. Hunt of TRC
Environmental, Fred Lee of G. Fred Lee & Associates, and Jordan Peccia of Yale University whose
thoughtful comments contributed greatly to the quality of the information. The document was prepared
by Computer Sciences Corporation (CSC) under EPA Contract No. EP-W-06-046.
Disclaimer
Mention of trade names or commercial products in this document does not constitute endorsement or
recommendation for use.
Questions concerning this document or its application should be addressed to:
Romy Lee
National Homeland Security Research Center
Office of Research and Development (NG16)
U.S. Environmental Protection Agency
26 West Martin Luther King, Jr. Drive
Cincinnati, OH 45268
(513)569-7016
lee.romy@epa.gov
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SAM Companion - Rapid Screening and Preliminary Identification Techniques and Methods
Foreword
Following the events of September 11, 2001, EPA's mission was expanded to account for critical needs
related to homeland security. Presidential Directives identified EPA as the primary federal agency
responsible for the country's water supplies and for decontamination following a chemical, biological,
and/or radiological (CBR) attack. To provide scientific and technical support to help EPA meet this
expanded role, EPA's National Homeland Security Research Center (NHSRC) was established. The
NHSRC research program is focused on conducting research and delivering products that improve the
capability of the Agency to carry out its homeland security responsibilities.
One specific focus area of NHSRC's research is to support the Environmental Response Laboratory
Network (ERLN), a nationwide association of federal, state, local, and commercial environmental
laboratories, established by EPA. The ERLN can be deployed in response to a large-scale environmental
disaster by providing consistent analytical capabilities, capacities, and quality data in a systematic,
coordinated manner. Toward this end, NHSRC has worked with experts from across EPA and other
federal agencies to develop a compendium of analytical methods to be used in support of remediation
following national homeland security related incidents. For specific analytes that have been determined
to be of concern during a homeland security related event, analytical methods have been chosen to
measure levels of contamination in different environmental matrices. The results of these efforts have
been published in EPA's Standardized Analytical Methods for Environmental Restoration Following
Homeland Security Events (SAM), available at http://www.epa.gov/sam.
In identifying and selecting appropriate analytical methods to be used in such instances, EPA recognized
that there may be situations in which laboratories receive large numbers of samples or when rapid
analyses are needed to support decision making. This document partially addresses these situations by
providing summary information regarding techniques, instruments, and/or methods that can be
used for rapid laboratory screening of samples and preliminary identification of the chemical and
radiochemical analytes listed in SAM.
NHSRC has made this publication available to assist in preparing for and recovering from disasters
involving chemical, radiochemical, and biological contamination; it specifically represents an important
next step in supporting the ERLN. We value your comments as we move toward the development of an
efficient process to manage environmental samples and move EPA one step closer to achieving its
homeland security mission and its overall mission of protecting human health and the environment while
supporting sustainable solutions.
Gregory D. Sayles, Ph.D., Acting Director
National Homeland Security Research Center
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Table of Contents
ACKNOWLEDGEMENTS ii
LIST OF TABLES iv
ACRONYMS AND ABBREVIATIONS v
1.0 BACKGROUND 1
2.0 SCOPE AND APPLICATION 1
2.1 Preliminary Identification Analysis 2
2.2 Information Tables 2
2.3 Limitations 2
3.0 REFERENCES 3
List of Tables
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for
the Chemical Analytes Listed in SAM
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for
the Radiochemical Analytes Listed in SAM
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Acronyms and Abbreviations
AA Atomic Absorption
AES Atomic Emission Spectrometry or Spectrograph
AMD Automated Multiple Development
ASTM American Society for Testing and Materials
APCI Atmospheric Pressure Chemical lonization
°C Degrees Centigrade
CaCO3 Calcium carbonate
CERCLA Comprehensive Environmental Response, Compensation, and Liability Act
CFR Code of Federal Regulations
CSC Computer Sciences Corporation
CVA Coefficient of variation
2-CVAA 2-Chlorovinylarsonous acid
DDE Dichlorodiphenyldichloroethylene
DDT Dichlorodiphenyltrichloroethane)
DESI Desorption Electrospray lonization
DIMP Diisopropyl methylphosphonate
DMT 3,4-Dimercaptotoluene
DMT N,N-Dimethyltryptamine
DNT Dinitrotoluene
2,6-DNT 2,6-Dinitrotoluene
DSCM Dry standard cubic meter
EA2192 Diisopropylaminoethyl methylthiophosphonate
ECD Electron Capture Detector
ED Ethyldichloroarsine
EDEA N-Ethyldiethanolamine
EOT 1,2-Ethane dithiol
El Electron ionization
ELISA Enzyme Linked Immunosorbent Assay
EMPA Ethyl methylphosphonic acid
EMSL Environmental Monitoring and Support Laboratory
EPA U.S. Environmental Protection Agency
ESI Electrospray lonization
FID Flame lonization Detector
FL Fluorescence
FPD Flame Photometric Detector
FRMAC Federal Radiological Monitoring and Assessment Center
FTIR Fourier Transform Infrared
g Gram(s)
GA Tabun
GB Sarin
GC Gas Chromatograph or Gas Chromatography
GD Soman
GE 1-Methylethyl ester ethylphosphonofluoridic acid
GF Cyclohexyl sarin
GFAAS Graphite Furnace Atomic Absorption Spectrophotometer or Spectrophotometry
HASL Health and Safety Laboratory (currently Environmental Measurements Laboratory)
HD Mustard, sulfur/mustard gas
HMTD Hexamethylenetriperoxidediamine
HMX Octahydro-l,3,5,7-tetranitro-l,3,5,7-tetrazocine
HN-1 Nitrogen mustard 1; bis(2-chloroethyl)ethylamine
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HN-2 Nitrogen mustard 2; N,N-bis(2-chloroethyl)methylamine
HN-3 Nitrogen mustard 3; tris(2-chloroethyl)amine
HPLC High Performance Liquid Chromatograph or Chromatography
HPTLC High Performance Thin-layer Chromatography
HRP Horseradish peroxidase
1C Ion Chromatograph or Chromatography
ICP Inductively Coupled Plasma
IMPA Isopropyl methylphosphonic acid
ISE Ion Specific Electrode
JCAD Joint Chemical Agent Detector
kg Kilogram(s)
L Liter
L-l Lewisite 1; 2-Chlorovinyldichloroarsine
L-2 Lewisite 2; bis(2-Chlorovinyl)chloroarsine
L-3 Lewisite 3; tris(2-Chlorovinyl)arsine
LC Liquid Chromatograph or Chromatography
LLE Liquid-Liquid Extraction
M Molar (concentration)
m3 Cubic meter(s)
MCPA 2-methyl-4-chlorophenoxyacetic acid; (4-chloro-2-methylphenoxy) acetic acid
MDL Method detection limit
MEKC Micellar electrokinetic capillary chromatorgraphy
MeOH Methanol
mg Milligram(s)
mL Milliliter(s)
mm Millimeter(s)
MPA Methylphosphonic acid
MS Mass Spectrometer or Spectrometry
MSB Mass Selective Detector
n Number
N Normal
NG Nitroglycerine
ng Nanogram(s)
NHSRC National Homeland Security Research Center
NIOSH National Institute for Occupational Safety and Health
NIST National Institute of Standards and Technology
nm Nanometer(s)
NPD Nitrogen-phosphorus Detector
NOS Not Otherwise Specified
NTP National Toxicology Program
OAQPS Office of Air Quality Planning and Standards
ORD Officer of Research and Development
ORIA Office of Radiation and Indoor Air
ORISE Oak Ridge Institute for Science and Education
OSHA Occupational Safety and Health Administration
OVS OSHA Versatile Sampler (tube)
OW Office of Water
PAO Phenylarsine oxide
pCi Picocurie(s)
PDECD Pulsed Discharge Electron Capture Detector
PDMS Polydimethyl siloxane
PERALS® Photon-electron Rejecting Alpha Liquid Scintillation
PETN Pentaerythritol tetranitrate
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pg. Page(s)
PID Photo-ionization Detector
PMPA Pinacolyl methyl phosphonic acid
ppb Parts per billion
ppm Parts per million
ppt Parts per trillion
PV Partially validated
QC Quality Control
RCRA Resource Conservation and Recovery Act
RDX Hexahydro-l,3,5-trinitro-l,3,5-triazine
Rh-102m Metastable rhodium-102
RSD Relative Standard Deviation
SAM Standardized Analytical Methods for Environmental Restoration Following Homeland
Security Events
SDWA Safe Drinking Water Act
SIM Selective Ion Monitoring
SM Standard Method
SPADNS 4,5-Dihydroxy-3-(p-sulfophenyazo)-2,7-hapthalene-disulfonic acid trisodium salt
SPE Solid-Phase Extraction
SPME Solid-Phase Microextraction
SRM Standard Reference Matrix
SW Solid Waste
S:N Signal-to-noise ratio
TATP Triacetone triperoxide
Tc-99m Metastable technetium-99
TDE Tetrachlorodiphenylethane
TDG Thiodiglycol
TEA Triethanolamine
TLC Thin-Layer Chromatography
1,3,5-TNB 1,3,5-Trinitrobenzene
TNT Trinitrotoluene
2,4,6-TNT 2,4,6-Trinitrotoluene
TO Toxic Organics
UV Ultraviolet
VE Phosphonothioic acid, ethyl-, S-(2-(diethylamino)ethyl) O-ethyl ester
VM Phosphonothioic acid, S-(2-(diethylamino)ethyl) O,O-diethyl ester
VR (R-33) Methylphosphonothioic acid, S-[2-(diethylamino)ethyl] O-2-methylpropyl ester
V/V Volume/Volume
VX O-Ethyl-S-(2-diisopropylaminoethyl)methylphosphonothiolate
Xe -131 m Metastable xenon-131
VII
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SAM Companion - Rapid Screening and Preliminary Identification Techniques and Methods
Rapid Screening and Preliminary Identification
Techniques and Methods
[Companion to Standardized Analytical Methods for Environmental
Restoration Following Homeland Security Events (SAM)]
1.0 Background
The U.S. Environmental Protection Agency's (EPA's) National Homeland Security Research
Center (NHSRC) has worked with experts from across EPA and its sister agencies since 2003 to
develop a compendium of analytical methods to be used when multiple laboratories are needed
to analyze samples during environmental restoration following national homeland security
related incidents. Analytical methods have been selected for measurement of chemical,
radiochemical, pathogen, and biotoxin analytes of concern for the types of environmental sample
matrices that are anticipated to be impacted by such incidents. The results of these efforts have
been published in several revisions of EPA's Standardized Analytical Methods for
Environmental Restoration Following Homeland Security Events (SAM), available at
http://www.epa.gov/sam. NHSRC periodically reviews and updates the SAM document to
reflect improvements in analytical methods and new technologies, and to incorporate changes in
target analytes.
During development of SAM, EPA recognized that there may be situations in which laboratories
receive large numbers of samples or when rapid analyses are needed to support decision making.
This document is intended to partially address these situations by providing summary
information regarding techniques, instruments, and/or methods that can be used for rapid
laboratory screening of samples and preliminary identification of the chemical and
radiochemical analytes listed in SAM, Revision 5.0. As with SAM, NHSRC plans to update
the information in this document periodically to reflect changes to the analytes and/or methods.
The information contained in this document is intended to support NHSRC's effort to
provide procedures for use when multiple laboratories are needed to perform rapid
preliminary analysis of environmental samples following a homeland security event. The
information will be reviewed and updated periodically, along with the SAM document, to
reflect advances in technologies, results of equipment testing and method evaluation, and
additional analytes or sample matrices.
2.0 Scope and Application
The information in this document is intended to assist the parties responsible for preparing
laboratories and/or response programs for scenarios in which rapid screening of environmental
samples is required. This document provides general information for use by EPA and its
contractors when rapid preliminary analysis of samples is needed to support and expedite
decision making. Information included in this document should be used to support decisions
regarding sample disposition, sample prioritization, and selection of confirmatory analytical
methods (i.e., what method/instrumentation should be used for analyte confirmation and
measurement). It is assumed that personnel using the information are knowledgeable about the
SAM, Revision 5.0 and its methods are available at: www.epa.gov/sam/pdfs/reportSAM092909.pdf.
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SAM Companion - Rapid Screening and Preliminary Identification Techniques and Methods
contaminants of concern and experienced in applying the equipment and procedures for
preparation and analysis of environmental samples.
2.1 Preliminary identification Analysis
Unlike SAM, which identifies a single method for confirmatory analysis and
measurement of each analyte in each sample type pair, this companion document lists
multiple options that are considered appropriate for providing preliminary
presence/absence determinations and identification of SAM chemical and radiochemical
analytes. It is assumed that, at this stage in sample analysis, the type of contamination is
known (e.g., radiochemical, chemical, organic versus inorganic, chemical agents) and
rapid decisions are needed to avoid use of inappropriate or time-consuming confirmatory
analyses. Summary information is provided regarding equipment and procedures that
can be used for each chemical and radiochemical analyte in each environmental sample
matrix listed in SAM, Revision 5.0, along with sources for additional information and
summary comments regarding equipment considerations.
2.2 Information Tables
This document contains the following two tables which provide information
regarding techniques, equipment, equipment capabilities (where available), and
additional sources of information:
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for
the Chemical Analytes Listed in SAM
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for
the Radiochemical Analytes Listed in SAM
Types of information provided in the tables include:
• Analyte - The compound or class of compounds that will be targeted by the
screening procedure. The analytes in this document are identical to those listed in
SAM.
• Matrix - The principal material of which the sample is composed. The matrices in
this document are identical to the sample types listed for each analyte in SAM,
Revision 5.0.
• Reference Source - The reference(s) supporting the information that is provided in
the table.
• Technique - The equipment, instrumentation, and/or method that can be used for
preliminary identification of an analyte or class of analytes in the environmental
sample type (matrix).
2.3 Limitations
This document provides only summary information regarding techniques that can be used
for rapid screening of samples for preliminary identification of the chemical and
radiochemical analytes listed in SAM. Pathogen and biotoxin analytes are not addressed
in the document at this time.
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SAM Companion - Rapid Screening and Preliminary Identification Techniques and Methods
General information regarding currently available equipment and protocols is included;
details regarding equipment use or analytical procedures, laboratory or field
requirements, or analytical concerns are not provided. The document is intended for use
in assisting responsible parties in preparing for scenarios in which rapid screening of
environmental samples is required. It does not provide detailed procedures, laboratory or
field requirements, and does not address analytical concerns. Document users should
consult the sources cited in Section 3.0 (References) and in Tables 1 and 2 for additional
details regarding testing and use of the equipment or methods listed. If confirmatory
identification or quantification of the analytes is needed, laboratories should consult with
the SAM document to identify appropriate analytical methods.
Although at this time, not all of the techniques and methods listed have been tested for a
particular analyte or matrix, the information listed is considered to be the most
appropriate information available at the time of publication. The SAM workgroup plans
to review and update SAM and the SAM companion documents periodically to reflect
advances in technologies, results of procedure evaluation and validation studies, and
additional analytes or matrices.
3.0 References
Analytical methods listed in Tables 1 and 2 can be accessed through SAM at: www.epa.gov/sam.
In addition to these methods, the following resources were used to prepare this document:
• Black, R.M., and Read, R.W. 1998. "Analysis of Degradation Products of Organophosphorus
Chemical Warfare Agents and Related Compounds by Liquid Chromatography-Mass
Spectrometry Using Electrospray and Atmospheric Pressure Chemical lonization." Journal of
Chromatography. 794: 234-244.
• Carrick, W.A., Cooper, D.B., and Muir, B. 2001. "Retrospective Identification of Chemical
Warfare Agents by High-Temperature Automatic Thermal Desorption-Gas Chromatography-
Mass Spectrometry." Journal of Chromatography A. 925: 241-249.
• Chua, H-C., Lee, H-S., and Sng, M-T. 2006. "Screening of Nitrogen Mustards and Their
Degradation Products in Water and Decontamination Solution by Liquid Chromatography-
Mass Spectrometry." Journal of Chromatography A. 1102: 214-223.
• Collin, O.L., Beier, M., and Jackson, G.P. "Detection of Explosives by Fast GC-Fast MS
Using an Ion Trap" (poster). Athens, OH: Ohio University, Department of Chemistry and
Biochemistry, Center for Intelligent Chemical Instrumentation.
http://oak.cats.ohiou.edu/~jacksong/Presentations/PosterExploTSWG_ver2.pdf (accessed on
November 19, 2009)
• Collin, O.L., Niegel, C., Derhodes, K.E., McCord, B.R, and Jackson, G.P. 2006. "Fast Gas
Chromatography of Explosive Compounds Using a Pulsed-Discharge Electron Capture
Detector." Journal of Forensic Science. 51: 815.
• Cotte-Rodriquez, I., Had, C., and Cooks, R.G. 2006. "Rapid Trace Detection of Triacetone
Triperoxide (TATP) by Complexation Reactions During Desorption Electrospray lonization."
Chemistry Communications. 93: 953-955.
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SAM Companion - Rapid Screening and Preliminary Identification Techniques and Methods
• Defense Threat Reduction Agency. 1997. Sample Preparation Method for GC/MS Analysis
On Site Joint Document: United States/Finland. 1: 1-125.
• Doble, P., Paull, B., and Roux, C. 2005. "Rapid Screening of Selected Organic Explosives by
High Performance Liquid Chromatography Using Reversed-Phase Monolithic Columns."
Journal of Forensic Science. 49(6): 1181-1186.
• Eckenrode, B.A. 1998. "The Application of an Integrated Multifunctional Field-Portable
GC/MS System" Field Analytical Chemistry and Technology. 2: 3-20.
• Federal Bureau of Investigation, Laboratory Division. Forensic Science and Communications
http://www.fbi.gov/hq/lab/fsc/current/backissu.htm (Accessed November 18, 2009)
• Fengmao, L., Bischoff, G., Pestemer, W., Wenna, X., and Kofoet, A. 2006. "Multi-Residue
Analyses of Some Polar Pesticides in Water Samples with SPE and LC-MS-MS."
Chromatogrpahia. 63(5/6): 233-237.
• Fung, Y.S., and Mak, J.L. 2001. "Determination of Pesticides in Drinking Water by Micellar
Electrokinetic Capillary Chromatography." Electrophoresis. 22(11): 2260-2269.
• Guan, F., Ishiia, A., Senoa, H., Watanabe-Suzukia, K., Kumazawab, T., and Suzuki, O. 1999.
"Use of an Ion-Pairing Reagent for High-Performance Liquid Chromatography-Atmospheric
Pressure Chemical lonization Mass Spectrometry Determination of Anionic Anticoagulant
Rodenticides in Body Fluids." Journal of Chromatography B. 731: 155-165.
• Haas, J.S., and Gonzalez, A.M. 2003. "Rapid On-Site Environmental Sampling and Analysis
of Propellant Stabilizers and Their Decomposition Products by Portable Sampling and Thin-
Layer Chromatography Kits." Paper presented at Chemistry for the Protection of the
Environment, June 9-12, 2002, in Hilo, HI.
• Hach Company. 2008. Hach Water Analysis Handbook. 5th Edition. Loveland, CO: Hach
Company, http://www.hach.com (accessed November 18, 2009)
• Health and Safety Laboratory. 1997. "Volatile Organic Compounds in Air•." Methods for the
Determination of Hazardous Substances. 88: 1-20.
• Hiemstra, M., and de Kok, A. 2007. "Comprehensive Multi-Residue Method for the Target
Analyses of Pesticides in Crops Using Liquid Chromatography-Tandem Mass Spectrometry."
Journal of Chromatography A. 1154(1): 3-25.
• Jibao, C., Baizhan, L., Ping, L., and Qingde, S. 2003. "Fast Analysis of Nicotine Related
Alkaloids in Tobacco and Cigarette Smoke by Megabore Capillary Gas Chromatography."
Journal of Chromatography A. 1017: 187-93.
• Lakshmi, V.V.S., Murty, M.R.V.S., Jagadeshwar, R.T., Ravikumar, M., Prabhakar, S., and
Vairamani, M. 2006. "Electrospray lonisation Mass Spectral Studies on Hydrolysed Products
of Sulfur Mustards." Rapid Communications in Mass Spectrometry. 20: 981-986.
• Lambropoulou, D.A., Sallas, V.A., Hela, D.G., and Albanis, T.A. 2002. "Application of
Solid-Phase Microextraction in the Monitoring of Priority Pesticides in the Kalamas River
(N.W.Greece)." Journal of Chromatography A. (963) 107-116.
September 2010
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SAM Companion - Rapid Screening and Preliminary Identification Techniques and Methods
• Logan, T.P., Smith, J.R., Jakubowski, E.M., and Nielson, R.E. 1999. "Verification of
Lewisite Exposure by the Analysis of 2-Chlorovinyl Arsonous Acid in Urine." Toxicology
Methods. 9: 275-294.
• Luan, T., Li, G., Zhao, M., and Zhang, Z. 2000. "Rapid Detection of
Tetramethylenedisulfotetramine in Human Blood by Solid-Phase Microextraction/Gas
Chromatography." AnalyticaChimicaActa. 404(2): 329-334.
• Muir, B., Coopera, D.B., Carricka, W.A., Timperleya, C.M., Slatera, B.J., and Quicka, S.
2005. "Analysis of Chemical Warfare Agents III. Use of bis-Nucleophiles in the Trace Level
Determination of Phosgene and Perfluoroisobutylene." Journal of Chromatography A. 1098:
156-165.
• National Bureau of Standards (NBS). August 1963. National Bureau of Standards Handbook,
Edition 69. Washington D.C., U.S. Government Printing Office.
• National Environmental Methods Index (NEMI). EPA, U.S., Geological Survey.
http://www.nemi.gov/apex/f?p=237:1:4430599066237331 (accessed November 18, 2009)
• Nogueira, J.M.F., Sanra, T., and Sanddra, P. 2004. "Multiresidue Screening of Neutral
Pesticides in Water Samples by High Performance Liquid Chromatography-Electrospray
Mass Spectrometry." Analytica Chimica Acta. 505: 209-215.
• Osolinski, T.W., and Knight, N.H. 1968. "Determination of Osmium by Atomic Absorption
Spectrophotometry" Applied Spectroscopy. 22(5): 532-535.
• Papadopoulou-Mourkidou, E., and Patsias, J. 1996. "Development of a Semi-Automated
High-Performance Liquid Chromatographic-Diode Array Detection System for Screening
Pesticides at Trace Levels in Aquatic Systems of the Axios River Basin." Journal of
Chromatography. 726: 99-113.
• Read, R.W., and Black, R.M. 1999. "Rapid Screening Procedures for the Hydrolysis Products
of Chemical Warfare Agents Using Positive and Negative Ion Liquid Chromatography-Mass
Spectrometry with Atmospheric Pressure Chemical lonization." Journal of Chromatography
A. 862(2): 169-177.
• Retho, C., and Blanchard, F. 2005. "Determination of 3-Chloropropane-l,2-diol as its 1,3-
Dioxolane Derivative at the Kg/Kg 1 Level: Application to a Wide Range of Foods." Food
Additives and Contaminants. 22(12): 1189-1197.
• Richter, P., Sepulveda, B., Oliva, R., Calderon, K., and Seguel, R. 2003. "Screening and
Determination of Pesticides in Soil Using Continuous Subcritical Water Extraction and Gas
Chromatography-Mass Spectrometry." Journal of Chromatography A. 994: 169-177.
• Ruangyuttikam, W., Law, M.Y., Rollins, D.E., and Moody, D.E. 1990. "Detection of
Fentanyl and Its Analogs by Enzyme-Linked Immunosorbent Assay." Journal of Analytical
Toxicology. 14(3): 160-164.
• Schulte-Ladbeck, R., Kolla, P., and Karst, U. 2003. "Trace Analysis of Peroxide-Based
Explosives." Analytical Chemistry. 75(4): 731-735.
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SAM Companion - Rapid Screening and Preliminary Identification Techniques and Methods
• Seta, Y., Kanamori-Kataoka, M., Tsuge, K., Ohsawa, I., Matushita, K., Sekiguchi, H., Itoi,
T., lura, K., Sano, Y., and Yamashira, S. 2005. "Sensing Technology for Chemical-Warfare
Agents and Its Evaluation Using Authentic Agents." Sensors and Actuators B. 108: 193-197.
• Smith, D.B., and Krause, L.A. 1978. "Analysis of Charcoal Tube Samples for Carbon
Bisulfide Using a Photoionization Detector. "American Industrial Hygiene Association
Journal. 39(12): 939-944.
• Smith, P.A., Lepage, C.R., Koch, D., Wyatt, H.D.M., Hook, G.L., Betsinger, G., Erickson,
R.P., and Eckenrode, B.A. 2004. "Detection of Gas-Phase Chemical Warfare Agents Using
Field-Portable Gas Chromatograph-Mass Spectrometry Systems: Instrument and Sampling
Strategy Considerations." TrAC - Trends in Analytical Chemistry. 23(4): 296-306.
• Steuckart, C., Berger-Preiss, E., and Levsen, K. 1994. "Determination of Explosives and
Their Biodegradation Products in Contaminated Soil and Water from Former Ammunition
Plants by Automated Multiple Development High-Performance Thin-Layer
Chromatography." Analytical Chemistry. 66: 2570-2577.
• Stuff, J.R., Cheicanter, R.L., Durst, H.D., and Ruth, J.L. 1999. "Detection of the Chemical
Warfare Agents bis-(2-Chloroethyl)ethylamine (HN-1) and tris-(2-Chloroethyl)amine (HN-3)
in Air." Journal of Chromatography A. 849: 529-540.
• Subbiaha, D., Kalab, S., and Mishra, A.K. 2005. "Study on the Fluorescence Characteristics
of Bromadiolone in Aqueous and Organized Media and Application in Analysis."
Chemosphere. 61: 1580-1586.
• Syage, J.A., Cai, S-S., Jianwei, L., and Evans, M.D. 2006. "Direct Sampling of Chemical
Weapons in Water by Photoionization Mass Spectrometry." Analytical Chemistry. 78: 2967-
2976.
• Tomkins, B.A. 1994. "Screening Procedure for Sodium Fluoroacetate (Compound 1080) at
Sub-Microgram Concentrations in Soils." Analytical Letters. 27(14): 2703-2718.
• Tomkins, B.A., Sega, G.A., and Ho, C.-H. 2001. "Determination of Lewisite Oxide in Soil
Using Solid-Phase Microextraction Followed by Gas Chromatography with Flame
Photometric or Mass Spectrometric Detection." Journal of Chromatography A. 909: 13-28.
• U.S. Department of Energy, Office of Environmental Policy and Assistance Air, Water and
Radiation Division (EH-412). June 1998. Compendium of EPA-Approved Analytical Methods
for Measuring Radionuclides in Drinking Water.
http://www.orau.org/ptp/PTP%20Librarv/library/DOE/Misc/radmeth3.pdf (accessed
November 18, 2009)
• U.S. Department of Transportation. 49 CFR 173.443. Contamination Control.
http://ecfr.gpoaccess.gov/cgi/t/text/text-
idx?c=ecfr&sid=83da38916033d89f6878ec32ec075547&rgn=div5&view=text&node=49:2.1
.1.3.8&idno=49#49:2.1.1.3.8.9.25.28 (accessed November 4, 2009)
• U.S. Environmental Protection Agency. 40 CFR 141.66. Safe Drinking Water Act, Maximum
Contaminant Levels for Radionuclides.
http://edocket.access.gpo.gov/cfr 2006/julqtr/pdf/40cfr 14L66.pdf (accessed November 18,
2009)
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U.S. Environmental Protection Agency. 40 CFR 300 - 310. Comprehensive Environmental
Response, Compensation, and Liability Act (CERCLA).
http://ecfr.gpoaccess.gov/cgi/t/text/text-
idx?sid=3ed9067eOaa631b91cdOe90a88cd904b&c=ecfr&tpl=/ecfrbrowse/Title40/40cfrv27 0
2.tpl (accessed November 19, 2009)
U.S. Nuclear Regulatory Commission. 10 CFR 20 Subpart O, Appendix B. Standards for
Protection Against Radiation, Enforcement, http://www.nrc.gov/reading-rm/doc-
collections/cfr/part020/ (accessed November 19, 2009)
Van Bergen, C. A., Collier, P.D., Cromie, D.D.O., Lucas, R.A., Preston, H.D., and Sissons,
D.J. 1992. "Determination of Chloropropanols in Protein Hydrolysates." Journal of
ChromatographyA. 589: 109-119.
Xu, X., de Craats, A.M., and de Bruyn, P. 2004. "Highly Sensitive Screening Method for
Nitroaromatic, Nitramine and Nitrate Ester Explosives by High Performance Liquid
Chromatography-Atmospheric Pressure lonization-Mass Spectrometry (HPLC-API-MS) in
Forensic Applications." Journal of Forensic Science. 49(6): 1171-80.
Xu, X., Song, G., Zhu, Y., Zhang, J., Zhao, Y., Shen, H., Cai, Z., Han, J., and Ren, Y. 2008.
"Simultaneous Determination of Two Acute Poisoning Rodenticides Tetramine and
Fluoroacetamide with a Coupled Column in Poisoning Cases." Journal of Chromatography
B. 876(1): 103-108.
September 2010
-------
SAM Companion - Rapid Screening and Preliminary Identification Techniques and Methods
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM
Note: When available, information is provided regarding detection, quantitation, working range, performance, sample throughput, sample preparation, and interferences (see Comments column).
Analyte
Matrix
Technique
Reference Source*
Comments
Acephate
Air
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
HPLC-MS
Journal of
Chromatography A.
2007. 1154(1): 3-25
Quantitation: 0.01 mg/kg (limit of quantification)
Working Range: 0.01 - 1.0 mg/kg
Performance: Mean recovery range 70 - 110 (±15%)
Sample Throughput: Retention time 4.70 min
Aqueous Liquid
Drinking Water
Chromatographia. 2006.
63(5/6): 233-237
Detection: Detection limit 30 [ig/L
Performance: Recovery range 95.3 - 118.4 %
Sample Throughput: Retention time 4.39 min
Acrylamide
Acrylonitrile
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
HPLC
EPA Method 8316 (SW-
846)
Detection: Detection limit 10 [ig/L (acrylamide) and 20 |jg/L (acrylonitrile)
Other: Full scan using limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but
no calibration standards)
Air
OSHA Method PV2004
Detection: Detection limit 0.7 |jg/mL (0.006 mg/m3 for a 1-mL desorption volume or 0.029 mg/m3 for a 5-
mL desorption volume based on a 120-L air volume)
Working Range: 0.017-1.5 mg/m3 (1-mL desorption volume) and 0.083 - 7.5 mg/m3 (5-mL desorption
volume)
Other: Full scan using limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but
no calibration standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -1
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference Source* Comments
Aldicarb (Temik)
Aldicarb sulfone
Aldicarb sulfoxide
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Immunoassay
RaPID Assay® Aldicarb
(built to order) (fieldable)
http://www.sdix.com
(accessed November 19,
2009)
Detection: Minimum detection level 0.25 ppb (as aldicarb)
Quantitation: 1-100 ppb (as aldicarb)
Sample Preparation: Oil samples and non-aqueous liquid samples require extraction into water
EnviroGard™ Aldicarb
Plate Kit (fieldable)
http://www.sdix.com
(accessed November 19,
2009)
Detection: Least detectable dose 0.4 |jg/L (aldicarb); 0.5 |jg/L (aldicarb sulfone); 25.0 |jg/L (aldicarb
sulfoxide)
Sample Preparation: Soil samples and non-aqueous liquid samples require extraction into water
Interferences: Particles in untreated ground and surface water can affect the minimum detectable level
Other: Does not differentiate between the three major forms of aldicarb (aldicarb, aldicarb sulfone, and
aldicarb sulfoxide)
HPLC
Journal of
Chromatography A.
1996.726:99-113
Detection: Detection range 0.5 - 1.0; limit of detection 0.1 |jg/L
Quantitation: 1-100 ppb (as aldicarb)
Working Range: Calibration range 1 - 1000 ng
Performance: Mean recovery 89 (±11)%
Sample Throughput: Retention time 23.8 minutes
Sample Preparation: Soil samples require extraction into water
Other: Diode array with online sample enrichment
HPLC-ESI-MS-SIM
Analytica Chimica Acta.
2004.505:209-215
Sample Preparation: SPE, soil samples, and non-aqueous liquid samples require extraction into water
Other: Tested for similar compounds (carbofuran, methomyl, oxamyl, etc.)
MEKC
Electrophoresis. 2001.
22(11): 2260-2269
Detection: Detection limit 0.46 |jg/L
Quantitation: Quantitation limit 1 |jg/L
Working Range: Working range 1 - 40 |jg/L
Performance: Recovery 48 (±26)% (drinking water)
Sample Throughput: Retention time <2 minutes
Sample Preparation: SPE and sample stacking. Solid samples require extraction into water. Water
samples require adjustment to pH 2 - 3.
Air
HPLC-UV
NIOSH Method 5601
Detection: Detection limit 0.005 |jg/L
Working Range: Working range 0.5 - 1 |jg/L
Sample Throughput: Retention times -13.5 minutes (in MeCN); -19.9 minutes (MeOH)
Sample Preparation: Collect air samples on sorbents. Extraction (with 0.2% V/V 0.1 M aqueous
triethylamine phosphate buffer in acetonitrile, pH 6.9 - 7.1) from filter/solid sorbent tube (OVS-2 Tube:
13-mm quartz fiber filter; XAD-2, 270 mg/140 mg)
Interferences: Potential interferences include chloroform, toluene, BHT, dialkyl phthalates, nicotine,
caffeine, impurities in HPLC reagents (e.g., in triethylamine), other pesticides (2,4-D, atrazine,
parathion, etc.), and pesticide hydrolysis products (1-naphthol)
Other: Full scan using limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but
no calibration standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -2
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Allyl Alcohol
4-Aminopyridine
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Aqueous Liquid
Drinking Water
Air
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
GC-MS
(purge and trap)
GC-FID (direct
injection)
GC-FID (direct
injection)
GC-MS
HPLC
HPLC
HPLC-ESI-MS-SIM
MEKC
Reference Source*
EPA Methods 5030C
(water), 5035A (solid), or
3585 (non-aqueous) with
8260C (SW-846)
EPA Method 801 5C (SW-
846)
EPA Method TO-8
(ORD)
Modified EPA Method
TO-10AorTO-17(ORD)
EPA Method 8330B (SW-
846)
Journal of
Chromatography A.
1996.726:99-113
Analytica Chimica Acta.
2004.505:209-215
Electrophoresis. 2001 .
22(11): 2260-2269
Comments
Detection: Detection limits 5 |jq/ka (wet weiaht) for soil/sediment samples: 0.5 ma/ka (wet weiaht) for
wastes; 5 |jg/L for ground water, using standard quadrupole instrumentation and the purge and trap
technique
Quantitation: Quantitation limit 5 |Jd/L (water): 5 |jq/ka (solid)
Workina Ranae: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples,
Method 5035A for solid samples, and Method 3585 for non-aqueous liquid/organic solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Sample Preparation: Based on Method 801 5C usina Method 5030C for preparation of water samples,
Method 5035A for solid samples, and Method 3585 for non-aqueous liquid/organic solid samples
Interferences: Samples can be contaminated by diffusion of volatile oraanics (particularly
chlorofluorocarbons and methylene chloride) through the sample container septum during shipment and
storage. Atrip blank prepared from organic-free reagent water and carried through sampling and
subsequent storage and handling must serve as a check on such contamination.
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Other: Aqueous impinaer collection
D^l-f^rn-l^l-l^^- Cr*r IWI^tkl^H TO -1 O A DCR r^mnfic- trjfinfmrj inn ^l-l -3 1-1-3 l\l+^\ fr^n-l Ci QOO/ /i-.-^CX- r^/*n\ /Ari Af
range from 65 - 1 25%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Detection: ppb levels of certain explosives and propellant residues
Sample Preparation: Soil and non-aqueous liquid/oraanic solid samples require extraction into water
Other: Diode array with online sample enrichment. Tested for similar compounds.
Sample Preparation: SPE. Soil and non-aqueous liquid/oraanic solid samples require extraction into
water.
Sample Preparation: SPE and sample stackina. Soil samples require extraction into water. Tested for
similar compounds.
Rapid Screening and Preliminary Identification Techniques and Methods
1 -3
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Ammonia
Matrix
Aqueous Liquid
Drinking Water
Air
Technique
Spectrophotometer
(fieldable)
Spectrophotometer
(fieldable)
Potentiometric-ion
selective electrode
Toxic Gas Leak
detector (fieldable)
Draeger gas
detection tube
Reference Source*
Hach Water Analysis
Handbook. 5th Edition.
2008
Hach Water Analysis
Handbook. 5th Edition.
2008
Hach Water Analysis
Handbook. 5th Edition.
2008
Hach Water Analysis
Handbook. 5th Edition.
2008
EPA Method 350.3 (OW)
CEA A-5200 Toxic Gas
Leak Detector
httD://www.ceainstr.com/
cdf datasheets/seriesu I
nfo.pdf (accessed
November 19, 2009)
Draeger gas detection
tube Ammonia 0.25/a
(P/N8101711);2/a(P/N
6733231 );5/b(P/N
8101941);5/a(P/N
CH20501)
httc://www.draeaer.com/
US/en US/ (accessed
November 19, 2009)
Comments
Detection: Detection ranae 0.02 - 2.5 ma/L
Interferences: Potential interferences include Cl, Ma, and Ca ions (>500 ma/L)
Other: Nessler method
Detection: Detection ranae 0.01 - 0.50 ma/L
Interferences: Potential interferences include CaCO, >1000 ma/L: Fe (all levels): Ma >6000 ma/L: NO,
>100 mg/L; NO2 >12 mg/L; PO4 >100 mg/L; SO4 >300 mg/L
Other: Salicvlate method
Detection: Detection ranae 0.01 - 0.50 ma/L
Interferences: Potential interferences include CaCO, >1000 ma/L: Fe (all levels): Ma >6000 ma/L: NO,
>100 mg/L; NO2 >12 mg/L; PO4 >100 mg/L; SO4 >300 mg/L
Other: Salicvlate method
Detection: Detection ranae 0.02 - 2.5 ma/L
Interferences: Potential interferences include Cl, Ma, and Ca ions (>500 ma/L)
Other: Nessler method
Detection: Detection ranae 0.01 - 0.50 ma/L
Other: Color and turbidity have no interferent effect
Detection: Detection ranaesO- 100 com: 0 -250 com : 0 -500 com : 0- 1000 com : 0-5000 com
Detection: Detection ranaes 0.25 - 3 ppm: 2-30 ppm: 2.5 - 100 ppm: 5 - 700 ppm
Sample Preparation: A calibrated 100-mL sample of air is drawn throuah the tube with a pump (Draeaer
accuro® or equivalent)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -4
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Ammonium
metavanadate (analyze
for total vanadium)
Arsenic, Total
Arsenic trioxide
(analyze for total
arsenic)
Arsine
Matrix
Air
(particulates)
Solid
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Air
Aqueous Liquid
Drinking Water
Solid
Wipes
Air
(particulates)
Solid
Wipes
Air
(particulates)
Solid
Wipes
Solid
Wipes
Technique
X-ray fluorescence
analyzer (fieldable)
Spectrophotometry
ICP-MS
ICP-AES
GC-PID, -FID, or-
ECD
Spectrophotometry
Draeger-type gas
detection tube or X-
ray fluorescence
analyzer (fieldable)
Draeger-type gas
detection tube or X-
ray fluorescence
analyzer (fieldable)
GFAAS, ICP, or GC-
MSD
Reference Source*
EPA Method 6200 (SW-
846)
Hach Water Analysis
Handbook. 5th Edition.
2008
SW-846 Method 6020A
(SW-846);
EPA Method 200.8 (OW)
SW-846 Method 601 OC
(SW-846);
EPA Method 200.7 (OW)
EPA field screening
Method FM9
Hach Water Analysis
Handbook. 5th Edition.
2008
Draeger gas detection
tube Arsine 140SA
httD://209.18.104.171/ucl
oads/docLib 639 140SA
.pdf (accessed
November 19, 2009)
Draeger gas detection
tube Arsine 0.05/a (P/N
CH25001)
http://www.draeaer.com/
US/en US/ (accessed
November 19, 2009)
EPA Methods 6020A,
601 OC, and 7010 (SW-
846);
EPA Methods 200.8 and
200.7 (OW)
Comments
Detection: Interference-free detection limit 40 ma/ka (arsenic)
Quantitation: Semi-quantitative
Interferences: Potential interferences include particle size, uniformity, homoaeneitv, surface condition,
high moisture content, and high concentration of other heavy metals
Detection: Detection ranae 0.02 - 0.20 ma/L (arsenic)
Interferences: Potential interferences include antimony salts
Other: Measures total arsenic. Silver diethvldithio-carbamate method.
Detection: In cases where low concentrations of compounds are beina addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES
Sample Preparation: Extraction in aqueous nitric acid
Other: Limited QC for rapid analysis
Detection: In cases where low concentrations of compounds are beina addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES
Sample Preparation: Extraction in aqueous nitric acid
Other: Limited QC for rapid analysis
Detection: Used to screen water, air, soil, and sediment samples on a GC with a PID, FID, or ECD
Sample Preparation: Method involves collectina desired sample in a 40-mL vial, preparina sample if soil
or sediment, and sampling and analyzing vapor headspace above aqueous solution
Other: Headspace analysis
Detection: Used to screen water, air, soil, and sediment samples on a GC with a PID, FID, or ECD
Sample Preparation: Method involves collectina desired sample in a 40-mL vial, preparina sample if soil
or sediment, and sampling and analyzing vapor headspace above aqueous solution
Detection: Detection limit 1 ppm (140SA): 0.05 - 60 ppm (0.05/a)
Other: Draeaer-tvpe aas detection tube on headspace of sample container or bv X-rav fluorescence
Detection: Detection limit 1 ppm (140SA): 0.05 - 60 ppm (0.05/a)
Other: Draeaer-tvpe aas detection tube on headspace of sample container or bv X-rav fluorescence
Detection: In cases where low concentrations of compounds are beina addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES
Sample Preparation: HNO, extraction. Extract soil sample or desorb arsine from soil.
Rapid Screening and Preliminary Identification Techniques and Methods
1 -5
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Asbestos
Boron Trifluoride
Brodifacoum
Bromadiolone
BZ [Quinuclidinyl
benzilate]
Matrix
Solid
Air
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Air (BZ only)
Technique
Polarized light
microscopy
TEM
AAorlCP-AES
Draeger gas
detection tube;
DraegerSensor®
ACL (fieldable)
ISE
HPLC-UV
HPLC-APCI-MS-SPE
HPLC-APCI-MS-LLE
Fluorescence with or
without HPLC
HPLC
Reference Source*
EPA Method 600/R-
93/11 6 (ORD)
NIOSH Method 7400
ASTM Method D6480-05
EPA Method 601 OC (SW-
846); EPA Method 200.7
(OW)
DraegerSensor® ACL
(P/N 6809375)
http://www.draeaer.co.uk/
ST/internet/cdf/Master/E
n/at/9023564 cvl ac d
e.pdf (accessed
November 19, 2009)
OSHA Method I D216SG
Chemosphere. 2005. 61 :
1580-1586
"A General Unknown
Screening For Drugs and
Toxic Compounds in
Human Serum." Thesis.
http://paaes.unibas.ch/di
ss/2005/DissB 7295.pdf
(accessed November 19,
2009)
Journal of
Chromatography B.
1999.731: 155-165
Chemosphere. 2005. 61 :
1580-1586
EPA Method TO-10A
(ORD)
Comments
Detection: Operates at maanifications of 400X and will not resolve fibers below 0.25 |jm in diameter.
Cannot distinguish asbestos fibers from other fibers (e.g., gypsum, mineral wool, fiberglass, cellulose,
etc.).
Other: Hard-surfaces wipes
Detection: Estimated detection limit 3.8 |Jd/L
Detection: Detection ranae 1-14 ppm: DraeaerSensor® 3-30 ppm
Detection: Detection limit 0.4 |Jd/mL (10 |ja/sample)
Detection: UV wavelenath 310 nm
Sample Preparation: Filtration, requires no extraction
Detection: Detection limit for bromadiolone in blood 1000 na/mL (positive ion mode): 250 na/mL
(negative ion mode)
Performance: Minimum recovery usina SPE cartridae 31% (bromadiolone)
Sample Throuahput: Retention time -12.86 minutes (bromadiolone)
Sample Preparation: SPE cartridae extraction
Detection: Detection limit 1.0 na/mL (blood): 0.5 na/mL (urine) (bromadiolone)
Sample Throuahput: Retention time -12.86 minutes (bromadiolone)
Sample Preparation: Extraction with ethvl acetate and evaporation to drvness, followed bv redissolvina
in acetonitrile
Detection: Detection limit for bromadiolone with the addition of cvclodexitrin 23 na/mL (the addition of
cyclodextrin resulted in an increase in fluorescence intensity at 390 nm of 13-fold)
Other: Method listed in SAM for BZ and similar compounds (pesticides and polvchlorinated biphenvls in
air)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -6
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Calcium arsenate
(analyze as total
arsenic)
Carbofuran (Furadan)
Matrix
Air
(particulates)
Solid
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Aqueous Liquid
Drinking Water
Technique
X-ray fluorescence
analyzer (fieldable)
Spectrophotometry
ICP-MS
ICP-AES
Immunoassay
HPLC
GC-MS
LC-ESI-MS-SIM
MEKC
Reference Source*
EPA Method 6200 (SW-
846)
Hach Water Analysis
Handbook. 5th Edition.
2008
EPA Method 6020A (SW-
846);
EPA Method 200.8 (OW)
EPA Method 601 OC (SW-
846);
EPA Method 200.7 (OW)
RaPID Assay®
Carbofuran Test Kit
http://www.sdix.com
(accessed November 19,
2009)
Journal of
Chromatography A.
1996.726:99-113
Journal of
Chromatography A.
2002.963: 107-116
Analytica Chimica Acta.
2004.505:209-215
Electrophoresis. 2001 .
22(11): 2260-2269
Comments
Detection: Interference-free detection limit 40 ma/ka (arsenic)
Quantitation: Semi-quantitative
Interferences: Potential interferences include particle size, uniformity, homoaeneitv, surface condition,
high moisture content, and high concentration of other heavy metals
Detection: Detection ranae 0.02 - 0.20 ma/L (arsenic)
Interferences: Potential interferences include antimony salts
Other: Measures total arsenic. Silver diethvldithio-carbamate method.
Detection: In cases where low concentrations of compounds are beina addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES
Sample Preparation: Extraction in aqueous nitric acid
Other: Limited QC for rapid analysis
Detection: In cases where low concentrations of compounds are beina addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES
Sample Preparation: Extraction in aqueous nitric acid
Other: Limited QC for rapid analysis
Detection: Detection limit 0.056 ppb
Quantitation: Quantitation ranae 0.1 -5.0 ppb. Can be used as a quantitative, semi-quantitative, or
qualitative enzyme immunoassay for analysis of carbofuran in water.
Detection: Detection limit 0.05 |ja/L
Performance: Recovery 102%
Sample Throuahput: Retention time -29 minutes
Other: Diode array with online sample enrichment
Detection: Detection limit 0.05 |ja/L
Performance: RSD 11%
Sample Throuqhput: Retention time -27.4 minutes
Sample Preparation: SPME
Detection: Detection limit 0.10 |ja/L
Performance: Recovery 76.3%
Sample Throuqhput: Retention time -11 minutes
Sample Preparation: SPE
Detection: Detection limit 0.17 |ja/L
Quantitation: Quantitation limit 0.4 |ja/L
Sample Throuahput: Retention time -2 minutes
Sample Preparation: SPE and sample stackina
Rapid Screening and Preliminary Identification Techniques and Methods
1 -7
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Carbofuran (Furadan)
Carfentanil
Matrix
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Technique
HPLC-FL, -UV, or
-MS
GC-MS
HPLC-UV
HPLC-UV
HPLC-APCI-MS-SPE
HPLC-APCI-MS-LLE
Immunoassay
Fluorescence with or
without HPLC
Reference Source*
EPA Methods 831 8A and
8321 B (SW-846)
Journal of
Chromatography A.
2003.994: 169-177
NIOSH Method 5601
Chemosphere. 2005. 61 :
1580-1586
"A General Unknown
Screening For Drugs and
Toxic Compounds in
Human Serum." Thesis.
http://paaes.unibas.ch/di
ss/2005/DissB 7295.pdf
(accessed November 19,
2009)
Journal of
Chromatography B.
1999.731: 155-165
Journal of Analytical
Toxicology. 1990. 14(3):
160-164
Chemosphere. 2005. 61 :
1580-1586
Comments
Workinq Ranqe: 0.5 - 5.0 ma/L
Sample Throuqhput: Retention time -18.28 minutes
Sample Preparation: Extraction with hexane, followed bv extraction with acetonitrile
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Detection: Detection limit 30.9 |ja/ka
Performance: Recovery 97.3%
Sample Throuahput: Extraction time 25 minutes: retention time 6.4 minutes
Sample Preparation: Subcritical water extraction
Detection: Detection limit 0.0025 ua/L
Workina Ranae: 0.05 - 1 ua/L
Sample Preparation: Collect air samples on sorbents
Other: Carbofuran has a very low vapor pressure (4.8 x 10~6 mm-Ha at 19 C): is not likely to be detected
in air using portable instruments
Sample Preparation: Filtration, requires no extraction
Sample Preparation: SPE cartridae extraction
Sample Preparation: Extraction with ethyl acetate and evaporation to drvness, followed bv redissolvina
in acetonitrile
Detection: 0.25 na/mL
Other: Tested for similar compounds (bromadiolone)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -8
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Carbon disulfide
Chlorfenvinphos
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
GC-MS (purge and
trap)
GC-ECD, -FPD, or
PID-MSD
GC-FPD
GC-FIDor-ECD
GC-MS (purge and
trap)
Reference Source*
EPA Methods 5030C
(water), 5035A (solid), or
3585 (non-aqueous) with
8260C (SW-846)
American Industrial
Hygiene Association
Journal. 1978.39(12):
939-944
No Method Identified
EPA Method TO-1 5
EPA Methods 5030C
(water) or 5035A (solid)
with 8260C (SW-846)
Comments
Detection: Detection limits 5 |jq/ka (wet weiaht) for soil/sediment samples: 0.5 ma/ka (wet weiaht) for
wastes; 5 |jg/L for ground water, using standard quadrupole instrumentation and the purge and trap
technique
Quantitation: Quantitation limit 5 |Jd/L (water): 5 |jq/ka (solid)
Workina Ranae: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples,
Method 5035A for solid samples, and Method 3585 for non-aqueous liquid/organic solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Detection: Detection ranae 1 .5 - 10 |ja/m3
Quantitation: 3 ppm for a 5-L air sample
Workina Ranae: 3-64 ppm for a 5-L air sample
Sample Preparation: Concentrate on charcoal tubes, extract with acetonitrile
Sample Preparation: Charcoal tube collection followed by solvent extraction
Other: Modified to use Tedlar® baas. Limited QC to ensure rapid analysis.
Detection: Detection limits 5 |ja/ka (wet weiaht) for soil/sediment samples: 0.5 ma/ka (wet weiaht) for
wastes; 5 |jg/L for ground water, using standard quadrupole instrumentation and the purge and trap
technique
Quantitation: Quantitation limit 5 |ja/L (water): 5 |ja/ka (solid)
Workina Ranqe: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples and
Method 5035Afor solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Rapid Screening and Preliminary Identification Techniques and Methods
1 -9
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference Source*
Comments
Chlorfenvinphos
Air
Automated thermal
desorption GC-MS
Journal of
Chromatography A.
2001.925:241-249
Quantitation: Semi-quantitative
Performance: RSD at 50 ng/tube for GB 21%; GD1 17%; GD2 13%; GA8%; GF 11%; VX30%; HN1
22%; HN228%; HNS 17%
Sample Throughput: Samples can be analyzed only once
Sample Preparation: Automated thermal desorption. Tube is connected to heated GC injector (100 C).
Other: Temperature and time of storage were found to influence recovery of analytes, with best
recoveries being observed after one day of storage in a freezer (-12 C)
Chlorine
Aqueous Liquid
Drinking Water
Amperometric
forward titration
(fieldable), ion
selective electrode,
or colorimetric
screening (fieldable)
Hach Water Analysis
Handbook. 5th Edition.
2008 or EPA Method
9212
Detection: Detection range 0 - 1000 |jg/L as CI2; detection range 0.4 - 1000 mg/L (Method 9212);
detection limit 2.0 mg/L (Method 9212)
Interferences: Potential interferences include Ag+, Cu+, Cu++; oxidized manganese; oxidizing agents;
high turbidity; high organic content; high concentrations of SO2, SO3, and bisulfite; highly buffered
samples
Other: Amperometric forward titration using 0.00564 N PAO (Hatch). Method 9212 is for the analysis of
simple chloride rather than total chloride.
Air
Draeger gas
detection tube
Draeger gas detection
tube Chlorine 0.2/3 (P/N
CH24301);0.3/b(P/N
6728411);50/a (P/N
CH20701)
http://www.draeger.com/
Detection: Detection ranges 0.2-30 ppm; 0.3- 10 ppm; 50-500 ppm
Sample Preparation: A calibrated 100-mL sample of air is drawn through the tube with a pump (Draeger
accuro® or equivalent)
US/en US/(accessed
November 19, 2009)
EPA Method 26A
(OAQPS)
Detection: Detection range 0.2 - 30 ppm; detection limit 0.1 |jg/mL
Interferences: Volatile materials, such as CIO2and NH4CI, which produce halide ions upon dissolution
during sampling, are potential interferents
Other: Collect gas/air in SUMMA canisters
2-Chloroethanol
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
GC-MS
EPA Methods 5030C
(water), 5035A (solid), or
3585 (non-aqueous) with
8260C (SW-846)
Detection: Detection limits 5 |jg/kg (wet weight) for soil/sediment samples; 0.5 mg/kg (wet weight) for
wastes; 5 |jg/L for ground water, using standard quadrupole instrumentation and the purge and trap
technique
Quantitation: Quantitation limit 5 |jg/L (water); 5 |jg/kg (solid)
Working Range: Calibration range 1-100 mg/L
Sample Preparation: Based on Method 8260 using Method 5030C for preparation of water samples and
Method 5035Afor solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan using limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Rapid Screening and Preliminary Identification Techniques and Methods
1 -10
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
2-Chloroethanol
3-Chloro-1,2-
propanediol
Matrix
Aqueous Liquid
Drinking Water
Air
Aqueous Liquid
Drinking Water
Air
Aqueous Liquid
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Technique
GC-FTIR
GC-MSor-FID
GC-FID (direct
injection)
GC-MS-SPE
GC-MS-SPE
GC-MS
Reference Source*
EPA Method 8340 (SW-
846)
Methods for the
Determination of
Hazardous Substances.
1997.88: 1-20
No Method Identified
EPA Method TO-8
Food Additives and
Contaminants. 2005.
22(12): 1189-1197
Journal of
Chromatography A.
1992.589: 109-119
"1 ,3-Dichloro-2-propanol,
Review of Toxicological
Literature" NTP, January
2005
httD://ntD.niehs.nih.aov/nt
D/htdocs/Chem Backaro
und/ExSumPdf/dichloroDr
opanol.pdf (accessed
November 19, 2009)
Comments
Detection: Minimum identifiable quantity 120 na
Workinq Ranqe: Workina ranae 25 - 500 ma/L
Sample Throuqhput: Run time 15 minutes
Sample Preparation: Direct aqueous injection
Interferences: Contaminants in solvents, reaaents, alassware, and other sample processina hardware
Workina Ranae: 1 - 1000 ma/m3
Sample Preparation: Use Draeaer diffusive sampler or sorbent tube (i.e, Anasorb® 747 or equivalent).
Analyze sampler or sorbent tube with GC-MSD or FID (NIOSH 2513), etc.
Interferences: Hiah humidity may affect recovery
Other: Limited QC for rapid analysis
Other: Aqueous impinaer collection
Sample Preparation: Elution from SPE column, Extrelut® 20 column, with ethyl acetate. Analysis by GC-
MS at the low ng/|jL level. Solids should be extracted with water prior to SPE.
Other: Limited QC for rapid analysis
Sample Preparation: Elution from SPE column, Extrelut® 20 column, with ethyl acetate. Analysis by GC-
MS at the low ng/|jL level.
Other: Limited QC for rapid analysis
Sample Preparation: Collect sample in SUMMA canister per method Method TO-15 and analyze by GC-
MS
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -11
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
3-Chloro-1,2-
propanediol
Chloropicrin
Chlorosarin
Matrix
Aqueous Liquid
Drinking Water
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Solid
Wipes
Technique
GC-FID (direct
injection)
GC-MS (purge and
trap)
Automated thermal
desorption GC-MS
GC-MS
Reference Source*
No Method Identified
EPA Method TO-8
EPA Methods 5030C
(water) or 5035A (solid)
with 8260C (SW-846)
Journal of
Chromatography A.
2001.925:241-249
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Comments
Other: Aqueous impinaer collection
Detection: Detection limits 5 |ja/ka (wet weiaht) for soil/sediment samples: 0.5 ma/ka (wet weiaht) for
wastes; 5 |jg/L for ground water, using standard quadrupole instrumentation and the purge and trap
technique
Quantitation: Quantitation limit 5 |Jd/L (water): 5 |jq/ka (solid)
Workina Ranae: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples and
Method 5035Afor solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Detection: Detection limit 50 no/tube (full scan). S:N ratio at 50 no/tube was >4:1 .
Quantitation: Semi-quantitative
Performance: RSD at 50 no/tube for GB 21%: GD1 17%: GD2 13%: GA8%: GF 11%: VX30%: HN1
22%; HN228%; HNS 17%
Sample Throuahput: Samples can be analyzed only once
Sample Preparation: Automated thermal desorption. Tube is connected to heated GC injector (100 C).
Other: Temperature and time of storaae were found to influence recovery of analvtes, with best
recoveries being observed after one day of storage in a freezer (-12 C)
Sample Throuahput: Samples can be analyzed only once
Sample Preparation: MeCI? extraction
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Rapid Screening and Preliminary Identification Techniques and Methods
1 -12
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Chlorosarin
Chlorosoman
Matrix
Aqueous Liquid
Drinking Water
Air
Non-aqueous
Liquid/Organic
Solid
Aqueous Liquid
Drinking Water
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Technique
Photoionization mass
spectrometry
Portable GC-MS
(fieldable)
GC-MS
Photoionization mass
spectrometry
GC-MS
Portable GC-MS
(fieldable)
Reference Source*
Analytical Chemistry.
2006. 78: 2967-2976
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Analytical Chemistry.
2006. 78: 2967-2976
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Comments
Sample Throuahput: Sample cycle time 45 seconds
Sample Preparation: Direct samplina in water
Other: Tested for a similar compound (GB)
Sample Throuqhput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Sample Throuqhput: Samples can be analyzed only once
Sample Preparation: MeCI? extraction
Other: Tested for MeCk GB, GD, HN, and CF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Detection: Method detection ranae 0.07 - 0.7 ma/L
Performance: RSDs were aenerallv <10%
Sample Throuqhput: Sample cycle time 45 seconds
Sample Preparation: Direct samplina in water
Other: Tested for similar compounds
Sample Throuqhput: Samples can be analyzed only once
Sample Preparation: MeCb extraction
Other: Tested for MeCk GB, GD, HN, and CF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Sample Throuqhput: Analysis time -16 minutes: total sample throuahput -3 samples/hour. Retention
time for GB -6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Rapid Screening and Preliminary Identification Techniques and Methods
1 -13
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
2-Chlorovinylarsonous
acid (2-CVAA)
(degradation product of
Lewisite)
Chlorpyrifos
Chlorpyrifos oxon
Matrix
Aqueous Liquid
Solid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
(particulates)
Solid
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Technique
GC-MS
Spectrophotometry
GC-MS
GC-MS-SPME
X-ray fluorescence
(fieldable)
Draeger gas
detection tube
(fieldable)
GC-MS (purge and
trap)
Automated thermal
desorption GC-MS
Reference Source*
Toxicology Methods.
1999.9:275-294
Hach Water Analysis
Handbook. 5th Edition.
2008
Toxicology Methods.
1999.9:275-294
Journal of
Chromatography A.
2001.909: 13-28
EPA Method 6200 (SW-
846)
Sensors and Actuators
B. 2005. 108: 193-197
EPA Methods 5030C
(water) or 5035A (solid)
with 8260C (SW-846)
Journal of
Chromatography A.
2001.925:241-249
Comments
Sample Preparation: Aqueous sample is extracted on C1 8 column, eluted with MeOH, dried and
derivatized with EOT, then shake and shoot
Other: If chromatoaraphic separation is not required, EOT can be omitted
Detection: Detection ranae 0.02 - 0.20 ma/L. Measures total arsenic.
Interferences: Potential interferences include antimony salts
Other: Silver diethvldithio-carbamate method.
Sample Preparation: Dissolve in MeCI? and derivatize with EOT
Other: If chromatoaraphic separation is not required, EOT can be omitted
Sample Throuqhput: Total sample processina time ~5 minutes
Sample Preparation: Soil samples are extracted usina ascorbic acid in water with propanedithiol,
centrifuged, and filtered. Analytes are concentrated from supernatant onto SPME fiber and detected by
GC-MS.
Detection: Interference-free detection limit 40 ma/ka
Interferences: Potential interferences include particle size, uniformity, homoaeneitv, surface condition,
high moisture content, and high concentration of other heavy metals
Other: Measures total arsenic
Detection: Detection in the sub-ma/m3 ranae
Sample Preparation: Takes several minutes for coloration to occur (could lead to false positives)
Other: Gives semi-qualitive information (i.e., can identify class of compound: phosphoric esters, oraano-
arsenic, thioether, cyanogen chloride, and cyanide)
Workinq Ranqe: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples and
Method 5035Afor solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Tested for similar compounds.
Quantitation: Semi-quantitative
Performance: RSD at 50 na/tube for GB 21%: GD1 17%: GD2 13%: GA8%: GF 11%: VX30%: HN1
22%; HN228%; HNS 17%
Sample Throuqhput: Samples can be analyzed only once
Sample Preparation: Automated thermal desorption. Tube is connected to heated GC injector (100°C).
Other: Temperature and time of storaae were found to influence recovery of analvtes, with best
recoveries being observed after one day of storage in a freezer (-12 C)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -14
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Crimidine
Cyanide, Amenable to
chlorination
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Solid
Wipes
Technique
HPLC
HPLC-ESI-MS-SIM
MEKC
Spectrophotometry
Spectrophotometry
(fieldable)
Reference Source*
Journal of
Chromatography A.
1996.726:99-113
Analytica Chimica Acta.
2004.505:209-215
Electrophoresis. 2001 .
22(11): 2260-2269
EPA Method 3135.21
(EPA RLAB)
Hach Water Analysis
Handbook. 5th Edition.
2008
Comments
Detection: Detection limit 0.1 |Jd/L
Performance: Recovery 89%
Sample Throuahput: Retention time -23.8 minutes
Sample Preparation: Soil and non-aqueous liquid/oraanic solid samples require extraction into water
Other: Diode array with online sample enrichment
Sample Preparation: SPE. Soil and non-aqueous liquid/oraanic solid samples require extraction into
water.
Detection: Detection limit 0.46 |Jd/L
Quantitation: Quantitation limit 1 |Jd/L
Sample Throuahput: Retention time <2 minutes
Sample Preparation: SPE and sample stackina. Soil samples require extraction into water.
Detection: Detection ranae 0.003 - 0.500 ma/L (cyanide in the distilate)
Sample Preparation: Acid diaestion followed by distilation
Detection: Detection ranae 0.001 - 0.240 ma/L
Sample Preparation: All samples to be analyzed for cyanide should be treated by acid distillation except
when experience has shown that there is no difference in results obtained with or without distillation
Interferences: Interferences include hiah levels of Cl, Ni, Co >1 ma/L, Cu >20 ma/L, Fe >5 ma/L, or
oxidizing agents. Remove metals by adding chelating reagents and remove oxidizing agents with
appropriate reagents.
Other: Pvridine-pvrazalone method
Rapid Screening and Preliminary Identification Techniques and Methods
1 -15
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Cyanide, Total
Matrix
Air
Aqueous Liquid
Drinking Water
Solid
Wipes
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Technique
Spectrophotometry
(fieldable)
EM Quant® Cyanide
Test (fieldable)
Draeger gas
detection tube
(fieldable)
Draeger gas
detection tube
(fieldable)
Spectrophotometry
Reference Source*
Hach Water Analysis
Handbook. 5th Edition.
2008
EM Quant® Cyanide
Test, Catalog (P/N
10044)
httD://www.aalladechem.c
om/ (accessed
November 19, 2009)
Draeger gas detection
tube Cyanogin chloride
0.25/a (P/N CH1 9801)
httD://www.afcintl.com/Ddf
/draeaer/CH19801.cdf
(accessed November 19,
2009)
Sensors and Actuators
B. 2005. 108: 193-197
Draeger gas detection
tube Cyanide 2/a (P/N
6728791 )
http://www.draeaer.com/
US/en US/ (accessed
November 19, 2009)
Hach Water Analysis
Handbook. 5th Edition.
2008
Comments
Detection: Detection ranae 0.001 - 0.240 ma/L
Sample Preparation: All samples to be analyzed for cyanide should be treated by acid distillation except
when experience has shown that there is no difference in results obtained with or without distillation
Interferences: Interferences include hiah levels of Cl, Ni, Co >1 ma/L, Cu >20 ma/L, Fe >5 ma/L, or
oxidizing agents. Remove metals by adding chelating reagents and remove oxidizing agents with
appropriate reagents.
Other: Pvridine-pvrazalone method
Detection: 1 - 30 ma/L
Sample Preparation: Soil is extracted into water
Interferences: Complexed cyanides and cyanides of Cu, Pd, Ha, and Aa aive low readinas or are not
detected at all
Detection: Detection ranae 0.25 - 5 ppm
Performance: Standard deviation is ±30%
Sample Throuahput: Measurement time ~five minutes
Interferences: Interferences include cvanoaen bromide
Detection: Detection ranae in the sub-ma/m3 ranae
Sample Throughput: Takes several minutes for tube coloration to occur
Other: Gives semi-qualitive information (i.e., can identify class of compound: phosphoric esters, oraano-
arsenic, thioether, cyanogen chloride, and cyanide)
Detection: Detection ranae 2-15 ma/m3
Sample Preparation: A calibrated 100-mL sample of air is drawn throuah the tube with a pump (Draeaer
accuro® or equivalent)
Detection: Detection ranae 0.01 - 0.50 ma/L
Interferences: Potential interferences include formaldehyde, sulfite, thiocvanate, and cyanide.
Other: Cvanoaen chloride method
Rapid Screening and Preliminary Identification Techniques and Methods
1 -16
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference Source*
Comments
Cyanogen chloride
Aqueous Liquid
Drinking Water
GC-MSD
EPA Method 524.2 (OW)
Sample Preparation: For soil samples, extract with water, purge, and trap
Other: Full scan using limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures because of thermal degradation.
Air
Portable GC-MS
(fieldable)
Sensors and Actuators
B. 2005. 108: 193-197
Detection: Detection limit 100 mg/m (in the no-GC separation mode)
Interferences: Potential interferences include Cl, Cu >20 mg/L, Fe >5 mg/L, oxidizing agents, and
reducing agents (these interferences can be eliminated by treatment)
Draeger gas
detection tube
(fieldable)
Draeger gas detection
tube Cyanogen chloride
0.25/a(P/NCH19801)
http://www.draeger.com/
US/en US/ (accessed
November 19, 2009)
Detection: Detection range 0.25 - 5 ppm
Sample Throughput: ~5 minutes per measurement
Sample Preparation: A calibrated 100-mL sample of air is drawn through the tube with a pump (Draeger
accuro® or equivalent)
Interferences: Cross sensitivity to cyanogen bromide
Draeger gas detection
tube Cyanogen chloride
0.25/a(P/NCH19801)
http://www.afcintl.com/pdf
/draeger/CH19801.pdf
(accessed November 19,
2009)
Cyclohexyl sarin (GF)
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
GC-MS
Air
GC-MS
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Performance: Recovery for GF 89 (±5)% (water); 74 (±10)% (soil)
Sample Throughput: Samples can be analyzed only once
Other: Tested for MeCI2, GB, GD, HD, and GF at concentrations of 5.0 mg/m3. Full scan using limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Journal of
Chromatography A.
2001.925:241-249
Detection: Detection limit 50 ng/tube (full scan). S:N ratio at 50 ng/tube was >4:1.
Quantitation: Semi-quantitative
Performance: RSD at 50 ng/tube for GB 21%; GD1 17%; GD2 13%; GA8%; GF 11%; VX30%; HN1
22%; HN228%; HNS 17%
Sample Throughput: Retention time -9.5 minutes. Samples can be analyzed only once.
Sample Preparation: Automated thermal desorption. Tube is connected to heated GC injector (100°C).
Other: Temperature and time of storage were found to influence recovery of analytes, with best
recoveries being observed after one day of storage in a freezer (-12 C)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -17
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Cyclohexyl sarin (GF)
1 ,2-Dichloroethane
(degradation product of
HD)
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
solid
Solid
Aqueous Liquid
Solid
Aqueous Liquid
Drinking Water
Air
Technique
Portable GC-MS
(fieldable)
Photoionization mass
spectrometry
GC-MS (purge and
trap)
GC-FIDor-MSD
GC-MS (purge and
trap)
GC-MS
GC-FID
Reference Source*
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Analytical Chemistry.
2006. 78: 2967-2976
EPA Methods 5030C
(water), 5035A (solid), or
3585 (non-aqueous) with
8260C (SW-846)
NIOSH Method 1003
EPA Method 524.2 (OW)
Field Analytical
Chemistry and
Technology. 1998.2(1):
3-20
EPA Method TO-3
(ORD)
Comments
Sample Throuahput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Detection: Method detection ranae 0.07 - 0.7 ma/L
Performance: RSDs <10%
Sample Throuahput: Sample cycle time 45 seconds
Sample Preparation: Direct samplina in water
Other: Tested for similar compounds
Detection: Detection limit 5 |ja/ka (wet weiaht) for soil/sediment: 0.5 ma/ka (wet weiaht) for wastes: 5
|jg/L for ground water, using standard quadrupole instrumentation and the purge and trap technique
Quantitation: Quantitation limit 5 |ja/L (water): 5 |ja/ka (solid)
Workina Ranae: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260, use Method 5030C for preparation of water samples,
Method 5035A for solid samples, and Method 3585 for non-aqueous liquid/organic solid samples
Interferences: Volatile materials in the laboratory and impurities in the inert puraina aas and in the
sorbent trap. May require low injection port temperatures due to thermal degradation.
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Sample Preparation: Collect sample headspace on sorbent tube for analysis usina GCD-FID or GC-
MSD
Detection: Detection limit 0.06 |ja/L
Performance: Mean accuracy of 0.1 - 10 |ja/L with RSD of 5.4%
Interferences: Volatile materials in the laboratory and impurities in the inert puraina aas and in the
sorbent trap. May require low injection port temperatures due to thermal degradation.
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Detection: Detection limit 0.81 ppb
Quantitation: Quantitation/qualifier ions 62, 49, 64
Sample Throuqhput: Elution time usina TO-14 aas mix 8.0 minutes: total time 15 minutes
Other: Usina VOCARB® 3000 Trap or eauivalent
Other: Tedlar® baa method. Limited QC for rapid analysis (e.a., an instrument blank and instrument
tune, but no calibration standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -18
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference Source*
Comments
Dichlorvos
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
solid
Solid
Wipes
GC-MS
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Sample Throughput: Samples can be analyzed only once
Sample Preparation: MeCI2 extraction
Other: Tested for MeCI2, GB, GD, HD, and GF at concentrations of 5.0 mg/m3. Full scan using limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Air
Portable GC-MS
(fieldable)
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Sample Throughput: Analysis time ~16 minutes; total sample throughput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD ~12 minutes; HD ~13 minutes; GF -14 minutes.
Sample Preparation: SPME sampling and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matching
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Dicrotophos
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
GC-MS (purge and
trap)
EPA Methods 5030C
(water) or 5035A (solid)
with 8260C (SW-846)
Working Range: Calibration range 1-100 mg/L
Sample Preparation: Based on Method 8260 using Method 5030C for preparation of water samples and
Method 5035Afor solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan using limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Tested for similar compounds.
Air
Automated thermal
desorption GC-MS
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Quantitation: Semi-quantitative
Performance: RSD at 50 ng/tube for GB 21%; GD1 17%; GD2 13%; GA8%; GF 11%; VX30%; HN1
22%; HN228%; HNS 17%
Sample Throughput: Samples can be analyzed only once
Sample Preparation: Automated thermal desorption. Tube is connected to heated GC injector (100 C).
Other: Temperature and time of storage were found to influence recovery of analytes, with best
recoveries being observed after one day of storage in a freezer (-12 C)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -19
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Diesel range organics
Diisopropyl
methylphosphonate
(DIMP) (degradation
product of GB)
Dimethylphosphite
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Solid
Wipes
Aqueous Liquid
Drinking Water
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
solid
Solid
Wipes
Technique
GC-MS
GC-MS
Photoionization mass
spectrometry
Portable GC-MS
(fieldable)
GC-MS
Reference Source*
EPA Method 801 5C (SW-
846)
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Analytical Chemistry.
2006. 78: 2967-2976
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Comments
Sample Preparation: Disolve in MeCk shake and shoot
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Sample Throuahput: Samples can be analyzed only once
Sample Preparation: MeCI? extraction
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Detection: Method detection ranae 0.07 - 0.7 ma/L
Performance: RSDs <10%
Sample Throuqhput: Sample cycle time 45 seconds
Sample Preparation: Direct samplina in water
Other: Tested for similar compounds
Sample Throuqhput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Sample Throuahput: Samples can be analyzed only once
Sample Preparation: MeCI? extraction
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Rapid Screening and Preliminary Identification Techniques and Methods
1 -20
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Dimethylphosphite
Dimethylphosphoramidi
c acid (degradation
product of GA)
Diphacinone
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
Portable GC-MS
(fieldable)
HPLC-APCI-MS-SIM
HPLC-MS
HPLC-UV
HPLC-APCI-MS-SPE
HPLC-APCI-MS-LLE
Reference Source*
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Journal of
Chromatography A.
1999.862(2): 169-177
Method TO-IOA(ORD)
Chemosphere. 2005. 61 :
1580-1586
"A General Unknown
Screening For Drugs and
Toxic Compounds in
Human Serum." Thesis.
http://paaes.unibas.ch/di
ss/2005/DissB 7295.pdf
(accessed November 19,
2009)
Journal of
Chromatography B.
1999.731: 155-165
Comments
Sample Throuahput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Detection: Detection limit <100 na/mL
Sample Throuahput: Retention time -1 .5 minutes
Sample Preparation: Water samples can be analyzed directly. Soil and non-aqueous liquid/oraanic solid
samples are extracted with water, filtered, and analyzed.
Other: Tested for similar compounds. Full scan usina limited QC for rapid analysis (e.a., an instrument
blank and instrument tune, but no calibration standards).
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Detection: UV wavelenath 310 nm
Sample Preparation: Filtration, requires no extraction
Other: Tested for similar compounds
Sample Preparation: SPE cartridae extraction
Other: Tested for similar compounds
Sample Preparation: Extraction with ethyl acetate and evaporation to drvness, followed by redissolvina
in acetonitrile
Other: Tested for similar compounds
Rapid Screening and Preliminary Identification Techniques and Methods
1 -21
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Disulfoton
Disulfoton sulfoxide
1,4-Dithiane
(degradation product of
HD)
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Solid
Wipes
Aqueous Liquid
Drinking Water
Technique
GC-MS
Fluorescence with or
without HPLC
GC-MS (fieldable)
GC-MS (purge and
trap)
GC-MS (fieldable)
GC-MS (purge and
trap)
Reference Source*
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Chemosphere. 2005. 61 :
1580-1586
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
EPA Methods 5030C
(water), 5035A (solid), or
3585 (non-aqueous) with
8260C (SW-846)
Field Analytical
Chemistry and
Technology. 1998. 2(1):
3-20
EPA Method 524.2 (OW)
Comments
Sample Preparation: MeCI? extraction
Other: Tested for similar compounds. Full scan usina limited QC for rapid analysis (e.a., an instrument
blank and instrument tune, but no calibration standards).
Other: Tested for similar compounds
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Detection: Detection limit 5 |jq/ka (wet weiaht) for soil/sediment: 0.5 ma/ka (wet weiaht) for wastes: 5
|jg/L for ground water, using standard quadrupole instrumentation and the purge and trap technique
Quantitation: Quantitation limit 5 |Jd/L (water): 5 |jq/ka (solid)
Workinq Ranqe: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples,
Method 5035A for solid samples, and Method 3585 for non-aqueous liquid/organic solid samples
Interferences: Volatile materials in the laboratory and impurities in the inert puraina aas and in the
sorbent trap. May require low injection port temperatures due to thermal degradation.
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Sample Preparation: Amount injected 2.6 na
Detection: Detection limit 0.06 |ja/L
Performance: Mean accuracy of 0.1 - 10 |ja/L is 95% with RSD of 5.4%
Interferences: Volatile materials in the laboratory and impurities in the inert puraina aas and in the
sorbent trap. May require low injection port temperatures due to thermal degradation.
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -22
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
EA2192
[Diisopropylaminoethyl
methylthiolophosphona
te] (hydrolysis product
ofVX)
Ethyl
methylphosphonic acid
(EMPA) (degradation
product ofVX)
Ethyldichloroarsine
(ED)
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
HPLC-ESI-MS-SIM
HPLC-MS
HPLC-ESI-MS-SIM
HPLC-MS
GC-MS
Reference Source*
Journal of
Chromatography. 1998.
794: 234-244
EPA Method TO-10A
(ORD)
Journal of
Chromatography. 1998.
794: 234-244
Method TO-IOA(ORD)
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Comments
Detection: Detection limits are two times lower than for LC-APCI-MS-SIM method
Sample Throuahput: Retention time -5.1 minutes
Sample Preparation: Water samples can be analyzed directly. Soil samples and non-aqueous
liquid/organic solid samples are extracted with water, filtered, and analyzed.
Other: Tested for similar compound (ethvlmethvl phosphonate). Limited QC for rapid analysis (an
instrument blank and instrument tune, but no calibration standards).
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Detection: Detection limits are two times lower than for LC-APCI-MS-SIM method
Sample Throuahput: Retention time -5.1 minutes
Sample Preparation: Water samples can be analyzed directly. Soil samples and non-aqueous
liquid/organic solid samples are extracted with water, filtered, and analyzed.
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Performance: Recovery for water 92 - 97%: recovery for soil 30 - 73%
Sample Preparation: Filtration, acidification, addition of 2,4-DMT and acetone extraction
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). Has been tested on a similar compound (Lewisite 3). Limited QC for rapid
analysis (possibly a blank and an instrument tune, but no standards).
Rapid Screening and Preliminary Identification Techniques and Methods
1 -23
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Ethyldichloroarsine
(ED)
N-Ethyldiethanolamine
(EDEA) (degradation
product of HN-1)
Ethylene oxide
Matrix
Aqueous Liquid
Drinking Water
Air
(particulates)
Solid
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
Spectrophotometry
Portable X-ray
fluorescence
LC-MS
HPLC-MS
GC-MS (purge and
trap)
Reference Source*
Hach Water Analysis
Handbook. 5th Edition.
2008
EPA Method 6200 (SW-
846)
Journal of
Chromatography A.
2006.1102:214-223
EPA Method TO-10A
(ORD)
EPA Methods 5030C
(water), 5035 (solid), or
3585 (non-aqueous) with
8260C (SW-846)
Comments
Detection: Detection ranae 0.02 - 0.20 ma/L. Measures total arsenic.
Interferences: Potential interferences include antimony salts
Other: Silver diethvldithio-carbamate method
Detection: Inteference-free detection limits 40 ma/ka. Measures total arsenic.
Interferences: Potential interferences include particle size, uniformity, homoaeneitv, surface condition,
high moisture content, and high concentration of other heavy metals
Sample Preparation: Soils and non-aqueous liquid/oraanic solid should first be extracted into water
Other: A liquid chromatoaraph with mixed mode column and isocratic elution aave aood
chromatography
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Detection: Detection limits 5 |ja/ka (wet weiaht) for soil/sediment samples: 0.5 ma/ka (wet weiaht) for
wastes; 5 |jg/L for ground water
Quantitation: Quantitation limit 5 |ja/L (water): 5 |ja/ka (solid)
Workinq Ranqe: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples,
Method 5035A for solid samples, and Method 3585 for non-aqueous liquid/organic solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Rapid Screening and Preliminary Identification Techniques and Methods
1 -24
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Ethylene oxide
Fenamiphos
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Technique
Draeger gas
detection tube
GC-FID
GC-MSD
GC-MS
GC-MS (fieldable)
Reference Source*
Draeger gas detection
tube Ethylene Oxide 1/a
(P/N 6728961)
httD://www.afcintl.com/Ddf
/draeaer/6728961.Ddf
(accessed November 19,
2009)
Draeger gas detection
tube Ethylene Oxide 1/a
(P/N 6728961 ); 25/a (P/N
6728241 )
httD://www.draeaer.com/
US/en US/ (accessed
November 19, 2009)
EPA Method TO-8
EPA Method TO-1 5
(ORD)
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Comments
Detection: Detection ranaes 1-15 ppm: 25 - 500 ppm
Sample Preparation: A calibrated 100-mL sample of air is drawn throuah the tube with a pump (Draeaer
accuro® or equivalent)
Other: EPA Method TO-8 modified for direct injection
Sample Preparation: Canister sample
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Sample Preparation: MeCb extraction
Other: Tested for similar compounds. Full scan usina limited QC for rapid analysis (e.a., an instrument
blank and instrument tune, but no calibration standards).
Sample Throuahput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Rapid Screening and Preliminary Identification Techniques and Methods
1 -25
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Fentanyl
Fluoride
Fluoroacetamide
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Aqueous Liquid
Drinking Water
Aqueous Liquid
Drinking Water
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
HPLC-UV
HPLC-APCI-MS-SPE
HPLC-APCI-MS-LLE
Immunoassay
Fluorescence with or
without HPLC
Spectrophotometry
Ion Selective
Electrode
GC-MS
Reference Source*
Chemosphere. 2005. 61 :
1580-1586
"A General Unknown
Screening For Drugs and
Toxic Compounds in
Human Serum." Thesis.
http://paaes.unibas.ch/di
ss/2005/DissB 7295.pdf
(accessed November 19,
2009)
Journal of
Chromatography B.
1999.731: 155-165
Journal of Analytical
Toxicology. 1990. 14(3):
160-164
Chemosphere. 2005. 61 :
1580-1586
Hach Water Analysis
Handbook. 5th Edition.
2008
EPA Method 9214 (SW-
846)
Journal of
Chromatography B.
2008.876(1): 103-108
Comments
Sample Preparation: Filtration, requires no extraction
Sample Preparation: SPE cartridae extraction
Sample Preparation: Extraction with ethvl acetate and evaporation to drvness, followed bv redissolvina
in acetonitrile
Detection: 0.25 na/mL
Other: Tested for similar analvte(s) (bromadiolone)
Detection: Detection ranae 0.02 - 2.00 ma/L
Interferences: This test is sensitive to small amounts of interference: alassware must be very clean
(acid rinse before each use)
Other: SPADNS reaaent
Detection: Detection ranae 0.025 - 500 ma/L: detection limit 0.5 ma/L
Interferences: Polyvalent cations (i.e., Fe3+ and AI3+)
Other: This method measures simple fluoride rather than total fluoride
Detection: Detection limit 0.01 |ja/mL
Quantitation: Quantitation limit 0.03 |ja/mL
Workina Ranae: 0.03 - 30 ua/mL
Sample Preparation: Acetonitrile extraction
Rapid Screening and Preliminary Identification Techniques and Methods
1 -26
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Fluoroacetic acid and
fluoroacetate salts
(analyze for
fluoroacetate ion)
2-Fluoroethanol
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Aqueous Liquid
Drinking Water
Air
Technique
GC-MS or -ECD
GC-MS
GC-FTIR
GC-FID (direct
injection)
GC-MS or -FID
GC-FID (direct
injection)
Reference Source*
Analytical Letters. 1997.
27(1 4): 2703-271 8
EPA Methods 5030C
(water), 5035A (solid), or
3585 (non-aqueous) with
8260C (SW-846)
EPA Method 8340 (SW-
846)
No Method Identified
Methods for the
Determination of
Hazardous Substances.
1997.88: 1-20
EPA Method TO-8
(ORD)
Comments
Detection: Detection ranae 0.02 - 2.00 ma/L
Sample Preparation: Solid and non-aqueous liquid/oraanic samples are extracted ultrasonicallv with
water, then partitioned with hexane and acidified prior to re-extraction with ethyl acetate. Aqueous and
drinking water samples are partitioned with hexane, and acidified prior to re-extraction with ethyl
acetate. The ethyl acetate fraction is taken to dryness in the presence of TEA, and the resulting acid is
derivatized with pentafluorobenzyl bromide.
Detection: Detection limits 5 |jq/ka (wet weiaht) for soil/sediment samples: 0.5 ma/ka (wet weiaht) for
wastes; 5 |jg/L for ground water, using standard quadrupole instrumentation and the purge and trap
technique
Quantitation: Quantitation limit 5 |Jd/L (water): 5 |jq/ka (solid)
Workinq Ranqe: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples and
Method 5035Afor solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Detection: Minimum identifiable quantity 120 na
Workinq Ranqe: Workina ranae 25 - 500 ma/L
Sample Throuqhput: Run time 15 minutes
Sample Preparation: Direct aqueous injection
Interferences: Contaminants in solvents, reaaents, alassware, and other sample processina hardware
-
Workina Ranae: 1 - 1000 ma/m3
Sample Preparation: Use Draeaer diffusive sampler or sorbent tube (i.e, Anasorb® 747 or equivalent).
Analyze sampler or sorbent tube with GC-MSD or FID (NIOSH 2513), etc.
Interferences: Hiah humidity may affect recovery
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Other: Aqueous impinaer collection
Rapid Screening and Preliminary Identification Techniques and Methods
1 -27
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference Source*
Comments
Formaldehyde
Aqueous Liquid
Drinking Water
Solid
Wipes
HPLC-UV
EPA Method 8315A (SW-
846)
Other: Limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration
standards)
Aqueous Liquid
Drinking Water
Spectrophotometry
Hach Water Analysis
Handbook. 5th Edition.
2008
Detection: Detection range 3 - 500 |jg/L
Quantitation: Results measured at 630 nm
Sample Preparation: Formaldehyde reacts with MBTH and a developing solution to form a blue color in
proportion to the formaldehyde concentration
Air
Draeger gas
detection tube
Draeger accuro® pump
kit and gas detection
tube
http://www.coleparmer.co
Detection: Detection ranges 0.2 - 5 ppm; 2-40 ppm
Quantitation: RSD ±20 - 30%
Sample Throughput: Measurement time ~1.5 minutes
Sample Preparation: A calibrated 100-mL sample of air is drawn through the tube with a pump (Draeger
m/catalog/product view.
asp?sku=8651434
(accessed November 19,
2009)
accuro® or equivalent)
Draeger gas detection
tube Formaldehyde 0.2/a
(P/N 6733081 );2/a(P/N
8101751)
http://www.draeger.com/
US/en US/(accessed
November 19, 2009)
Draeger gas detection
tube Formaldehyde 0.2/a
(P/N 6733081)
http://www.afcintl.com/pdf
/draeger/6733081.pdf
(accessed November 19,
2009)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -28
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Gasoline range
organics
Hexahydro-1 ,3,5-trinitro-
1,3,5-triazine(RDX)
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Non-aqueous
Liquid/Organic
Solid
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
GC-MS (purge and
trap)
HPTLC-AMD
Rapid HPLC
Fast GC-PDECD or
-MS
GC-MS
Rapid TLC (fieldable)
Immunoassay
Fast GC-PDECD or
-MS
GC-MS
Reference Source*
EPA Methods 5030C
(water), 5035A (solid), or
3585 (non-aqueous) with
8260C (SW-846)
Analytical Chemistry.
1994.66:2570-2577
Journal of Forensic
Science. 2005. 49(6):
1181-1186
Journal of Forensic
Science. 2006. 51: 815
Poster: "Detection of
Explosives by Fast GC -
Fast MS using an Ion
Trap"
Chemistry for the
Protection of the
Environment 4. 2003. 59:
125-135
EPA Method 4050 (SW-
846)
EPA Method 4051 (SW-
846)
Journal of Forensic
Science. 2006. 51: 815
Poster: "Detection of
Explosives by Fast GC -
Fast MS using an Ion
Trap"
Comments
Detection: Detection limits 5 |jq/ka (wet weiaht) for soil/sediment samples: 0.5 ma/ka (wet weiaht) for
wastes; 5 |jg/L for ground water, using standard quadrupole instrumentation and the purge and trap
technique
Quantitation: Quantitation limit 5 |Jd/L (water): 5 |jq/ka (solid)
Workina Ranae: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples,
Method 5035A for solid samples, and Method 3585 for non-aqueous liquid/organic solid samples
Interferences: Volatile materials in the laboratory and impurities in the inert puraina aas and in the
sorbent trap
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Sample Throuahput: Up to 20 samples can be chromatoaraphed simultaneously
Sample Throuqhput: Rapid version of this technique can separate seven explosives in <2 minutes
Other: This procedure is based on a method for soil analyses, but could be modifed to analyze water
matrices
Sample Throuahput: Nine explosives could be detected in under three minutes
Sample Preparation: No sample preparation method was investiaated: Method 8330 is recommended
for solids, and Method 3535 is recommended for liquids
Quantitation: Semi-quantitative
Detection: Detection limit >500 ppm
Other: Desianed to detect TNT
Detection: Detection limit 5 ppb
Performance: +99% of soil samples containina 1 .0 ppm will produce a positive result
Sample Throuqhput: Nine explosives detected in <3 minutes
Sample Preparation: No sample preparation method was investiaated: Method 8330 is recommended
for solids, and Method 3535 is recommended for liquids
Sample Throuahput: Nine explosives detected in <3 minutes
Sample Preparation: No sample preparation method was investiaated: Method 8330 is recommended
for solids, and Method 3535 is recommended for liquids
Rapid Screening and Preliminary Identification Techniques and Methods
1 -29
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Hexahydro-1 ,3,5-trinitro-
1,3,5-triazine(RDX)
Hexamethylenetriperoxi
dediamine (HMTD)
Hydrogen bromide
Hydrogen chloride
Matrix
Solid
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Air
Technique
Rapid TLC (fieldable)
Colorimetric
screening
DESI mass
spectrometry
HPLC
Gas detection tube
Impinger collection or
ion selective
electrode
1C
Reference Source*
Chemistry for the
Protection of the
Environment 4. 2003. 59:
125-135
Journal of Forensic
Science. 2005. 49(6):
1181-1186
EPA Method 8515 (SW-
846)
EPA Method 8510 (SW-
846)
Chemistry
Communications. 2006.
93: 953-955
Analytical Chemistry.
2003. 75(4): 731-735
OSHA Method I D-165SG
EPA Method TO-8
(ORD); EPA Method
9211 (SW-846)
OSHA Method I D-174SG
Comments
Quantitation: Semi-quantitative
Quantitation: Semi-quantitative
Sample Throuahput: A rapid version of this technique can separate seven explosives in <2 minutes
Other: Procedure is based on a method for soil analyses, but could be modifed to analyze water
matrices.
Detection: Detection of TNT at concentrations >1 ppm. 95% of samples containina 0.7 ppm of TNT or
less will produce a negative result.
Workina Ranae: 1 - 30 com (TNT)
Sample Preparation: Sample is treated with color-chanae reaaents and read in spectrophotometer
Performance: Averaae recovery for 5 ppm spike (n=22) 5.1 (±0.4) ppm with 7.8% RSD
Detection: Detection of TNT at concentrations >1 ppm. 95% of samples containina 0.7 ppm of TNT or
less will produce a negative result.
Workina Ranae: 1 - 30 ppm (TNT)
Other: Tested for similar compound (TATP). DESI mass spectrometrv is used for detection of trace
amounts of TATP by alkali metal complexation.
Detection: Limit of detection 5 |jmol/L
Sample Throughput: Allows field testina with readily available and portable instrumentation
Sample Preparation: Substances and interferences are separated on a C-1 8 column, the analvtes are
subsequently decomposed to hydrogen peroxide by UV irradiation, and detected fluorometrically based
on HRP-catalyzed oxidative coupling of phenols by hydrogen peroxide
Other: Detects TATP and HMTD: post-column photochemical treatment and fluorescence detection
Detection: Detection limit 0.20 |ja (based on a sample volume of 10 mL and an injection volume of 100
ML)
Workina Ranae: 0.2 - 50 ua/mL
Performance: The averaae coefficient of variation is 0.035
Sample Preparation: A known volume of air is drawn throuah a silica ael tube. H^SO^ H,PO4 and other
particulates are collected on the glass fiber plug while HBr and HNO3 are collected on the silica gel
sorbant.
Detection: Detection ranae 0.1 - 1000 ma/L: detection limit 0.2 ma/L
Sample Throuahput: This procedure may be more cumbersome than silica ael collection
Interferences: Polyvalent cations (i.e., Fe3+ and AI3+)
Other: Method 921 1 for the analysis of simple bromide ion rather than total bromide
Sample Preparation: Collect air sample on silica ael tubes
Rapid Screening and Preliminary Identification Techniques and Methods
1 -30
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference Source* Comments
Hydrogen chloride
Air
Draeger gas
detection tube
Draeger gas detection
tube Hydrochloric Acid
1/a(P/NCH29501)
http://www.afcintl.com/pdf
Detection: Detection ranges 1 - 10 ppm; 50 - 5,000 ppm
Sample Preparation: A calibrated 100-mL sample of air is drawn through the tube with a pump (Draeger
accuro® or equivalent)
/draegei7CH29501.pdf
(accessed November 19,
2009)
Draeger gas detection
tube Hydrochloric Acid
1/a(P/NCH29501);50/a
(P/N 6728181)
http://www.draeger.com/
US/en US/(accessed
November 19, 2009)
Impinger collection or
ion selective
electrode
EPA Method TO-8
(ORD); EPA Method
9212(SW-846)
Detection: Detection range 0.4 - 1000 mg/L; detection limit 2.0 mg/L
Interferences: Polyvalent cations (Fe3+and AI3+)
Sample Throughput: This procedure may be more cumbersome than silica gel collection
Other: Method is for the analysis of simple chloride rather than total chloride
Hydrogen cyanide
Air
Toxic gas detector
General Monitors toxic
gas detectors
http://www.generalmonito
Detection: Detection range 0-20 ppm
rs.com/products/toxic ga
sdetectors.html
(accessed November 19,
2009)
Agueous Liguid
Drinking Water
Spectrophotometry
(fieldable)
Hach Water Analysis
Handbook. 5th Edition.
2008
Detection: Detection range 0.001 - 0.240 mg/L
Interferences: Interferences include high levels of Cl, Ni, Co >1 mg/L, Cu >20 mg/L, Fe >5 mg/L, or
oxidizing agents. Remove metals by adding chelating reagents and remove oxidizing agents with
appropriate reagents.
Other: Pyridine-pyrazalone spectrophotometer
Hydrogen fluoride
Air
Draeger/Nextteg
Gastec® gas
detection tube
(fieldable)
Nextteg Gastec®
Hydrogen Fluoride (P/N
19026210)
https://www1 .fishersci.co
Detection: Detection ranges 0.25 - 100 ppm; 0.5- 90 ppm
Working Range: Working range 0.25 - 100 ppm
m/Coupon:isessionid=Eo
YtTAmK7vdGN1Nic1v90
9NFOwtwNAeoJtfcJFfuD
1Khfn5XdteN!-
43026010?cid=1342&gid
=2444789&details=Y
(accessed November 19,
2009)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -31
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Hydrogen fluoride
Hydrogen sulfide
Matrix
Air
Air
Technique
Draeger/Nextteq
Gastec® gas
detection tube
(fieldable)
Impinger collection
GC-FIDor-ECD
Nextteq Gastec® gas
detection tube
(fieldable)
Draeger gas
detection tube
UV-luminescence
detector
Reference Source*
Draeger gas detection
tube Hydrogen Fluoride
0.5/a(P/N 81 03251)
httD://www.draeaer.com/
US/en US/ (accessed
November 19, 2009)
EPA Method TO-8
(ORD); EPA Method
9214(SW-846)
EPA field screening
Method FM9
Nextteq Gastec® gas
detection tube Hydrogen
Sulfide (P/Ns
19026294,19026293,
19026291,19026286)
httcs://www1 .fishersci.co
m/CouDon:isessionid=Eo
YtTAmK7vdGN1Nidv90
9NFOwtwNAeoJtfcJFfuD
1Khfn5XdteN!-
1 34302601 0?cid=1342&
did=2444789&details=Y
(accessed November 19,
2009)
Draeger gas detection
tube Hydrogen Sulfide
0.2/a(P/N8101461);
0.2/b(P/N8101991);
0.5/a(P/N 6728041); 1/d
(P/N8101831);2/a(P/N
6728821 );2/b(P/N
8101961);5/b(P/N
CH29801)
httD://www.draeaer.com/
US/en US/ (accessed
November 19, 2009)
Environmental
technology verification
report Horiba
Instruments APSA-360
Ambient Hydrogen
Sulfide Analyzer
httD://www.eca.aov/etv/D
ubs/01 vr acsa360.Ddf
(accessed November 19,
2009)
Comments
Detection: Detection ranaes 0.25- 100 ppm: 0.5-90 ppm
Workinq Ranqe: Workina ranae 0.25 - 100 ppm
Detection: Detection ranae 0.025 - 500 ma/L: detection limit 0.5 ma/L
Samcle Throuahput: This procedure may be more cumbersome than silica del collection
Interferences: Polyvalent cations (i.e., Fe3+ and AI3+)
Other: This method measures simple fluoride rather than total fluoride
Other: Used to screen water, air, soil, and sediment samples on a GC with a PID, FID, or ECD. Air
screened directly by collecting sample and injecting into GC for analysis.
Detection: Detection ranaes from 0.1 - 4 ppm to 10 - 4000 ppm
Detection: Detection ranaes from 0.1 - 4 ppm to 10 - 4000 ppm
Detection: Detection ranae 4 - 300 ppb
Quantitation: Recovery 131%
Interferences: Interferences include carbanvl sulfide, dimethyl sufide, and methyl mercaptan
Rapid Screening and Preliminary Identification Techniques and Methods
1 -32
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Hydrogen sulfide
Isopropyl
methylphosphonic acid
(IMPA) (degradation
product of GB)
Kerosene
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
Toxic Gas Leak
detector (fieldable)
Portable H2S
Analyzer (fieldable)
GC-FIDor-ECD
LC-ESI-MS-SIM
LC-APCI-MS-SIM
HPLC-MS
GC-MS
Reference Source*
CEA HS-2200 Toxic Gas
Leak Detector
httD://www.ceainstr.com/
cdf datasheets/seriesu I
nfo.pdf (accessed
November 19, 2009)
Arizona Instruments
Jerome® 631 -X Portable
Handheld H2S Analyzer
http://www.trs-
environmental.com/Mode
I/AZI X631 H2S ANALY
ZER.aspx (accessed
November 19, 2009)
EPA Method TO-1 5
Journal of
Chromatography. 1998.
794: 234-244
Journal of
Chromatography A.
1999.862(2): 169-177
Method TO-1 OA(ORD)
EPA Method 801 5C (SW-
846)
Comments
Detection: Detection ranaes 0-50 ppm: 0-100 ppm: 0-500 ppm: 0- 1000 ppm
Detection: Detection ranae 0.003 - 50 ppm
Other: Modified to include Tedlar® bags with limited QC to ensure rapid sample screening
Detection: Detection limits are two times lower than for LC-APCI-MS-SIM
Sample Throughput: Retention time ~10.9 minutes
Sample Preparation: Water samples can be analyzed directly. Soil samples and non-aqueous
liquid/organic solid are extracted with water, filtered, and analyzed.
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Detection: Detection limits <10 na/mL
Sample Throuahput: Retention time -3.9 minutes
Sample Preparation: Water samples can be analyzed directly. Soil and non-aqueous liquid/oraanic solid
samples are extracted with water, filtered, and analyzed.
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Sample Preparation: MeCb extraction
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -33
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Lead arsenate (analyze
as total arsenic)
Lewisite 1 (L-1) [2-
chlorovinyldichloroarsi
ne] (analyze for total
arsenic)
Matrix
Air
(particulates)
Solid
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Air
(particulates)
Solid
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Air
Technique
X-ray fluorescence
analyzer (fieldable)
Spectrophotometry
ICP-MS
ICP-AES
Portable X-ray
fluorescence
GC-MS
Spectrophotometry
Surface acoustic
wavelength detector
(fieldable)
Draeger gas
detection tube
(fieldable)
Reference Source*
EPA Method 6200 (SW-
846)
Hach Water Analysis
Handbook. 5th Edition.
2008
EPA Method 6020A (SW-
846);
EPA Method 200.8 (OW)
EPA Method 601 OC (SW-
846);
EPA Method 200.7 (OW)
EPA Method 6200 (SW-
846)
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Hach Water Analysis
Handbook. 5th Edition.
2008
Sensors and Actuators
B. 2005. 108: 193-197
Sensors and Actuators
B. 2005. 108: 193-197
Comments
Detection: Interference-free detection limit 40 ma/ka (arsenic)
Quantitation: Semi-quantitative
Interferences: Potential interferences include particle size, uniformity, homoaeneitv, surface condition,
high moisture content, and high concentration of other heavy metals
Detection: Detection ranae 0.02 - 0.20 ma/L (arsenic)
Interferences: Potential interferences include antimony salts
Other: Measures total arsenic. Silver diethyldithio-carbamate method.
Detection: In cases where low concentrations of compounds are beina addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES
Sample Preparation: Extraction in aqueous nitric acid
Other: Limited QC for rapid analysis
Detection: In cases where low concentrations of compounds are beina addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES
Sample Preparation: Extraction in aqueous nitric acid
Other: Limited QC for rapid analysis
Detection: Inteference-free detection limit 40 ma/ka (measures total arsenic)
Interferences: Potential interferences include particle size, uniformity, homoaeneitv, surface condition,
high moisture content, and high concentration of other heavy metals
Performance: May have limited application for detection of Lewisite 1 . Recovery for water 92 - 97%: for
soil 30 - 73%.
Sample Preparation: Filtration, acidification, addition of 2,4-DMT and acetone extraction
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). Has been tested on a similar compound (Lewisite 3).
Detection: Detection ranae 0.02 - 0.20 ma/L. Measures total arsenic.
Interferences: Potential interferences include antimony salts
Other: Silver diethyldithio-carbamate method
Detection: Detection limit 40 ma/m3 (cannot distinauish between mustard and Lewisite)
Quantitation: Gives semi-qualitative information
Other: JCAD surface acoustic wavelenath detector
Detection: Detection in the sub-ma/m3 ranae
Sample Throuahput: Takes several minutes for tube coloration to occur. Could lead to false positives.
Other: Gives semi-qualitative information (i.e., can identify class of compound: phosphoric esters,
organo-arsenic, thioether, cyanogen chloride, and cyanide)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -34
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Lewisite 1 (L-1) [2-
chlorovinyldichloroarsi
ne] (analyze for total
arsenic)
Lewisite 2 (L-2) [bis(2-
chlorovinyl)-
chloroarsine] (analyze
for total arsenic)
Matrix
Aqueous Liquid
Drinking Water
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
(particulates)
Solid
Wipes
Air
Technique
Portable GC-MS
(fieldable)
Spectrophotometry
(fieldable)
GC-MS
X-ray fluorescence
(fieldable)
Draeger gas
detection tube
(fieldable)
Portable GC-MS
(fieldable)
Reference Source*
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Hach Water Analysis
Handbook. 5th Edition.
2008
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
EPA Method 6200 (SW-
846)
Sensors and Actuators
B. 2005. 108: 193-197
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Comments
Sample Throuahput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Detection: Detection ranae 0.02 - 0.20 ma/L
Interferences: Potential interferences include antimony salts: measures total arsenic
Other: Silver diethvldithio-carbamate method. Hach DR/4000 and 2500 photometer.
Sample Preparation: Filtration, acification, addition of 2,4-DMT and acetone extraction
Other: Tested for similar compound (Lewisite 1)
Detection: May have limited application for detection of Lewisite 2
Sample Preparation: MeCI? extraction
Other: Has been tested on a similar compound (Lewisite 3). Full scan usina limited QC for rapid
analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Detection: Interference-free detection limit 40 ma/ka (measures total arsenic)
Interferences: Potential interferences include particle size, uniformity, homoaeneitv, surface condition,
high moisture content, and high concentrations of other heavy metals
Detection: Detection in the sub-ma/m3 ranae
Sample Throuqhput: Takes several minutes for tube coloration to occur. Could lead to false positives.
Other: Gives semi-qualitative information (i.e., can identify class of compound: phosphoric esters,
organo-arsenic, thioether, cyanogen chloride, and cyanide)
Sample Throuahput: Analysis time -16 minutes: total sample throuahput -3 samples/hour. Retention
time for GB -6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Rapid Screening and Preliminary Identification Techniques and Methods
1 -35
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Lewisite 3 (L-3) [tris(2-
chlorovinylj-arsine]
(analyze for total
arsenic)
Lewisite oxide
(degradation product of
Lewisite)
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
(particulates)
Solid
Wipes
Aqueous Liquid
Drinking Water
Air
Air
(particulates)
Solid
Aqueous Liquid
Drinking Water
Technique
GC-MS
Portable X-ray
fluorescence
(fieldable)
Spectrophotometry
Portable GC-MS
(fieldable)
Portable X-ray
fluorescence
(fieldable)
GC-MS
Spectrophotometry
GC-MS
Reference Source*
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
EPA Method 6200 (SW-
846)
Hach Water Analysis
Handbook. 5th Edition.
2008
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
EPA Method 6200 (SW-
846)
Toxicology Methods.
1999.9:275-294
Hach Water Analysis
Handbook. 5th Edition.
2008
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Comments
Performance: Recoveries in water ranaed from 54 - 55%: soil recoveries ranaed from 30 - 78%
Sample Preparation: MeCI? extraction
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). Has been tested on a similar compound (Lewisite 3).
Detection: Interference-free detection limit 40 ma/ka. Measures total arsenic.
Interferences: Potential interferences include particle size, uniformity, homoaeneitv, surface condition,
high moisture content, and high concentration of other heavy metals
Detection: Detection ranae 0.02 - 0.20 ma/L. Measures total arsenic.
Interferences: Potential interferences include antimony salts
Other: Silver diethvldithio-carbamate method
Sample Throuqhput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Detection: Interference-free detection limit 40 ma/ka. Measures total arsenic.
Interferences: Potential interferences include particle size, uniformity, homoaeneitv, surface condition,
high moisture content, and high concentration of other heavy metals
Sample Preparation: Aqueous sample is extracted on C1 8 column, eluted with methanol, dried, and
derivatized with EOT. If chromatographic separation is not required then EOT can be omitted.
Detection: Detection ranae 0.02 - 0.20 ma/L
Interferences: Potential interferences include antimony salts: measures total arsenic
Other: Silver diethvldithio-carbamate method
Performance: Recovery ranae for water 92 - 94%: for soil 35 - 71 %
Sample Preparation: Filtration, acidification, addition of 2,4-DMT and acetone extraction
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -36
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Lewisite oxide
(degradation product of
Lewisite)
Mercuric chloride
(analyze for total
mercury)
Matrix
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Solid
Wipes
Aqueous Liquid
Drinking Water
Air
Technique
GC-MS
GC-MS-SPME
Draeger gas
detection tube
Spectrophotometry
Nextteq Gastec® gas
detection tube
(fieldable)
Reference Source*
Toxicology Methods.
1999.9:275-294
Journal of
Chromatography A.
2001.909: 13-28
Sensors and Actuators
B. 2005. 108: 193-197
EPA Method 7473 (SW-
846)
Mercury Tracker 3000 IP
Portable Mercury Vapor
Detector
http://www.mercurv-
instrumentsusa.com/Trac
kerlP.htm (accessed
November 19, 2009)
Hach Water Analysis
Handbook. 5th Edition.
2008
Nextteq Gastec® gas
detection tube Mercury
Vapor (P/N 19026282)
https://www1 .fishersci.co
m/CouDon:isessionid=Eo
YtTAmK7vdGN1Nidv90
9NFOwtwNAeoJtfcJFfuD
1Khfn5XdteN!-
1 34302601 0?cid=1342&
did=2444789&details=Y
(accessed November 19,
2009)
Comments
Sample Preparation: MeCI? extraction. Derivatize with EOT. If chromatoaraphic separation is not
required, then EOT can be omitted.
Sample Throuqhput: Total sample processina time ~5 minutes
Sample Preparation: Samples are extracted (usina ascorbic acid in water with propanedithiol),
centrifuged, and filtered. Analytes are concentrated from supernatant onto SPME fiber and analyzed by
GC-MS.
Detection: Detection is in the sub-ma/m3 ranae
Sample Throuahput: Takes several minutes for tube coloration to occur. Could also lead to false
positives.
Other: Gives semi-qualitive information (i.e., can identify class of compound: phosphoric esters, oraano-
arsenic, thioether, cyanogen chloride, and cyanide)
Detection: Detection limit 0.01 na (total mercury)
Workina Ranae: Workina ranae 0.05 - 600 na
Sample Throuahput: Analysis time <5 minutes
Interferences: Inteferfences include memory effects from hiah concentration samples
Other: Thermal decomposition, desorption, and atomic absorption
Detection: Detection limit 0.1 |ja/m3: detection ranae 0.1 -2000 |ja/m3
Detection: Detection ranae 0.1 -2.5 |ja/L
Sample Throuahput: >2 hours
Interferences: No known interferences
Other: Cold vapor method
Detection: Detection ranae 0.05 - 13.2 ma/m3
Rapid Screening and Preliminary Identification Techniques and Methods
1 -37
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Mercury, Total
Matrix
Aqueous Liquid
Drinking Water
Solid
Wipes
Air
Technique
Spectrophotometry
Nextteq Gastec® gas
detection tube
(fieldable)
Draeger gas
detection tube
(fieldable)
Spectrophotometry
EPA M30B Carbon
Trap
Lumex Mercury
Analyzers
Reference Source*
Hach Water Analysis
Handbook. 5th Edition.
2008
EPA Method 7473 (SW-
846)
Nextteq Gastec® gas
detection tube Mercury
Vapor (P/N 19026282)
httDs://www1 .fishersci.co
m/CouDon:isessionid=Eo
YtTAmK7vdGN1Nidv90
9NFOwtwNAeoJtfcJFfuD
1Khfn5XdteN!-
1 34302601 0?cid=1342&
did=2444789&details=Y
(accessed November 19,
2009)
Draeger gas detection
tube Mercury Vapor 0.1 /b
(P/NCH23101)
httD://www.draeaer.com/
US/en US/ (accessed
November 19, 2009)
Mercury Tracker 3000 IP
Portable Mercury Vapor
Detector
httD://www.mercurv-
instrumentsusa.com/Trac
kerlP.htm (accessed
November 19, 2009)
EPA Method SOB
(OAQPS)
Lumex Mercury
Analyzers (including
direct read gas only
model)
httD://www.ohiolumex.co
m (accessed November
19,2009)
Comments
Detection: Detection ranae 0.1 -2.5 |ja/L
Sample Throuqhput: >2 hours
Interferences: No known interferences
Other: Cold vapor method
Detection: Instrument detection limit 0.01 na (total mercury)
Workina Ranqe: Workina ranae 0.05 - 600 na
Sample Throuqhput: Analysis time <5 minutes
Interferences: Memory effects from hiah concentration samples
Other: Thermal desorption
Detection: Detection ranae 0.05 - 13.2 ma/m3
Detection: Detection ranae 0.05 - 2 ma/m3
Detection: Detection limit 0.1 |ja/m3: detection ranae 0.1 - 2000 |ja/m3
Detection: Detection ranae 0.1 |ja/dscm to >50 |ja/dscm
Detection: Detection limit 2 na/m3
Workina Ranae: 0.00001 -0.1 ma/m3
Rapid Screening and Preliminary Identification Techniques and Methods
1 -38
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Mercury, Total
Methamidophos
Methomyl
Matrix
Air
Air
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Technique
Jerome® Mercury
Vapor Analyzer
HPLC
Immunoassay
(fieldable)
HPLC-ESI-MS-SIM
HPLC
HPLC-UV
Reference Source*
Arizona Instruments
Jerome® 41 1 Mercury
Vapor Analyzer
httD://www.azic.com/Ddf/
manual SS-101.pdf
(accessed November 19,
2009)
Journal of
Chromatography A.
2007. 11 54(1): 3-25
Chromatographia. 2006.
63(5/6): 233-237
RaPID Assay® Methomyl
(built to order)
http://www.sdix.com
(accessed November 19,
2009)
Analytica Chimica Acta.
2004.505:209-215
Journal of
Chromatography A.
1996.726:99-113
NIOSH Method 5601
Comments
Detection: Detection Ranae 0.000 - 1 .999 ma/m3
Performance: ±5% at 0.107 ma/m3 Ha
Quantitation: 0.01 ma/ka (limit of quantification)
Workina Ranae: 0.01 - 1 .0 ma/ka
Performance: Mean recovery ranae 70 - 1 10 (±15)%
Sample Throuqhput: Retention time 4.70 minutes
Detection: Detection limit 30 |ja/L
Performance: Recovery ranae 95.3 - 1 18.4 %
Sample Throuahput: Retention time 4.39 minutes
Detection: Detection level 0.45ppb (as methomvl)
Quantitation: Quantitation between 1.0- 15.0 ppb
Other: Used as a quantitative, semi-quantitative, or qualitative enzyme immunoassav for the analysis of
methomyl in water
Sample Preparation: SPE, soil samples, and non-aqueous liquid samples require extraction into water
Detection: Detection limit 0.5 |ja/L
Performance: Recovery 19%
Sample Throuqhput: Retention time ~12.8 minutes
Sample Preparation: Soil samples and non-aqueous liquid samples require extraction into water
Other: Diode array with online sample enrichment
Detection: Detection limit 0.05 ua/L
Workinq Ranqe: 1-10 |ja/L
Sample Preparation: Collect air samples on sorbents. Extraction with 0.2% v/v 0.1 M aqueous
triethylamine phosphate buffer in acetonitrile (pH 6.9 - 7.1) from filter/solid sorbent tube (OVS-2 Tube:
13-mm quartz fiber filter; XAD-2, 270 mg/140 mg)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -39
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Methoxyethylmercuric
acetate (analyze for
total mercury)
Methyl acrylonitrile
Matrix
Aqueous Liquid
Drinking Water
Solid
Wipes
Aqueous Liquid
Drinking Water
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Technique
Spectrophotometry
Nextteq Gastec® gas
detection tube
(fieldable)
HPLC
Reference Source*
EPA Method 7473 (SW-
846)
Mercury Tracker 3000 IP
Portable Mercury Vapor
Detector
httD://www.mercurv-
instrumentsusa.com/Trac
kerlP.htm (accessed
November 19, 2009)
Hach Water Analysis
Handbook. 5th Edition.
2008
Nextteq Gastec® gas
detection tube Mercury
Vapor (P/N 19026282)
httcs://www1 .fishersci.co
m/CouDon:isessionid=Eo
YtTAmK7vdGN1Nidv90
9NFOwtwNAeoJtfcJFfuD
1Khfn5XdteN!-
1 34302601 0?cid=1342&
did=2444789&details=Y
(accessed November 19,
2009)
EPA Method 8316 (SW-
846)
OSHA Method PV2004
Comments
Detection: Detection limit 0.01 na (total mercury)
Workinq Ranqe: Workina ranae 0.05 - 600 na
Sample Throuqhput: Analysis time <5 minutes
Interferences: Inteferfences include memory effects from hiah concentration samples
Other: Thermal decomposition, desorption, and atomic absorption
Detection: Detection limit 0.1 |Jd/m3: detection ranae 0.1 -2000 |ja/m3
Detection: Detection ranae 0.1 -2.5 |ja/L
Sample Throuqhput: Method takes >2 hours
Interferences: No known interferences
Other: Cold vapor method
Detection: Detection ranae 0.05 - 13.2 ma/m3
Detection: Detection limit 10 |ja/L (acrvlamide) and 20 |ja/L (acrvlonitrile)
Detection: Detection limit 0.7 |ja/mL (0.006 ma/m3 for a 1-mL desorption volume or 0.029 ma/m3 for a 5-
m L desorption volume based on a 1 20-L air volume)
Workina Ranae: 0.017-1.5 ma/m3 (1-mL desorption volume) and 0.083 - 7.5 ma/m3 (5-m L desorption
volume1)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -40
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Methyl fluoroacetate
(analyze for
fluoroacetate ion)
Methyl hydrazine
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
GC-MS (purge and
trap)
GC-MS or -ECD
GC-MSD
GC-MS (purge and
trap)
Reference Source*
EPA Methods 5030C
(water), 5035A (solid), or
3585 (non-aqueous) with
8260C (SW-846)
Analytical Letters. 1997.
27(1 4): 2703-271 8
Modified EPA Method
TO-10AorTO-17(ORD)
EPA Method 5030C
(water), 5035A (solid), or
3585 (non-aqueous) with
8260C (SW-846)
Comments
Detection: Detection limits 5 |jq/ka (wet weiaht) for soil/sediment samples: 0.5 ma/ka (wet weiaht) for
wastes; 5 |jg/L for ground water, using standard quadrupole instrumentation and the purge and trap
technique
Quantitation: Quantitation limits 5 |Jd/L (water): 5 |jq/ka (solid)
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples,
Method 5035A for solid samples, and Method 3585 for non-aqueous liquid/organic solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Detection: Detection ranae 0.02 - 2.00 ma/L
Sample Preparation: Solid and non-aqueous liquid/oraanic samples are extracted ultrasonicallv with
water, then partitioned with hexane and acidified prior to re-extraction with ethyl acetate. Aqueous and
drinking water samples are partitioned with hexane, and acidified prior to re-extraction with ethyl
acetate. The ethyl acetate fraction is taken to dryness in the presence of TEA, and the resulting acid is
derivatized with pentafluorobenzyl bromide.
Sample Preparation: Thermal desorption or extraction from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Detection: Detection limits 5 |ja/ka (wet weiaht) for soil/sediment samples: 0.5 ma/ka (wet weiaht) for
wastes; 5 |jg/L for ground water, using standard quadrupole instrumentation and the purge and trap
technique
Quantitation: Quantitation limit 5 |ja/L (water): 5 |ja/ka (solid)
Workina Ranae: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples,
Method 5035A for solid samples, and Method 3585 for non-aqueous liquid/organic solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Rapid Screening and Preliminary Identification Techniques and Methods
1 -41
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Methyl hydrazine
Methyl isocyanate
Methyl paraoxon
Methyl parathion
Methylamine
Matrix
Aqueous Liquid
Drinking Water
Solid
Wipes
Air
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Air
Air
Technique
GC-MS
GC-MS (purge and
trap)
HPLC fluorescence
orUV
GC-MS
GC-MS-SPME
GC-MS
Passive Sampler for
Amines
DraegerSensor®
Reference Source*
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
EPA Method TO-1 5
(ORD)
OSHA Method 54
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Journal of
Chromatography A.
2002.963: 107-116
EPA Method TO-1 OA
(ORD)
UMEX 400 Passive
Sampler for Amines
http://www.skcinc.com/pr
od/500-400.asc
(accessed November 19,
2009)
DraegerSensor® XS
Amine
httD://www.afcintl.com/Ddf
/draeaer/6809545.cdf
(accessed November 19,
2009)
Comments
Sample Preparation: Shake and shoot solvent extraction
Other: Tested on similar compounds. Full scan usina limited QC for rapid analysis (e.a., an instrument
blank and instrument tune, but no calibration standards).
Sample Preparation: Analyze from canisters usina Method TO-1 5 and limited QC for rapid analysis
Detection: Detection limit 0.072 |ja/sample
Sample Throuqhput: Retention time -8-12 minutes
Sample Preparation: Sorbent tube collection
Sample Preparation: MeCI? extraction
Other: Tested on similar compounds. Full scan usina limited QC for rapid analysis (e.a., an instrument
blank and instrument tune, but no calibration standards).
Detection: Detection limit 0.09 |ja/L (methyl parathion)
Sample Throuqhput: Retention time ~31 .26 minutes (methyl parathion)
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Detection: Detection ranae 0.5 - 10 ppm
Performance: Recovery ±30%
Other: Detection at 254 nm. Does distinauish between different amines.
Detection: Detection limit 50 ppm
Other: Does not distinauish between different amines
Rapid Screening and Preliminary Identification Techniques and Methods
1 -42
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Methylamine
N-
Methyldiethanolamine
(MDEA) (degradation
product of HN-2)
1 -Methylethyl ester
ethyl-
phosphonofluoridic
acid (GE)
Methyl phosphonic acid
(MPA) (degradation
product of VX, GB, &
GD)
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
Gas detection tube
LC-MS
HPLC-MS
HPLC-ESI-MS-SIM
HPLC-MS
HPLC-ESI-MS-SIM
Reference Source*
Kitagawa Gas Detector
Tube System
httD://www.itraders.biz/ko
mvo/index.html
(accessed November 19,
2009)
Journal of
Chromatography A.
2006. 1102:214-223
EPA Method TO-10A
(ORD)
Journal of
Chromatography. 1998.
794: 234-244
EPA Method TO-10A
(ORD)
Journal of
Chromatography. 1998.
794: 234-244
Comments
Detection: Detection limit 50 ppm
Interferences: Interferences include PH,, H?S, NO, H?, methanol, CO?, Ck and NO?
Other: Does not distinauish between different amines
Sample Preparation: Soils and non-aqueous liquid/oraanic solid should first be extracted into water
Other: Qualitative screenina procedure developed usina LC-MS and eliminatina the need for additional
sample handling and derivatization typically required for GC-MS analysis. An LC with a mixed mode
column and isocratic elution gave good Chromatography.
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Detection: Detection limits are two times lower than for LC-APCI-MS-SIM
Sample Throuahput: Retention time ~5.1 minutes
Sample Preparation: Water samples can be analyzed directly. Soil samples and non-aqueous liquid
samples are extracted with water, filtered, and analyzed.
Other: Limited QC for rapid analysis (an instrument blank and instrument tune, but no calibration
standards)
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Detection: Detection limits are two times lower than for LC-APCI-MS-SIM
Sample Throuqhput: Retention time -5.1 minutes
Sample Preparation: Water samples can be analyzed directly. Soil samples and non-aqueous
liquid/organic solid samples are extracted with water, filtered, and analyzed.
Other: Limited QC for rapid analysis (an instrument blank and instrument tune, but no calibration
standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -43
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Methyl phosphonic acid
(MPA) (degradation
product of VX, GB, &
GD)
Mevinphos
Monocrotophos
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Technique
HPLC-MS
GC-MS
SPME sampling
portable GC-MS
(fieldable)
GC-MS (purge and
trap)
Automated thermal
desorption GC-MS
Reference Source*
EPA Method TO-10A
(ORD)
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
EPA Method 5030C
(water) or 5035A (solid)
with 8260C (SW-846)
Journal of
Chromatography A.
2001.925:241-249
Comments
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (an instrument blank and instrument tune, but no calibration
standards)
Sample Preparation: MeCb extraction
Other: Tested on similar compounds. Full scan usina limited QC for rapid analysis (e.a., an instrument
blank and instrument tune, but no calibration standards).
Sample Throuahput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Workina Ranae: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples and
Method 5035Afor solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Tested for similar compounds.
Quantitation: Semi-quantitative
Performance: RSD at 50 na/tube for GB 21%: GD1 17%: GD2 13%: GA8%: GF 11%: VX30%: HN1
22%; HN228%; HNS 17%
Sample Throuahput: Samples can be analyzed only once
Sample Preparation: Automated thermal desorption. Tube is connected to heated GC injector (100°C).
Other: Temperature and time of storaae were found to influence recovery of analvtes, with best
recoveries being observed after one day of storage in a freezer (-12°C)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -44
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Mustard, nitrogen (HN-
1) [bis(2-chloroethyl)
ethylamine]
Mustard, nitrogen (HN-
2) [2,2'-dichloro-N-
methyldiethylamineN,N-
bis(2-chloroethyl)
methylamine]
Mustard, nitrogen (HN-
3) [tris(2-chloroethyl)
amine]
Mustard, sulfur/
Mustard gas (HD)
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Aqueous Liquid
Drinking Water
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
GC-MS
HPLC-ESI-MS
Photoionization mass
spectrometry
GC-MS
GC-NPD
Portable GC-MS
(fieldable)
GC-MS
Reference Source*
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Journal of
Chromatography A.
2006. 1102:214-223
Analytical Chemistry.
2006. 78: 2967-2976
Journal of
Chromatography A.
2006. 1102:214-223
Journal of
Chromatography A.
1999.849:529-540
Field Analytical
Chemistry and
Technology. 1998. 2(1):
3-20
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Comments
Performance: Recovery ranae in water 2 - 4%: in soil 28 - 60%
Sample Preparation: MeCI? extraction
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Other: Qualitative screenina procedure developed usina LC-MS and eliminatina the need for additional
sample handling and derivatization typically required for GC-MS analysis. An LC with a mixed mode
column and isocratic elution gave good Chromatography.
Detection: Method detection ranae 0.07 - 0.7 ma/L
Performance: RSDs <10%
Sample Throuahput: Sample cycle time 45 seconds
Sample Preparation: Direct samplina in water
Other: Tested for similar compounds
Detection: Detection limit 50 na/tube (full scan). S:N ratio at 50 na/tube was >4:1 .
Quantitation: Semi-quantitative
Performance: RSD at 50 na/tube for GB 21%: GD1 17%: GD2 13%: GA8%: GF 11%: VX30%: HN1
22%; HN228%; HNS 17%
Sample Throuqhput: Samples can be analyzed only once
Sample Preparation: Automated thermal desorption. Tube is connected to heated GC injector (100°C).
Other: Temperature and time of storaae were found to influence recovery of analvtes, with best
recoveries being observed after one day of storage in a freezer (-12 C)
Sample Preparation: GC-NPD confiaured for thermal desorption of a DAAMS tube
Other: Tested for HN1 and HNS
Other: S:N for 0.7 na iniection (neat) 8.5
Performance: Recovery in water 50%: in soil 72 - 98%
Sample Preparation: MeCI? extraction
Other: Tested for similar compounds. Full scan usina limited QC for rapid analysis (e.a., an instrument
blank and instrument tune, but no calibration standards).
Rapid Screening and Preliminary Identification Techniques and Methods
1 -45
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference Source*
Comments
Mustard, sulfur/
Mustard gas (HD)
Aqueous Liquid
Solid
Wipes
GC-MS-EI
EPA Methods 357173572
with 8271 (SW-846)
Performance: For direct injection soil recovery range (and RSD) for GB 99.6 - 145 (±12.3)%; HD 103 -
112 (±19)%); VX 61 - 110 (±6.9)%. For DAAMS soil recovery range (and RSD) for GB 78 - 95 (±7.2)%;
HD 84 - 94 (±5.4)%; VX 71 - 85 (±6.9)%. For direct injection water recovery range (and RSD) for GB
103 - 135 (±5.7)%; HD 95 - 151 (±6)%; VX 95 - 151 (±17)%.
Sample Preparation: Uses a solid sorbent (Chromosorb® 106 [GB]; Chromosorb® 106/AgF [VX] or
Tenax® TA [HD]) for extract or standard concentration followed by thermal desorption into the analytical
system
Other: Limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration
standards)
GC-FPD
EPA Methods 357173572
with 8170 (SW-846)
Performance: For direct injection soil recovery range (and RSD) for GB 88-104 (±5.7)%; HD 94-104
(±3.9)%); VX 92 - 114 (±8.2)%. For DAAMS soil recovery range (and RSD) for GB 96-128 (±9)%; HD
124-139 (±7)%; VX 85-107 (±8)%. For direct injection water recovery range (and RSD) for GB 77 -
90 (±5.7)%; HD 77 - 90 (±6)%; VX 87-103 (±5.7)%.
Sample Preparation: Employs a solid sorbent [Chromosorb® 106 (GB); Chromosorb® 106/AgF (VX); or
Tenax® TA (HD)] for extract or standard concentration followed by thermal desorption into the analytical
system
Other: Limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration
standards)
Aqueous Liquid
Drinking Water
Photoionization mass
spectrometry
Analytical Chemistry.
2006. 78: 2967-2976
Detection: Method detection range 0.07 - 0.7 mg/L
Performance: RSDs <10%
Sample Throughput: Sample cycle time 45 seconds
Sample Preparation: Direct sampling in water
Other: Tested for similar compounds
Air
Portable GC-MS
(fieldable)
Sensors and Actuators
B. 2005. 108: 193-197
Quantitation: Able to qualitatively and semi-quantitatively identify mustard
Sample Throughput: Analyte identified within 12 minutes
Interferences: High mustard concentrations lead to memory effects
GC-MS
Journal of
Chromatography A.
2001.925:241-249
Detection: Detection limit 50 ng/tube (full scan). S:N at 50 ng/tube >4:1.
Quantitation: Semi-quantitative
Performance: RSD at 50 ng/tube for GB 21%; GD1 17%; GD2 13%; GA8%; GF 11%; VX30%; HN1
22%; HN228%; HNS 17%
Sample Throughput: Samples can be analyzed only once
Sample Preparation: Automated thermal desorption. Tube is connected to heated GC injector (100 C).
Other: Temperature and time of storage were found to influence recovery of analytes, with best
recoveries being observed after one day of storage in a freezer (-12 C)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -46
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Nicotine compounds
(analyze as nicotine)
Octahyd ro-1, 3,5,7-
tetranitro-1 ,3,5,7-
tetrazocine (HMX)
Organophosphate
pesticides, NOS
Matrix
Aqueous Liquid
Drinking Water
Solid
Wipes
Non-aqueous
Liquid/Organic
Solid
Aqueous Liquid
Drinking Water
Solid
Wipes
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Solid
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Technique
GC-MS
Rapid HPLC
Rapid TLC (fieldable)
Immunoassay
Colorimetric
screening
GC-MS
GC-MS
Reference Source*
Journal of
Chromatography A.
2003. 1017: 187-93
EPA Method 8270D (SW-
846)
Journal of Forensic
Science. 2005. 49(6):
1181-1186
Chemistry for the
Protection of the
Environment 4. 2003. 59:
125-135
EPA Method 4050 (SW-
846)
EPA Method 4051 (SW-
846)
EPA Method 8510 (SW-
846)
EPA Method 8270D (SW-
846)
EPA Method TO-10A
(ORD)
Comments
Sample Throuahput: Retention time -18.7 minutes
Sample Preparation: Extract with ether and 10% sodium hydroxide solution
Sample Preparation: MeCI? extraction
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Detection: Detection of TNT at concentrations >1 ppm. 95% of samples containina <0.7 ppm of TNT
will produce a negative result.
Workina Ranae: 1 - 30 ppm (TNT)
Quantitation: Semi-quantitative
Detection: Detection limit >500 ppm
Sample Preparation: Performed usina an extract of a soil sample
Other: Test desianed to detect TNT
Detection: Detection limit 150 ppb
Other: Test desianed to detect RDX
Interferences: Other chemically-related explosives (i.e., nitroauanidine, NG, PETN, and tetrvl)
Detection: Compound dependent, detection ranae between 10- 1000 |ja/L for aqueous liquid samples
and 660 - 3300 |jg/kg for soil samples
Sample Preparation: MeCI? shake and shoot extraction
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -47
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Osmium tetroxide
(analyze for osmium)
Oxamyl
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
(particulates)
Solid
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Technique
Atomic absorption
spectroscopy
Portable X-ray
fluorescence
(fieldable)
HPLC
HPLC-ESI-MS-SIM
MEKC
HPLC-UV
Reference Source*
Applied Spectroscopy.
1968. 22(5): 532-535
EPA Method 6200 (SW-
846)
Journal of
Chromatography A.
1996.726:99-113
Analytica Chimica Acta.
2004.505:209-215
Electrophoresis. 2001 .
22(11): 2260-2269
EPA Method 831 8A (SW-
846)
NIOSH Method 5601
Comments
Detection: Sensitivity 1 ppm
Quantitation: Relative error ±4%
Workina Ranae: Concentration ranae 1 -300 ppm (total osmium)
Sample Throuahput: Operator time <5 minutes/sample
Interferences: Results are not affected bvthe valence state of osmium
Detection: MDL above the toxicitv characteristic reaulatorv level for most RCRA analvtes
Sample Preparation: For air samples, use hiah-volume air samplers, and collect sample filters
Detection: Detection limit 0.5 |Jd/L
Performance: Recovery 21%
Sample Throuqhput: Retention time ~1 1 .88 minutes
Other: Diode array with online sample enrichment
Detection: Detection limit 0.10 |Jd/L
Performance: Recovery 65%
Sample Throuahput: Retention time <3 minutes
Sample Preparation: SPE
Workina Ranae: 0.5 - 5.0 ma/L
Sample Preparation: SPE and sample stackina. N-Methvlcarbamates are extracted from aqueous
samples with MeCI2, and from soils, oily solid waste, and oils with acetonitrile.
Interferences: Fluorescent compounds, primarily alkvl amines and compounds which yield primary alkvl
amines on base hydrolysis, are potential sources of interferences
Other: Developed for the determination of 14 pesticides such as aldicarb, carbofuran, isoproturon,
chlorotoluron, metolachlor, mecoprop, dichlorprop, MCPA, 2,4-D, methoxychlor, IDE, DDT, dieldrin,
and DDE in drinking water. Good recoveries of pesticides were obtained using SPE with sample pH
adjusted to 2 - 3.
Other: Tested for similar compounds (aldicarb and carbofuran)
Detection: Detection limit 0.0025 ua/L
Workina Ranae: 0.05 - 1 |ja/L
Rapid Screening and Preliminary Identification Techniques and Methods
1 -48
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Paraquat
Paraoxon
Parathion
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Air
Technique
Immuoassay
(fieldable)
HPLC-MS
GC-MS
GC-MS-SPME
GC-MS
Reference Source*
Envirologix Quantiplate
Kit EP 023
www.enviroloaix.com
(accessed November 19,
2009)
SDI RAPID Assay®
http://www.sdix.com/Prod
uctSDecs.asc?nProductl
D=26 (accessed
November 19, 2009)
"Rapid Screening
Method for the Analysis
of Paraquat and Diquat
by LC-MSD Using
Selective Ion Monitoring
and Large Volume
Injection," Agilent
Application Note, 2002
httD://www.chem.aailent.c
om/Librarv/aDDlications/5
988-7220EN.cdf
(accessed November 19,
2009)
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Journal of
Chromatography A.
2002.963: 107-116
EPA Method TO-10A
(ORD)
Comments
Detection: Detection limit 0.10 |Jd/L
Workina Ranae: 0.02 - 1 .0 ppb
Sample Throuahput: Results in 90 minutes
Other: Antibody-coated microwell plate: eiaht removable strips of 12 microwells each, in reclosable foil
bag with desiccant
Detection: Detection limit 20 ppt
Sample Preparation: The Paraquat RAPID Assay® applies the principles of ELISA for the determination
of free paraquat cation
Detection: Detection limit <0.4 |Jd/L
Sample Preparation: Uses an ion-pairina reaaent to help separate compounds and prepare paraquat in
ionic form
Sample Throuahput: -20 minutes per sample
Sample Preparation: MeCI? extraction
Other: Tested on similar compounds. Full scan usina limited QC for rapid analysis (e.a., an instrument
blank and instrument tune, but no calibration standards).
Detection: Detection limit 0.09 |Jd/L (methyl parathion)
Sample Throuahput: Retention time ~31 .26 minutes (methyl parathion)
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -49
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Pentaerythritol
tetranitrate (PETN)
Phencyclidine
Phenol
Matrix
Aqueous Liquid
Drinking Water
Solid
Wipes
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
Rapid HPLC
Immunoassay
(fieldable)
GC-MS
GC-MS
Reference Source*
Journal of Forensic
Science. 2005. 49(6):
1181-1186
Chemistry for the
Protection of the
Environment 4. 2003. 59:
125-135
Phencyclidine
RapiCard™ Test
httD://www. raDidtest.com
(accessed November 19,
2009)
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
EPA Method TO-13A
(ORD)
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
EPA Methods
3520C/3535A (water),
3545A/3541 (solid), or
3580A (non-aqueous)
with 8270D (SW-846)
Comments
Quantitation: Semi-quantitative
Sample Throuahput: Usina HPLC with reversed-phase monolithic columns, 1 1 explosives can be
quantified in <14 minutes. A rapid version of this technique can separate seven explosives in <2
minutes.
Other: 2,6-DNT is not resolved from other DNT isomers. Procedure is based on a method for soil
analyses, but could be modifed to analyze water matrices.
Detection: Detection limit 25 |Jd/L
Sample Preparation: Soil samples should be extracted in water
Other: Phencvclidine RapiCard™ Test specifically desianed for urine, but may work for water and soil
analysis
Sample Throuahput: Samples can be analyzed only once
Sample Preparation: MeCI? extraction
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Other: Air samples collected onto SUMMA canister for analysis by GC-MS. Full scan usina limited QC
for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Sample Throuahput: Samples can be analyzed only once
Sample Preparation: MeCI? extraction
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Quantitation: Quantitation limit 10 |ja/L (water): 660 |ja/L (solid)
Performance: Averaae recovery (n=4 with test concentration of 100 |ja/L) 16.6 - 100.0%
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards).
Rapid Screening and Preliminary Identification Techniques and Methods
1 -50
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Phenol
Phorate
Phorate sulfone
Phorate sulfoxide
Phosgene
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Air
Technique
SPME sampling
portable GC-MS
(fieldable)
Draeger gas
detection tube
GC-FID (direct
injection)
GC-MS or HPLC
GC-MS
GC-MS
GC-NPD
Draeger gas
detection tube
Reference Source*
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Draeger gas detection
tube Phenol 1/b (P/N
8101641)
http://www.draeaer.com/
US/en US/ (accessed
November 19, 2009)
EPA Method TO-8
(ORD)
EPATO-IOA(ORD)
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
EPA Method TO-10A
(ORD)
OSHA Method 61
Draeger gas detection
tube Phosgene 0.02/a
(P/N 81 01 521)
httD://www.afcintl.com/Ddf
/draeaer/8101521.cdf
(accessed November 19,
2009)
Comments
Sample Throuahput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Detection: Detection ranae 1-20 ppm
Sample Preparation: A calibrated 100-mL sample of air is drawn throuah the tube with a pump (Draeaer
accuro® or equivalent)
Other: Aqueous impinaer collection. Glass impinaers may be fraaile and thus may be easily broken.
Detection: Detection limits 0.2-10 ua/mL (HPLC)
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Sample Throuahput: Samples can be analyzed only once
Sample Preparation: MeCI? extraction
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Sample Preparation: Collect air samples on sorbent tubes for derivatization by 2-
(hydroxymethyl)piperidine
Detection: Detection ranaes 0.02 - 1 ppm: 0.02 - 0.6 ppm
Performance: Standard deviation ±10- 15%
Sample Throuahput: -12 minutes/sample
Sample Preparation: A calibrated 100-mL sample of air is drawn throuah the tube with a pump (Draeaer
accuro® or equivalent)
Interferences: Chlorine and hydrochloric acid. Absolute humidity over 3 - 15 ma H?O/L.
Rapid Screening and Preliminary Identification Techniques and Methods
1 -51
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Phosphamidon
Phosphine
Phosphorus trichloride
Pinacolyl methyl
phos phonic acid
(PMPA) (degradation
product of GD)
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Air
Air
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
GC-MS
GC-MS-SPME
GC-MS
Draeger gas
detection tube
(fieldable)
ICP-AES
Spectrophotometer
HPLC-ESI-MS-SIM
HPLC-APCI-MS-SIM
Reference Source*
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Journal of
Chromatography A.
2002.963: 107-116
EPA Method TO-10A
(ORD)
Draeger gas detection
tube
Phosphine 0.01 /a (P/N
8101 611); 0.1/a(P/N
CH31101); 1/a(P/N
8101801);25/a(P/N
8101621);50/a(P/N
CH21201)
http://www.draeaer.com/
US/en US/ (accessed
November 19, 2009)
OSHA Method 1003
NIOSH Method 6402
Journal of
Chromatography. 1998.
794: 234-244
Journal of
Chromatography A.
1999.862(2): 169-177
Comments
Sample Preparation: MeCI? extraction
Other: Tested on similar compounds. Full scan usina limited QC for rapid analysis (e.a., an instrument
blank and instrument tune, but no calibration standards).
Detection: Detection limit 0.09 |Jd/L (methyl parathion)
Sample Throuahput: Retention time -31 .26 minutes (methyl parathion)
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Detection: Detection ranaes 0.01 -1 ppm: 0.1 -4ppm: 1 - 100 ppm: 25- 10,000 ppm: 15-1,000
ppm; 0.01 -100 ppm
Sample Throuqhput: Measurina time 20 seconds - 13 minutes (dependina on concentration)
Sample Preparation: A calibrated 100-mL sample of air is drawn throuah the tube with a pump (Draeaer
accuro® or equivalent)
Sample Preparation: Samples are collected by drawina air, with personal samplina pumps, throuah
sampling cassettes containing a glass fiber filter and a mercuric chloride-treated polyester filter.
Samples are digested with sulfuric acid and analyzed.
Sample Preparation: Samples are collected in bubbler for analysis by Spectrophotometer
Sample Throuqhput: Retention time ~3.1 minutes
Sample Preparation: Water samples can be analyzed directly. Soil and non-aqueous liquid samples are
extracted with water, filtered, and analyzed.
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Detection: Detection limits are two times lower than for LC-APCI-MS-SIM method
Sample Throuahput: Retention time -3.1 minutes
Sample Preparation: Water samples can be analyzed directly. Soil samples are extracted with water,
filtered, and analyzed.
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -52
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Pinacolyl methyl
phos phonic acid
(PMPA) (degradation
product of GD)
Propylene oxide
R-33 (VR)
[Methylphosphonothioi
c acid, S-[2-
(diethylamino)ethyl] O-2
methylpropyl ester]
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Air
Technique
HPLC-MS
GC-MS (purge and
trap)
GC-MS
GC-MS
Photoionization mass
spectrometry
Portable GC-MS
(fieldable)
Reference Source*
EPA Method TO-10A
(ORD)
EPA Methods 5030C
(water), 5035A (solid), or
3585 (non-aqueous) with
8260C (SW-846)
NIOSH Method 1612
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Analytical Chemistry.
2006. 78: 2967-2976
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Comments
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: No derivatization required. Limited QC for rapid analysis (e.a., an instrument blank and
instrument tune, but no calibration standards).
Detection: 1 - 2 |jL injection of a 1:1 dilution can be used to provide detection limits of 0.5 ppm
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples,
Method 5035A for solid samples, and Method 3585 for non-aqueous liquid/organic solid samples
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Detection: Estimated 0.01 ma per sample
Workina Ranqe: Workina ranae 8 - 295 ppm for air samples of 5 L
Sample Preparation: Thermal desorption from charcoal sorbent tube
Other: Limited QC for rapid analysis
Performance: Averaae recovery for VX 52 - 59% (water): 59 - 68% (soil, usina MeOH with 1 % TEA)
Sample Throuqhput: Samples can be analyzed only once
Sample Preparation: MeCI? extraction (aqueous and solid samples). VX may require MeOH with 1%
TEA for extraction from solids.
Other: Tested for similar compound (VX) in water only. Full scan usina limited QC for rapid analysis
(e.g., an instrument blank and instrument tune, but no calibration standards).
Detection: Method detection ranae 0.07 - 0.7 ma/L
Performance: RSDs were aenerallv <10%
Sample Throuqhput: Sample cycle time 45 seconds
Sample Preparation: Direct samplina in water
Other: Tested for similar compounds
Sample Throuahput: Analysis time ~16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD ~12 minutes; HD ~13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds (G-aaents and mustards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -53
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference Source*
Comments
Sarin (GB)
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
GC-MS
Aqueous Liquid
Drinking Water
Solid
Wipes
GC-FPD
GC-MS-EI
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Performance: Recovery for GB 69 - 80% (water); 62 - 114% (soil)
Sample Throughput: Samples can be analyzed only once
Sample Preparation: Shake and shoot MeCI2 extraction
Other: Tested for MeCI2, GB, GD, HD, and GF at concentrations of 5.0 mg/m3. Full scan using limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
EPA Methods 357173572
with8170(SW-846)
Performance: For direct injection soil recovery range (and RSD) for GB 88-104 (±5.7)%; HD 94-104
(±3.9)%); VX 92 - 114 (±8.2)%. For DAAMS soil recovery range (and RSD) for GB 96-128 (±9)%; HD
124-139 (±7)%; VX 85-107 (±8)%. For direct injection water recovery range (and RSD) for GB 77 -
90 (±5.7)%; HD 77 - 90 (±6)%; VX 87-103 (±5.7)%.
Sample Preparation: Uses a solid sorbent [Chromosorb® 106 (GB); Chromosorb® 106/AgF (VX); or
Tenax® TA (HD)] for extract or standard concentration followed by thermal desorption into the analytical
system. Sample collection, preparation, preservation, and storage are described in Methods 3571 and
3572.
Other: Limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration
standards)
EPA Methods 357173572
with 8271 (SW-846)
Performance: For direct injection soil recovery range (and RSD) for GB 99.6 - 145 (±12.3)%; HD 103 -
112 (±19)%); VX 61 - 110 (±6.9)%. For DAAMS soil recovery range (and RSD) for GB 78 - 95 (±7.2)%;
HD 84 - 94 (±5.4)%; VX 71 - 85 (±6.9)%. For direct injection water recovery range (and RSD) for GB
103 - 135 (±5.7)%; HD 95 - 151 (±6)%; VX 95 - 151 (±17)%.
Sample Preparation: Uses a solid sorbent [Chromosorb® 106 (GB); Chromosorb® 106/AgF (VX); or
Tenax® TA (HD)] for extract or standard concentration followed by thermal desorption into the analytical
system. Sample collection, preparation, preservation, and storage are described in Methods 3571 and
3572.
Other: Limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration
standards)
Aqueous Liquid
Drinking Water
Photoionization mass
spectrometry
Analytical Chemistry.
2006. 78: 2967-2976
Sample Throughput: Sample cycle time 45 seconds
Sample Preparation: Direct sampling in water
Other: Tested on a similar compound (GB). No sample preparation required.
Drinking Water
GC-MS (fieldable)
Field Analytical
Chemistry and
Technology. 1998.2(1):
3-20
Detection: S:N for injection of 0.6 ng (neat) 8.5
Rapid Screening and Preliminary Identification Techniques and Methods
1 -54
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Sarin (GB)
Semivolatile organic
compounds, NOS
Sodium arsenite
(analyze for total
arsenic)
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Air
(particulates)
Solid
Wipes
Aqueous Liquid
Drinking Water
Technique
GC-MS (fieldable)
Automated Thermal
Desorption GC-MS
GC-MS
GC-MSD
X-ray fluorescence
analyzer (fieldable)
Spectrophotometry
Reference Source*
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Journal of
Chromatography A.
2001.925:241-249
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Modified EPA Method
TO-10AorTO-17(ORD)
EPA Method 6200 (SW-
846)
Hach Water Analysis
Handbook. 5th Edition.
2008
Comments
Sample Throuahput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Detection: Detection limit 50 no/tube (full scan). S:N ratio at 50 no/tube was >4:1 .
Quantitation: Semi-quantitative
Performance: RSD at 50 no/tube for GB 21%: GD1 17%: GD2 13%: GA8%: GF 11%: VX30%: HN1
22%; HN228%; HNS 17%
Sample Throuqhput: Retention time -8.3 minutes. Samples can be analyzed only once.
Sample Preparation: Automated thermal desorption. Tube is connected to heated GC injector (100°C).
Other: Temperature and time of storaae were found to influence recovery of analvtes, with best
recoveries being observed after one day of storage in a freezer (-12 C)
Sample Throuqhput: Samples can be analyzed only once
Sample Preparation: MeCb extraction
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Performance: RSD ranae 5 - 30% (n>5). Recoveries ranaina from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Detection: Interference-free detection limit 40 ma/ka
Interferences: Potential interferences include particle size, uniformity, homoaeneitv, surface condition,
high moisture content, and high concentration of other heavy metals
Detection: Detection ranae 0.02 - 0.20 ma/L. Measures total arsenic
Interferences: Potential interferences include antimony salts
Other: Silver diethvldithio-carbamate method
Rapid Screening and Preliminary Identification Techniques and Methods
1 -55
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference Source*
Comments
Sodium arsenite
(analyze for total
arsenic)
Aqueous Liquid
Drinking Water
ICP-AES or -MS
EPA Method 601OC (SW-
846); EPA Methods
200.7/200.8 (OW)
Detection: Estimated detection limit 53 ng/L (Method 200.7). Method detection limit 1.4 |jg/L (water); 0.6
M9/L (solids) (for Method 200.8).
Sample Preparation: Acid-digestion, filtration. Add HNO3 and evaporate to near dryness then reflux.
Continue heating and add additional acid as necessary, until the digestion is complete (Method 200.7).
Groundwater samples which have been prefiltered and acidified will not need acid digestion (Method
601 OC).
Interferences: Background contribution from emission of high concentration elements, >100 mg/L of
aluminum, dust in the laboratory environment, impurities in reagents, and on laboratory apparatus which
the sample contacts (Method 200.7)
Other: Limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration
standards). In cases where low concentrations of compounds are being addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES.
Non-aqueous
Liquid/Organic
Solid
ICP-MS
EPA Method 6020A (SW-
846)
Sample Preparation: Extraction in aqueous nitric acid
Other: Limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration
standards). In cases where low concentrations of compounds are being addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES.
Air
ICP-AES
EPA Method 200.7 (OW)
Sample Throughput: A significant amount of time is saved by digesting air samples in plastic centrifuge
tubes using microwave energy at atmospheric pressure
Other: In cases where low concentrations of compounds are being addressed, ICP-MS instrumentation
may be more appropriate than ICP-AES
Sodium azide (analyze
as azide ion)
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
GC-MS (purge and
trap)
EPA Methods 5030C
(water), 5035A (solid) or
3585 (non-aqueous) with
8260C (SW-846)
Detection: Detection limits 5 |jg/kg (wet weight) for soil/sediment samples; 0.5 mg/kg (wet weight) for
wastes; 5 |jg/L for ground water, using standard quadrupole instrumentation and the purge and trap
technique
Quantitation: Quantitation limits 5 |jg/L (water); 5 |jg/kg (solid)
Sample Preparation: Based on Method 8260 using Method 5030C for preparation of water samples,
Method 5035A for solid samples, and Method 3585 for non-aqueous liquid/organic solid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan using limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Aqueous Liquid
Drinking Water
Solid
Wipes
1C
J. of Forensic Sciences.
1998. 43(1): 200-202
Detection: Detection limit 30 ng/mL
Performance: Recovery range 83 - 85%
Working Range: Calibration range 100- 10,000 ng/mL
Sample Preparation: Acidification to NH3 (gas) and bubbled through NaOH
Rapid Screening and Preliminary Identification Techniques and Methods
1 -56
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Sodium azide (analyze
as azide ion)
Soman (GD)
Strychnine
Matrix
Air
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Solid
Wipes
Technique
1C
GC-MS
Photoionization mass
spectrometry
Portable GC-MS
(fieldable)
GC-MS
HPLC-MS
Reference Source*
OSHA Method ID-211
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Analytical Chemistry.
2006. 78: 2967-2976
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Based on results of
Battelle evaluation
(2006) of analytical
procedures for detection
of strychnine
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
EPA Method 8321 B (SW-
846)
Comments
Detection: Detection limit (for 5-L air sample) 0.001 ppm (0.003 ma/m )
Quantitation: Quantitation limit 0.004 ppm (0.011 ma/m3)
Workina Ranae: 0.057 - 2.63 com
Interferences: Ions such as bromides, adipic acid, or nitrates. Do not use wipe materials composed of
cellulose (PVC or glass fiber wipes recomended).
Performance: Recovery for GD 84 (+9)% (water): 85 - 99% (soil)
Sample Throughput: Samples can be analyzed only once
Sample Preparation: MeCb extraction
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Detection: Method detection ranae 0.07 - 0.7 ma/L
Performance: RSDs <10%
Sample Throughput: Sample cycle time 45 seconds
Sample Preparation: Direct samplina in water
Other: Tested for similar compounds
Sample Throuahput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Sample Preparation: Base extraction
Sample Throughput: Samples can be analyzed only once
Sample Preparation: MeCI? extraction
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Sample Preparation: Acetonitrile/water extraction
Interferences: Compounds with hiah proton affinity may mask taraet analvtes
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -57
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Sulfur dioxide
Sulfur trioxide
Tabun (GA)
Matrix
Air
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Aqueous Liquid
Technique
UV luminescence
detector
Toxic Gas leak
detector
Draeger gas
detection tube
Titrimetry
GC-MS
GC-MS (portable)
(fieldable)
Photoionization mass
spectrometry
Reference Source*
Environmental Field
Technologies Verification
Program
http://www.epa.aov/etv/vt-
ams.html#hsm
(accessed November 19,
2009)
CEA S-3200 Toxic Gas
Leak Detector
httD://www.ceainstr.com/
cdf datasheets/seriesu I
nfo.pdf (accessed
November 19, 2009)
Draeger gas detection
tube Sulfur Dioxide 0.1 /a
(P/N 67271 01 );0.5/a
(P/N 6728491); 1/a (P/N
CH31701);20/a(P/N
CH24201);50/b(P/N
8101531)
http://www.draeaer.com/
US/en US/ (accessed
November 19, 2009)
EPA Method 8 (OAQPS)
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Field Analytical
Chemistry and
Technology. 1998. 2(1):
3-20
Analytical Chemistry.
2006. 78: 2967-2976
Comments
Detection: Detection ranae 4 - 300 ppb
Performance: Recovery 131%
Interferences: Interferences include carbanvl sulfide, dimethyl sufide, and methyl mercaptan
Detection: Detection ranaes 0-250 com: 0-1000 com: 0- 10,000 com
Detection: Detection ranaes 0.1 - 3 com: 0.5 - 25 com: 1 - 25 com: 20 - 20,000 com: 50 - 8,000 com
Sample Preparation: A calibrated 100-mL sample of air is drawn throuah the tube with a pump (Draeaer
accuro® or equivalent)
Detection: Detection limit 0.06 ma/m3 (as H,SO^)
Performance: Averaae recovery for GA 51 - 66% (water): 66 - 115% (soil)
Sample Throuahput: Samples can be analyzed only once
Sample Preparation: MeCI? extraction
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Other: S:N ratio for injection of 1 .5 na (neat) 5.9
Detection: Method detection ranae 0.07 - 0.7 ma/L
Performance: RSDs <10%
Sample Throuahput: Sample cycle time 45 seconds
Sample Preparation: Direct samplina in water
Other: Tested for similar compounds
Rapid Screening and Preliminary Identification Techniques and Methods
1 -58
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Tabun (GA)
Tetraethyl
pyrophosphate
Tetramethylene-
disulfotetramine
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Technique
Portable GC-MS
(fieldable)
GC-MS
GC-MS
GC-MS
SPME-GC-NPD
GC-MS
Reference Source*
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Journal of
Chromatography A.
2001.925:241-249
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Analytica Chimica Acta.
2000. 404(2): 329-334
EPA Method TO-10A
(ORD)
Comments
Sample Throuahput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Detection: Detection limit 50 no/tube (full scan). S:N ratio at 50 no/tube was 54:1 .
Quantitation: Semi-quantitative
Performance: RSD at 50 no/tube for GB 21%: GD1 17%: GD2 13%: GA8%: GF 11%: VX30%: HN1
22%; HN228%; HNS 17%
Sample Throuahput: Retention time -8.3 minutes. Samples can be analyzed only once.
Sample Preparation: Automated thermal desorption. Tube is connected to heated GC injector (100°C).
Other: Temperature and time of storaae were found to influence recovery of analvtes, with best
recoveries being observed after one day of storage in a freezer (-12°C)
Sample Throughput: Samples can be analyzed only once
Sample Preparation: MeCb extraction (aqueous and solid samples)
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Sample Throughput: Samples can be analyzed only once
Sample Preparation: MeCb extraction (aqueous and solid samples)
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Detection: Detection limit 0.001 ma/mL
Workina Ranae: Concentration ranae 0.008 - 0.5 ma/mL (with correlation coefficient of 0.998)
Sample Preparation: Tetramine was extracted with a fused silica fiber coated with 100-mm PDMS and
detected by GC with a NPD
Performance: RSD ranae 5 - 30% (n>5). Recoveries ranaina from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -59
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Thallium sulfate
(analyze for total
thallium)
Thiodiglycol (TDG)
(degradation product of
HD)
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Air
(particulates)
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Solid
Aqueous Liquid
Drinking Water
Air
Technique
Spectrophotometry
ICP-AES or -MS
ICP-MS
X-ray fluorescence
analyzer (fieldable)
ICP-AES
HPLC-APCI-MS-SIM
ESI-MS-SRM
GC-MS
Reference Source*
Hach Water Analysis
Handbook. 5th Edition.
2008
EPA Method 601 OC (SW-
846); EPA Methods
200.7/200.8 (OW)
EPA Method 6020A (SW-
846)
EPA Method 6200 (SW-
846)
EPA Method 200.7 (OW)
Journal of
Chromatography A.
1999.862(2): 169-177
Rapid Communications
in Mass Spectrometry.
2006. 20: 981-986
EPA Method TO-10A
(ORD)
Comments
Interferences: Potential interferences include antimony salts: measures total arsenic
Other: Silver diethvldithio-carbamate method
Sample Preparation: Acid-diaestion, filtration. Add HNO, and evaporate to near drvness then reflux.
Continue heating and add additional acid as necessary, until the digestion is complete (Method 200.7).
Groundwater samples which have been prefiltered and acidified will not need acid digestion (Method
601 OC).
Interferences: Backaround contribution from emission of hiah concentration elements, >100 ma/L of
aluminum, dust in the laboratory environment, impurities in reagents, and on laboratory apparatus which
the sample contacts (Method 200.7)
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards). In cases where low concentrations of compounds are being addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES.
Sample Preparation: Extraction in aqueous nitric acid
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards). In cases where low concentrations of compounds are being addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES.
Interferences: Potential interferences include particle size, uniformity, homoaeneitv, surface condition,
high moisture content, and high concentration of other heavy metals.
Sample Throughput: A sianificant amount of time is saved by diaestina air samples in plastic centrifuae
tubes using microwave energy at atmospheric pressure
Other: In cases where low concentrations of compounds are beina addressed, ICP-MS instrumentation
may be more appropriate than ICP-AES
Detection: Detection limit <10 na/mL (in water, usina 20 |jL injections)
Sample Throuahput: Retention time -5.2 minutes
Sample Preparation: Water samples can be analyzed directly. Soil samples are extracted with water,
filtered, and analyzed.
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Detection: Detection limit 500 |ja/L (with 10 |jL injection). For low concentrations, the addition of
ammonium halides is required to see the [M-H]- peak.
Sample Preparation: Water samples can be analyzed directly. Does not require any sample
preparation.
Performance: RSD ranae 5 - 30% (n>5). Recoveries ranaina from 65 - 125%.
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -60
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Thiofanox
1,4-Thioxane
(degradation product of
HD)
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
HPLC-UV
HPLC-APCI-MS-SPE
HPLC-APCI-MS-LLE
HPLC-UV
GC-MS (fieldable)
GC-MS
Reference Source*
Chemosphere. 2005. 61 :
1580-1586
"A General Unknown
Screening For Drugs and
Toxic Compounds in
Human Serum." Thesis.
httD://Daaes.unibas.ch/di
ss/2005/DissB 7295.pdf
(accessed November 19,
2009)
Journal of
Chromatography B.
1999.731: 155-165
NIOSH Method 5601
Field Analytical
Chemistry and
Technology. 1998.2(1):
3-20
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Comments
Sample Preparation: Filtration, requires no extraction
Other: Tested for similar compounds
Sample Preparation: SPE cartridae extraction
Other: Tested for similar compounds
Sample Preparation: Extraction with ethvl acetate and evaporation to drvness, followed bv redissolvina
in acetonitrile
Other: Tested for similar compounds
Sample Preparation: Collect air samples on sorbents. Extraction (with 0.2% V/V 0.1 M aqueous
triethylamine phosphate buffer in acetonitrile, pH 6.9 - 7.1) from filter/solid sorbent tube (OVS-2 Tube:
13-mm quartz fiber filter; XAD-2, 270 mg/140 mg).
Interferences: Potential interferences include chloroform, toluene, BHT, dialkvl phthalates, nicotine,
caffeine, impurities in HPLC reagents (e.g., in triethylamine), other pesticides (2,4-D, atrazine,
parathion, etc.), and pesticide hydrolysis products (1-naphthol)
Other: Tested for similar compounds
Other: S:N for iniection of 3.1 na (neat) 17.3
Sample Throuqhput: Samples can be analyzed once
Sample Preparation: MeCb extraction
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Rapid Screening and Preliminary Identification Techniques and Methods
1 -61
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Titanium tetrachloride
(analyze for total
titanium)
Triethanolamine (TEA)
(degradation product of
HN-3)
Trimethyl phosphite
Matrix
Solid
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
ICP-AES
Portable X-ray
fluorescence
(fieldable)
ICP-MS
LC-MS
HPLC-MS
GC-MS
Reference Source*
EPA Method 601 OC (SW-
846);
EPA Method 200.7 (OW)
EPA Method 6200 (SW-
846)
EPA Method 6020A (SW-
846);
EPA Method 200.8 (OW)
Journal of
Chromatography A.
2006. 1102:214-223
EPA Method TO-10A
(ORD)
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Comments
Detection: Estimated instrument detection limit 5 |Jd/L (for Method 601 OC, as titanium at 334.9 nm)
Sample Preparation: Acid-diaestion, filtration. Add HNO^and evaporate to near drvness then reflux.
Continue heating and add additional acid as necessary, until the digestion is complete (Method 200.7).
Groundwater samples which have been prefiltered and acidified will not need acid digestion (Method
601 OC).
Interferences: Backaround contribution from emission of hiah concentration elements, >100 ma/L of
aluminum, dust in the laboratory environment, impurities in reagents and on laboratory apparatus
Other: Use limited QC for rapid analysis (e.a., an instrument blank and an instrument tune, but no
standards). In cases where low concentrations of compounds are being addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES.
Detection: MDL above the toxicitv characteristic reaulatorv level for most RCRA analvtes
Sample Preparation: Acid-diaestion and filtration
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards). In cases where low concentrations of compounds are being addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES.
Detection: Detection limit 0.02 ppm
Sample Throughput: Analysis time <20 minutes
Sample Preparation: Soils and non-aqueous liquid/oraanic solids should first be extracted into water.
Acetonitrile (1 mL) is added to emulsion and vortexed for 10 seconds followed by centrifugation at
4500g for 10 minutes. Water samples are analyzed directly.
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Sample Throughput: Samples can be analyzed only once
Sample Preparation: MeCb extraction
Other: Tested for MeCk GB, GD, HD, and GF at concentrations of 5.0 ma/m3. Full scan usina limited
QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration standards).
Rapid Screening and Preliminary Identification Techniques and Methods
1 -62
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference Source*
Comments
Trimethyl phosphite
Air
Portable GC-MS
(fieldable)
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Sample Throughput: Analysis time -16 minutes; total sample throughput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME sampling and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matching
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
1,3,5-Trinitrobenzene
(1,3,5-TNB)
Aqueous Liquid
Drinking Water
Solid
Wipes
Rapid HPLC
Journal of Forensic
Science. 2005. 49(6):
1181-1186
Sample Throughput: A rapid version of this technique can separate seven explosives in <2 minutes
Other: Has been evaluated for similar compounds. TNT cannot be resolved from tetryl. This procedure
is based on a method for soil analyses but could be modifed to analyze water matrices.
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Rapid TLC (fieldable)
Chemistry for the
Protection of the
Environment 4. 2003. 59:
125-135
Quantitation: Semi-quantitative
Solid
Wipes
Immunoassay
EPA Method 4050 (SW-
846)
Detection: Detection limit 4 ppm
2,4,6-Trinitrotoluene
(2,4,6-TNT)
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Rapid HPLC
Journal of Forensic
Science. 2005. 49(6):
1181-1186
Sample Throughput: A rapid version of this technique can separate seven explosives in <2 minutes
Other: Has been evaluated for similar compounds. TNT cannot be resolved from tetryl. This procedure
is based on a method for soil analyses but could be modifed to analyze water matrices.
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Fast GC-PDECD or
-MS
Journal of Forensic
Science. 2006. 51: 815
Sample Throughput: Nine explosives detected in <3 minutes
Sample Preparation: No sample preparation method was investigated; Method 8330 is recommended
for solids and Method 3535 is recommended for liquids
Rapid Screening and Preliminary Identification Techniques and Methods
1 -63
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
2,4,6-Trinitrotoluene
(2,4,6-TNT)
Vanadium pentoxide
(analyze for total
vanadium)
Matrix
Solid
Wipes
Solid
Wipes
Air
(particulates)
Solid
Wipes
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Air
Technique
Immunoassay
Colorimetric
screening
X-ray fluorescence
analyzer (fieldable)
Spectrophotometry
ICP-AES or -MS
ICP-MS
ICP-AES
Reference Source*
EPA Method 4050 (SW-
846)
EPA Method 851 5 (SW-
846)
EPA Method 6200 (SW-
846)
Hach Water Analysis
Handbook. 5th Edition.
2008
EPA Method 601 OC (SW-
846); EPA Methods
200.7/200.8 (OW)
EPA Method 6020A (SW-
846)
EPA Method 200.7 (OW)
Comments
Detection: Detection limit 0.5 ppm
Performance: Usina the test kit from which this method was developed, 93% of soil samples containina
<0.25 ppm of 2,4,6-TNT will produce a negative result, and 99+% of soil samples containing >1 .0 ppm
of 2,4,6-TNT will produce a positive result
Detection: Detection of TNT at concentrations >1 ppm. 95% of samples containina <0.7 ppm of TNT will
produce a negative result.
Workina Ranae: 1 - 30 com (TNT)
Sample Preparation: Sample is treated with color-chanae reaaents and read in spectrophotometer
Performance: Averaae recovery for 5 ppm spike (n=22) 5.1 (±0.4) com with 7.8% RSD
Interferences: Potential interferences include particle size, uniformity, homoaeneitv, surface condition,
high moisture content, and high concentration of other heavy metals
Detection: Measures total arsenic
Interferences: Potential interferences include antimony salts
Other: Silver diethvldithio-carbamate method
Sample Preparation: Acid-diaestion, filtration. Add HNO, and evaporate to near drvness then reflux.
Continue heating and add additional acid as necessary, until the digestion is complete (Method 200.7).
Groundwater samples which have been prefiltered and acidified will not need acid digestion (Method
601 OC).
Interferences: Backaround contribution from emission of hiah concentration elements, >100 ma/L of
aluminum, dust in the laboratory environment, impurities in reagents, and on laboratory apparatus which
the sample contacts (Method 200.7)
Other: Use limited QC for rapid analysis (e.a., a blank and an instrument tune, but no standards). In
cases where low concentrations of compounds are being addressed, ICP-MS instrumentation may be
more appropriate than ICP-AES.
Sample Preparation: Extraction in aqueous nitric acid
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards). In cases where low concentrations of compounds are being addressed, ICP-MS
instrumentation may be more appropriate than ICP-AES.
Sample Throughput: A sianificant amount of time is saved by diaestina air samples in plastic centrifuae
tubes using microwave energy at atmospheric pressure
Other: In cases where low concentrations of compounds are beina addressed, ICP-MS instrumentation
may be more appropriate than ICP-AES
Rapid Screening and Preliminary Identification Techniques and Methods
1 -64
September 2010
-------
Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
VE [phosphonothioic
acid, ethyl-, S-(2-
(diethylamino)ethyl) O-
ethyl ester]
VG [phosphonothioic
acid, S-(2-
diethylamino)ethyl)O,O-
diethyl ester]
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Technique
GC-MS
Photoionization mass
spectrometry
Portable GC-MS
(fieldable)
GC-MS
Photoionization mass
spectrometry
Reference Source*
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Analytical Chemistry.
2006. 78: 2967-2976
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Analytical Chemistry.
2006. 78: 2967-2976
Comments
Performance: Averaae recovery for VX 52 - 59% (water): 59 - 68% (soil, usina MeOH with 1 % TEA)
Sample Throuqhput: Samples can be analyzed only once
Sample Preparation: MeCI? extraction (aqueous and solid samples). VX may require MeOH with 1%
TEA for extraction from solids.
Other: Tested for similar compound (VX) in water only. Full scan usina limited QC for rapid analysis
(e.g., an instrument blank and instrument tune, but no calibration standards).
Detection: Method detection ranae 0.07 - 0.7 ma/L
Performance: RSDs were aenerallv <10%
Sample Throuqhput: Sample cycle time 45 seconds
Sample Preparation: Direct samplina in water
Other: Tested for similar compounds
Sample Throuahput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Performance: Averaae recovery for VX 52 - 59% (water): 59 - 68% (soil, usina MeOH with 1 % TEA)
Sample Throuqhput: Samples can be analyzed once
Sample Preparation: MeCI? extraction (aqueous and solid samples). VX may require MeOH with 1%
TEA for extraction from solids.
Other: Tested for VX in water. Full scan usina limited QC for rapid analysis (e.a., an instrument blank
and instrument tune, but no calibration standards).
Detection: Method detection ranae 0.07 - 0.7 ma/L
Performance: RSDs <10%
Sample Throuahput: Sample cycle time 45 seconds
Sample Preparation: Direct samplina in water
Other: Tested for similar compounds
Rapid Screening and Preliminary Identification Techniques and Methods
1 -65
September 2010
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Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
VG [phosphonothioic
acid, S-(2-
diethylamino)ethyl)O,O-
diethyl ester]
VM [phosphonothioic
acid, methyl-,S-(2-
diethylaminojethyl) O-
ethyl ester]
Volatile Organic
Compounds, NOS
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Technique
Portable GC-MS
(fieldable)
GC-MS
Photoionization mass
spectrometry
Portable GC-MS
(fieldable)
GC-MS (purge and
trap)
Reference Source*
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Analytical Chemistry.
2006. 78: 2967-2976
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
EPA Methods 5030C
(water), 5035A (solid), or
3585 (non-aqueous) with
8260C (SW-846)
Comments
Sample Throuahput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Performance: Averaae recovery for VX 52 - 59% (water): 59 - 68% (soil, usina MeOH with 1 % TEA)
Sample Throuahput: Samples can be analyzed only once
Sample Preparation: MeCI? extraction (aqueous and solid samples). VX may require MeOH with 1%
TEA for extraction from solids.
Other: Tested for VX in water. Full scan usina limited QC for rapid analysis (e.a., an instrument blank
and instrument tune, but no calibration standards).
Detection: Method detection ranae 0.07 - 0.7 ma/L
Performance: RSDs were aenerallv <10%
Sample Throuahput: Sample cycle time 45 seconds
Sample Preparation: Direct samplina in water
Other: Tested for similar compounds
Sample Throuahput: Analysis time -16 minutes: total sample throuahput -3 samples/hour. Retention
time for GB -6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Detection: Detection limits 5 |ja/ka (wet weiaht) for soil/sediment samples: 0.5 ma/ka (wet weiaht) for
wastes; 5 |jg/L for ground water, using standard quadrupole instrumentation and the purge and trap
technique
Quantitation: Quantitation limit 5 |ja/L (water): 5 |ja/ka (solid)
Workina Ranqe: Calibration ranae 1-100 ma/L
Sample Preparation: Based on Method 8260 usina Method 5030C for preparation of water samples,
Method 5035A for solid samples, and Method 3585 for non-aqueous liquid samples
Interferences: Major contaminant sources are volatile materials in the laboratory and impurities in the
inert purging gas and in the sorbent trap
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards). May require low injection port temperatures due to thermal degradation.
Rapid Screening and Preliminary Identification Techniques and Methods
1 -66
September 2010
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Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Volatile Organic
Compounds, NOS
VX [O-ethyl-S-(2-
diisopropylaminoethyl)
methyl
phosphonothiolate]
Matrix
Air
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Aqueous Liquid
Drinking Water
Air
Technique
GC-MSD
GC-FIDor-ECD
SUMMA canister
Portable GC-MS
(fieldable)
GC-MS
Photoionization mass
spectrometry
Portable GC-MS
(fieldable)
Reference Source*
Modified EPA Method
TO-10AorTO-17(ORD)
EPA Method TO-3
(ORD)
EPA Method TO-1
(ORD)
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Sample Preparation
Method for GC/MS
Analysis On Site Joint
Document: United
States/Finland. 1997. 1:
1-125
Analytical Chemistry.
2006. 78: 2967-2976
TrAC — Trends in
Analytical Chemistry.
2004. 23(4): 296-306
Comments
Performance: RSD ranae 5 - 30% (n>5): recoveries ranae from 65 - 125%
Sample Preparation: Thermal desorption from XAD with Tenax® tube
Other: Full scan usina limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but
no calibration standards)
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
Sample Throuahput: Analysis time -16 minutes: total sample throuahput ~3 samples/hour. Retention
time for GB ~6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Performance: Averaae recovery for VX 52 - 59% (water): 59 - 68% (soil, usina MeOH with 1 % TEA)
Sample Throuahput: Samples can be analyzed only once
Sample Preparation: MeCI extraction (aqueous and solid samples). VX may require MeOH with 1% TEA
for extraction from solids.
Other: Tested for similar compound VX in water only. Full scan usina limited QC for rapid analysis (e.a.,
an instrument blank and instrument tune, but no calibration standards).
Detection: Method detection ranae 0.07 - 0.7 ma/L
Performance: RSDs <10%
Sample Throuqhput: Sample cycle time 45 seconds
Sample Preparation: Direct samplina in water
Other: Tested for similar compounds
Sample Throuahput: Analysis time -16 minutes: total sample throuahput -3 samples/hour. Retention
time for GB -6 minutes; phenol -11 minutes; GD -12 minutes; HD -13 minutes; GF -14 minutes.
Sample Preparation: SPME samplina and thermal desorption
Interferences: GF and HD resolution were poor and required spectral manipulation for library matchina
(i.e., subtraction of interfering compound spectrum). Soman diastereomers could not be distinguished
with this system.
Other: Tested for similar compounds
Rapid Screening and Preliminary Identification Techniques and Methods
1 -67
September 2010
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Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference Source*
Comments
VX [O-ethyl-S-(2-
diisopropylaminoethyl)
methyl
phosphonothiolate]
Air
GC-MS
Journal of
Chromatography A.
2001.925:241-249
Detection: Detection limit 50 ng/tube (full scan). S:N ratio at 50 ng/tube was >4:1.
Quantitation: Semi-quantitative
Performance: RSD at 50 ng/tube for GB 21%; GD1 17%; GD2 13%; GA8%; GF 11%; VX30%; HN1
22%; HN228%; HNS 17%
Sample Throughput: Retention time -12 minutes. Samples can be analyzed only once.
Sample Preparation: Automated thermal desorption. Tube is connected to heated GC injector (100 C).
Other: Temperature and time of storage were found to influence recovery of analytes, with best
recoveries observed after one day of storage in a freezer (-12 C)
Aqueous Liquid
Solid
Wipes
GC-MS-EI
EPA Methods 357173572
with 8271 (SW-846)
Performance: For direct injection soil recovery range (and RSD) for GB 99.6 - 145 (±12.3)%; HD 103 -
112 (±19)%); VX 61 - 110 (±6.9)%. For DAAMS soil recovery range (and RSD) for GB 78 - 95 (±7.2)%;
HD 84 - 94 (±5.4)%; VX 71 - 85 (±6.9)%. For direct injection water recovery range (and RSD) for GB
103 - 135 (±5.7)%; HD 95 - 151 (±6)%; VX 95 - 151 (±17)%.
Sample Preparation: Employs a solid sorbent [Chromosorb® 106 (GB); Chromosorb® 106/AgF (VX); or
Tenax® TA (HD)] for extract or standard concentration followed by thermal desorption into the analytical
system. Sample collection, preparation, preservation, and storage are described in Methods 3571 and
3572.
Other: Limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration
standards)
GC-FPD
EPA Methods 3571/3571
with 8170 (SW-846)
Performance: For direct injection soil recovery range (and RSD) for GB 88-104 (±5.7)%; HD 94-104
(±3.9)%); VX 92 - 114 (±8.2)%. For DAAMS soil recovery range (and RSD) for GB 96-128 (±9)%; HD
124-139 (±7)%; VX 85-107 (±8)%. For direct injection water recovery range (and RSD) for GB 77 -
90 (±5.7)%; HD 77 - 90 (±6)%; VX 87-103 (±5.7)%.
Sample Preparation: Employs a solid sorbent [Chromosorb® 106 (GB); Chromosorb® 106/AgF (VX); or
Tenax® TA (HD)] for extract or standard concentration followed by thermal desorption into the analytical
system. Sample collection, preparation, preservation, and storage are described in Methods 3571 and
3572.
Other: Limited QC for rapid analysis (e.g., an instrument blank and instrument tune, but no calibration
standards)
Rapid Screening and Preliminary Identification Techniques and Methods
1 -68
September 2010
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Table 1: Rapid Screening and Preliminary Identification Techniques and Methods for the Chemical Analytes Listed in SAM (cont.)
Analyte
White phosphorus
Matrix
Aqueous Liquid
Drinking Water
Non-aqueous
Liquid/Organic
Solid
Solid
Wipes
Air
Technique
GC-MS
GC-FPD
Reference Source*
Based on EPA Method
7580 (SW-846) using an
MS detector
NIOSH Method 7905
Comments
Detection: Two different extraction procedures for water with sensitivities on the order of 0.01 |Jd/L and
0.1 |jg/L. Soil extraction procedure provides sensitivity on the order of 1 |jg/kg.
Performance: Mean recovery 30 - 130%
Sample Preparation: Shake and shoot isooctane or ether extraction. Solid samples may require
extraction for up to 18 hours prior to analysis.
Other: Method has been evaluated for this compound usina an NPD detector
Detection: 0.005 |Jd per sample
Quantitation: 0.5 - 5 |Jd per sample
Workina Ranae: 0.04-0.8 ma/m3 (0.0008 -0.16 com) for a 12-L air sample
Performance: Averaae recovery -106% (n=18): 0.056 - 0.24 ma/m3for 12-L samples
Sample Preparation: Extraction from sorbent tube with xvlene
Other: Limited QC for rapid analysis (e.a., an instrument blank and instrument tune, but no calibration
standards)
*SAM methods listed in this column can be located using the U.S. Environmental Protection Agency, National Homeland Security Research Center's (NHSRC), Standardized Analytical Methods for
Environmental Restoration Following Homeland Security Events (www.epa.gov/sam). SAM is intended to be used concurrently with this Rapid Screening and Preliminary Identification Techniques
and Methods document. Full citations for references not accessible through SAM are provided in Section 3.0 of this document.
Rapid Screening and Preliminary Identification Techniques and Methods
1 -69
September 2010
-------
Rapid Screening and Preliminary Identification Techniques and Methods
1 -70 September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM
Note: When available, information is provided for emission energies, expected identifiable concentration (with 20% efficiency p-type), sample preparation, and analysis time (see Comments
column).
Analyte
Matrix
Technique
Reference
Source *
Comments
Gamma Emitters
Gamma
Emitters,
General
Americium-241
(gamma emitter)
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Gamma
Spectrometry
Analysis
Gamma
Spectrometry
Analysis
EPA Method
901.1
SM Method
7120
HASL-300
Method
Ga-01-R
EPA Method
901.1
SM Method
7120
HASL-300
Method
Ga-01-R
Emission Eneraies: 50 - 2000 keV: refer to selected aamma-emittina radionuclides for isotope-specific emission
energies
Expected Identifiable Concentration (with 20% efficiency p-tvpe): See specific aamma-emittina radionuclides for
expected identifiable concentrations. Note: Identifiable concentrations in samples may vary from these published
values due to spectroscopy peak interferences from mixed radionuclides (if present) in the sample, spectroscopy
summing effects, sample volumes, and counting times.
Sample Preparation: Dependina on the sample matrix, pretreatment (e.a., arindina, sievina) may be necessary to
obtain a homogeneous sample. As much as is practical, aqueous/liquid and soil samples are loaded into a Marinelli
beaker or other calibrated geometry (e.g., "tuna can") for counting. Air filters and swipes are placed on top of the
detector, and may be retained in shipping envelope or placed in other laboratory-calibrated counting geometry
material.
Analysis Time (Counts): Samples are counted for 30 minutes: increased countina time will increase detection
sensitivity. At 30 minutes, an uncertainty of 50% at 2 sigma can be expected to provide clear delineation of the target
analyte.
Other: Perform simultaneously with Gross Alpha
Emission Eneraies: 59.4 keV (36%)
Expected Identifiable Concentration (with 20% efficiency p-type):
Air Filter: 100 - 300 pCi/sample
Aqueous/Liquid: 30 - 50 pCi/L
Drinking Water: 20 pCi/L
Soil/Sediment: 300 - 500 pCi/ kg
Wipe: 1 00 - 300 pCi/sample
Sample Preparation: See Sample Preparation for Gamma Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated in far left of center point of aamma spectrum (lower eneraies), Am-241 can be easily misidentified or
have the activity miscalculated. The peak is not properly resolved and may be shifted, preventing identification at low
concentrations.
Rapid Screening and Preliminary Identification Techniques and Methods
2-1
September 2010
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Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Gamma Emitters cont.
Cesium-137
(gamma emitter)
Cobalt-60
(gamma emitter)
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Gamma
Spectrometry
Analysis
Gamma
Spectrometry
Analysis
EPA Method
901.1
SM Method
7120
HASL-300
Method
Ga-01-R
EPA Method
901.1
SM Method
7120
HASL 300
Method
Ga-01-R
Emission Eneraies: 661 .6 keV (85%)
Expected Identifiable Concentration (with 20% efficiency p-type):
Air Filter: 100 - 300 pCi/sample
Aqueous/Liquid: 30 - 50 pCi/L
Drinking Water: 20 pCi/L (SDWA limit is 200 pCi/L)
Soil/Sediment: 300 - 500 pCi/kg
Wipe: 1 00 - 300 pCi/sample
Sample Preparation: See Sample Preparation for Gamma Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated at the left of center point of a typical aamma spectrum (50 - 2500 keV), the isotope is easily identified
and has few other isotopic energies that might interfere with the peak or result in improper identification
Emission Eneraies: 1 173 keV (100%) and 1332 keV (100%)
Expected Identifiable Concentration (with 20% efficiency p-type):
Air Filter: 100 - 300 pCi/sample
Aqueous/Liquid: 30 - 50 pCi/L
Drinking Water: 20 pCi/L (SDWA limit is 100 pCi/L)
Soil/Sediment: 100 - 300 pCi/kg
Wipe: 1 00 - 300 pCi/sample
Sample Preparation: See Sample Preparation for Gamma Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated at the riaht of center point of a typical aamma spectrum (50 - 2500 keV), the isotope is easily
identified by two distinct and relatively equal height peaks. Co-60 has few other isotopic energies that might interfere
with the peak or result in improper identification.
Rapid Screening and Preliminary Identification Techniques and Methods
2-2
September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Gamma Emitters cont.
Europium-154
(gamma emitter)
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Gamma
Spectrometry
Analysis
EPA Method
901.1
SM Method
7120
HASL-300
Method
Ga-01-R
Emission Energies: 123 keV (38%) and 1274 keV (37%)
Expected Identifiable Concentration (with 20% efficiency p-type):
Air Filter: 100 - 300 pCi/sample
Aqueous/Liquid: 30 - 50 pCi/L
Drinking Water: 20 pCi/L (SDWA limit is 60 pCi/L)
Soil/Sediment: 500 - 1000 pCi/kg
Wipe: 100 - 300 pCi/sample
Sample Preparation: See Sample Preparation for Gamma Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated at the far left of center point of a typical gamma spectrum (50 - 2500 keV) and halfway in the
spectrum, the isotope is easily identified. Eu-154 peak at 1274 keV falls at the same energy as Na-22, which is a
product of cosmic ray interactions, but is also extremely low in natural abundance. Identification can be determined
solely on the 123 keV peak, as it is the higher yield of the two peaks for the isotope and has no other interferences.
lodine-125
(gamma emitter)
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Gamma
Spectrometry
Analysis
ORISE
Procedure #9
Emission Energies: 35.49 keV (6.7%)
Expected Identifiable Concentration (with 20% efficiency p-type):
Air Filter: 100 - 300 pCi/sample
Aqueous/Liquid: 30 - 50 pCi/L
Drinking Water: 20 pCi/L (SDWA limit is 60 pCi/L)
Soil/Sediment: 500 - 1000 pCi/kg
Wipe: 100 - 300 pCi/sample
Sample Preparation: The sample is prepared by matrix-specific techniques and the final sample is placed in a 16
millimeter culture tube and counted in a 3" x 3" thin window Nal(TI) well detector attached to a pulse height analyzer.
1-125 gamma counting rate is determined in the 25 to 35 keV energy range by pulse height analysis. NIST-traceable
liquid standards are also counted in the same geometric configuration as the samples to determine 1-125 counting
efficiency.
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated at the left of center point of a typical gamma spectrum (50 - 2500 keV). Due to the low photon energy
of 1-125, the Compton scattering and x-ray photons from other radionuclides may cause significant interferences in
this procedure.
Rapid Screening and Preliminary Identification Techniques and Methods
2-3
September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Gamma Emitters cont.
lodine-131
(gamma emitter)
lridium-192
(gamma emitter)
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Gamma
Spectrometry
Analysis
Gamma
Spectrometry
Analysis
EPA Method
901.1
SM Method
7120
HASL-300
Method
Ga-01-R
EPA Method
901.1
SM Method
7120
HASL-300
Method
Ga-01-R
Emission Enerqies: 1 63.9 keV (1 .91 %) (aamma rav of Xe-1 31 m proaenv of 1-131)
Expected Identifiable Concentration (with 20% efficiency p-type):
Air Filter: 100 - 300 pCi/sample
Aqueous/Liquid: 30 - 50 pCi/L
Drinking Water: 20 pCi/L (SDWA limit is 60 pCi/L)
Soil/Sediment: 500 - 1000 pCi/kg
Wipe: 1 00 - 300 pCi/sample
Sample Preparation: See Sample Preparation for Gamma Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated at the left of center point of a typical aamma spectrum (50 - 2500 keV). Due to the low aamma
abundance of 1-131 (Xe-1 31m), longer counting times may be required to obtain positive identification. Compton
scattering and x-ray photons from other radionuclides may cause significant interferences in this procedure.
Emission Energies: 296 keV (29%), 308 keV (30%), 316 keV (83%), 468 keV (48%), 485 keV (3%), 588 keV (5%),
604 keV (8%), and 612 keV (5%)
Expected Identifiable Concentration (with 20% efficiency p-type):
Air Filter: 100 - 300 pCi/sample
Aqueous/Liquid: 30 - 50 pCi/L
Drinking Water: 20 pCi/L (SDWA limit is 100 pCi/L)
Soil: 100-300pCi/kg
Sediment: 300 - 500 pCi/kg
Wipe: 1 00 - 300 pCi/sample
Sample Preparation: See Sample Preparation for Gamma Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated at the left of center point of a typical aamma spectrum (50 - 2500 keV), the isotope is easily
identified. The peak at 296 keV falls at the same energy as Pb-214at 295 keV, and the peak at 468 keV falls at the
same energy as Rh-102m. However, the peaks at 308 and 316 keV are used in identification.
Rapid Screening and Preliminary Identification Techniques and Methods
2-4
September 2010
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Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Gamma Emitters cont.
Molybdenum-99
(gamma emitter)
Radium-226
(gamma emitter)
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Gamma
Spectrometry
Analysis
Gamma
Spectrometry
Analysis
EPA Method
901.1
SM Method
7120
HASL-300
Method
Ga-01-R
EPA Method
901.1
SM Method
7120
HASL 300
Method
Ga-01-R
Emission Eneraies: 140.51 keV(89%), 181 keV(6%), 740keV(12%)
Expected Identifiable Concentration (with 20% efficiency p-type):
Air Filter: 100 - 300 pCi/sample
Aqueous/Liquid: 30 - 50 pCi/L
Drinking Water: 20 pCi/L (SDWA limit is 100 pCi/L)
Soil: 100-300pCi/kg
Sediment: 300 - 500 pCi/kg
Wipe: 1 00 - 300 pCi/sample
Sample Preparation: See Sample Preparation for Gamma Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated at the riaht of center point of a typical aamma spectrum (50 - 2500 keV), the isotope is easily
identified. The peak at 140.51 keV falls at the same energy as Tc-99m at 140.5 keV; however, the peak at 740 keV is
generally used in identification.
Emission Eneraies: Ra-226 is primarily an alpha emitter (95%), but does have aamma peaks that result in the
remaining (5.5%) decays at 186 keV and other insignificant energies
Expected Identifiable Concentration (with 20% efficiency p-tvpe):
Air Filter: 500 - 1000 pCi/sample
Aqueous/Liquid: 3000 - 5000 pCi/L
Drinking Water: 2000 pCi/L (SDWA limit is 5 pCi/L)
Soil/Sediment: 1000 - 3000 pCi/kg
Wipe: 1 000 - 3000 pCi/sample
Sample Preparation: See Sample Preparation for Gamma Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated left of the center point of a typical aamma spectrum (50 - 2500 keV), the isotope is NOT easily
identified based on potential interferences. U-235 also has a peak at 185 keV (57.2%). Based on the capability of the
system and the concentrations of the isotopes, Ra-226 may not be clearly quantifiable; however, it may be
determined as present in the sample.
Rapid Screening and Preliminary Identification Techniques and Methods
2-5
September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Gamma Emitters cont.
Ruthenium-103
(gamma emitter)
Ruthenium-106
(gamma emitter)
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Gamma
Spectrometry
Analysis
Gamma
Spectrometry
Analysis
EPA Method
901.1
SM Method
7120
HASL-300
Method
Ga-01-R
EPA Method
901.1
SM Method
7120
HASL-300
Method
Ga-01-R
Emission Eneraies: 497 keV (88%), 557 keV (1%), and 610 keV (6%)
Expected Identifiable Concentration (with 20% efficiency p-type):
Air Filter: 100 - 300 pCi/sample
Aqueous/Liquid: 30 - 50 pCi/L
Drinking Water: 20 pCi/L (SDWA limit is 200 pCi/L)
Soil/Sediment: 100 - 300 pCi/ kg
Wipe: 1 00 - 300 pCi/sample
Sample Preparation: See Sample Preparation for Gamma Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated left of the center point of a typical aamma spectrum (50 - 2500 keV), the isotope is easily identified
with no potential interferences
Emission Enerqies: Ru-106 decays solely by a weak beta decay (39 keV). Its proaenv, Rh-106, has several aamma
peaks that can be used in analysis. These include 51 1 keV (21 %), 622 keV (1 1 %), 1 050 keV (1 .5%), 1 1 28 keV
(0.4%), and 1562 keV (0.2%).
Expected Identifiable Concentration (with 20% efficiency p-type):
Air Filter: 100 - 300 pCi/sample
Aqueous/Liquid: 30 - 50 pCi/L
Drinking Water: 20 pCi/L (SDWA limit is 30 pCi/L)
Soil/Sediment: 500 - 1000 pCi/kg
Wipe: 1 00 - 300 pCi/sample
Sample Preparation: See Sample Preparation for Gamma Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated to the left and riaht of the center point of a typical aamma spectrum (50 - 2500 keV), the isotope Rh-
106 is not easily identified. The peak at 51 1 keV (the most abundant peak at 20%) corresponds to numerous other
isotopes. The peak at 622 keV corresponds to the peak for 1-1 32, a potential fission product, which is also the means
of production for Ru-106. The peaks at 1050 keV, 1 128 keV, and 1562 keV have no known interferences but have
low yields.
Rapid Screening and Preliminary Identification Techniques and Methods
2-6
September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Gamma Emitters cont.
Selenium-75
(gamma emitter)
Uranium-235
(gamma emitter)
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Gamma
Spectrometry
Analysis
Gamma
Spectrometry
Analysis
EPA Method
901.1
SM Method
7120
HASL-300
Method
Ga-01-R
EPA Method
901.1
SM Method
7120
HASL-300
Method
Ga-01-R
Emission Enerqies: Se-175 decays bv beta decay to its proaenv, stable As-75. Se-75 has several aamma peaks that
can be used in analysis. These include 96.73 keV (3.4%), 121 .12 keV (17.2%), 136.0 keV (58.3%), 264.66 keV
(58.9%), 279.54 keV (25%), and 400.66 keV (1 1 .47%).
Expected Identifiable Concentration (with 20% efficiency p-type):
Air Filter: 100 - 300 pCi/sample
Aqueous/Liquid: 30 - 50 pCi/L
Drinking Water: 20 pCi/L (SDWA limit is 30 pCi/L)
Soil/Sediment: 500 - 1000 pCi/kg
Wipe: 1 00 - 300 pCi/sample
Sample Preparation: See Sample Preparation for Gamma Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated to the left and riaht of the center point of a typical aamma spectrum (50 - 2500 keV), the isotope Se-
75 is easily identified with the two primary peaks at 136 keV and 264.66 keV
Emission Eneraies: U-235 has peaks at 1 44 keV (1 1 %), 1 63 keV (5%), 1 85 keV (57%), 202 keV (1 %), and 205 keV
(5%)
Expected Identifiable Concentration (with 20% efficiency p-type):
Air Filter: 1000 - 3000 pCi/sample
Aqueous/Liquid: 3000 - 5000 pCi/L
Drinking Water: 2000 pCi/L (SDWA limit is 5 pCi/L)
Soil/Sediment: 1000 - 3000 pCi/kg
Wipe: 1 000 - 3000 pCi/sample
Sample Preparation: See Sample Preparation for Gamma Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Gamma Emitters, General
Other: Situated left of the center point of a typical aamma spectrum (50 - 2500 keV), the isotope is NOT easily
identified based on potential interferences and decay yields. Depending on the source and concentration of the
isotope in the sample, it may be possible to determine that the isotope is present. Pa-234, a progeny of the decay of
U-238, has gamma energies of 185 keV and 203 keV. Th-227, a progeny of U-235, has a gamma peak at 185 keV,
and lr-192 has a gamma peak at 205 keV.
Rapid Screening and Preliminary Identification Techniques and Methods
2-7
September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Alpha and Beta Emitters
Gross Alpha
and Beta
Alpha Emitters
Americium-241
Californium-252
Radium-226
Uranium-234
Uranium-235
Uranium-238
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Gas-flow
Proportional
Detector or
Solid
Scintillation
Detector
Alpha
Spectrometry
Analysis
EPA Method
900.0
SM Method
711 OB
ORISE Method
AP1
FRMAC, Vol 2,
pg.33
EPA Method
907.0
EPA Method
EMSL-19
ASTM Method
D3084-05
ORISE Method
APS
Emission Eneraies: Alpha emitters > 3.9 MeV: beta emitters > 0.1 MeV
Expected Identifiable Concentration: The expected identifiable concentration depends on sample size, countina
system characteristics, background, and counting time. See specific alpha- and beta-emitting radionuclides for
expected identifiable concentrations.
Sample Preparation: Aqueous and liquid samples are prepared bv evaporation and transfered to a planchet for final
evaporation and counting. Soil and sediment samples are dried, ground, and dispersed across the planchet for
further drying and counting. Air filters and wipes are counted as is. If the sample is larger than can be counted via a
planchet counting system, use hand-held instrument detectors.
Analysis Time (Counts): Sample is counted usina either a das-flow proportional detector or solid scintillation detector
for 30 minutes
Other: Perform simultaneously with Gamma Spectrometrv analysis for water, liquid, soil, and sediment. Perform after
Gamma Spectrometry analysis for air filters and surface wipes. Measures only gross alpha or gross beta (presence
of alpha and beta decay particles), with no isotopic determination. If alpha or beta radiation is detected, proceed to
alpha spectrum or gamma spectrum for determination of specific radioisotopes.
Emission Eneraies: Refer to selected alpha-emittina radionuclides for isotope-specific emission eneraies
Expected Identifiable Concentration:
15 pCi/L for aqueous liquids and drinking water samples (EPA 40 CFR 141.66, Alpha without Uranium and Radon)
5 pCi/g for soils and sediments (CERCLA, Ra-226 limit)
2 E-14 |jCi/mL for air filter sample (10 CFR 20 Subpart O, Appendix B, Table 2 based on most conservative value for
effluent concentrations, Pu-238 and Am-241)
220 pCi/swipe for swipe sample (49 CRF 173.443)
Sample Preparation: Dependina on the sample matrix, pretreatment (e.a., arindina, sievina) may be necessary to
obtain a homogeneous sample. The sample is processed by various chemical separation methods (e.g., acid
digestion, chemical fusion, co-precipitation, liquid-liquid extraction, ion exchange), along with method-specific
radioisotopic tracers, to isolate and extract the radioisotope(s) in their purest form. The radioisotope(s) extract is 1)
mounted as a thin layer on an appropriate alpha Spectrometry counting geometry (depending on the separation
method used) by electrodeposition, evaporation of organic solvent, or fluoride precipitation, or 2) extracted into liquid
scintillation cocktail and counted by PERALS® Spectrometry system.
Rapid Screening and Preliminary Identification Techniques and Methods
2-8
September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Alpha and Beta Emitters (cont.)
Alpha Emitters
(cont.)
Americium-241
Californium-252
Radium-226
Uranium-234
Uranium-235
Uranium-238
Beta Emitter
Strontium-90
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Aqueous/Liquid
Drinking Water
Alpha
Spectrometry
Analysis
Beta Counting
EPA Method
907.0
EPA Method
EMSL-19
ASTM Method
D3084-05
ORISE Method
APS
SM Method
7500-Sr B
HASL-300
Method
Sr-03-RC
Analysis Time (Counts): Samples are counted, dependina on the sample activity, for a sufficient lenath of time
(generally one to eight hours) to provide clear delineation of the target nuclide(s) and/or tracer, and to ensure good
alpha peak resolution (Full Width Half-Maximum) of approximately: 20 - 50 keV for electrodeposited and organically
evaporated samples by alpha spectrometry, 25 - 200 keV for precipitated samples by alpha spectrometry, and 400 -
500 keVfor liquid scintillation counted samples. Sample count may be stopped at anytime if clear evidence is
obtained as to the isotope or tracer present in the sample with well resolved peak(s); increased counting time will
increase detection sensitivity.
Other: Usina aross alpha detection, if results are computed as alpha activity areater than shown for expected
identifiable concentration, analyze sample with alpha spectrum analysis
Emission Eneraies: 195.8 keV
Expected Identifiable Concentration: The expected identifiable concentration depends on sample size, countina
system characteristics, background, and counting time
Sample Preparation: Aqueous and liquid samples are prepared by addina a known amount of inactive strontium ions
(e.g., Sr(NO3)2) 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 Sr(NO3)2 from fuming nitric acid solution. The
strontium carrier, together with the radionuclides of strontium, finally is precipitated as SrCO3, which is dried, weighed
to determine recovery of carrier, and measured for radioactivity. The activity in the final precipitate is due to
radioactive strontium only, because all other radioactive elements have been removed. A correction is applied to
compensate for losses of carrier and activity during the various purification steps.
Analysis Time (Counts): Sample is counted usina a das-flow proportional detector for 60 minutes. Increased countina
time will increase detection sensitivity.
Other: Radioactive barium (Ba-140, La-140) interferes in the determination of radioactive strontium inasmuch as it
precipitates with the radioactive strontium. Eliminate this interference by adding inactive barium nitrate as carrier and
separating this from the strontium by precipitating barium chromate in acetate buffer solution. Radium isotopes also
are eliminated by this treatment. In hard water, some calcium nitrate may be coprecipitated with strontium nitrate and
can cause errors in recovery of the final precipitate and in measuring its activity. Eliminate this interference by
repeated precipitations of strontium as the nitrate followed by leaching the strontium nitrate with acetone. CAUTION:
For total radiostrontium, count the precipitate within three to four hours after the final separation and before ingrowth
ofY-90.
Rapid Screening and Preliminary Identification Techniques and Methods
2-9
September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Alpha and Beta Emitters cont.
Beta Emitter
Strontium-90
Air Filters
Soil and
Sediment
Surface Wipes
Beta Counting
HASL-300
Method
Sr-03-RC
Emission Energies: 195.8 keV
Expected Identifiable Concentration: The expected identifiable concentration depends on sample size, counting
system characteristics, background, and counting time
Sample Preparation: Strontium is separated from Ca, other fission products, and natural radioactive elements.
Fuming nitric acid separations removes the Ca and most other interfering ions. Ra, Pb, and Ba are removed with
barium chromate. Traces of other fission products are scavenged with iron hydroxide. After Sr-90 and Y-90
equilibrium has been attained, Y-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 Sr-85 tracer by counting in a gamma
well detector.
Analysis Time (Counts): Sample is counted using a gas-flow proportional detector for 60 minutes. Increased counting
time will increase detection sensitivity
Technetium-99
Aqueous/Liquid
Drinking Water
Liquid
Scintillation
HASL-300
Method
Tc-02-RC
Emission Energies: 84.6 keV
Expected Identifiable Concentration: The expected identifiable concentration depends on sample size, counting
system characteristics, background, and counting time
Sample Preparation: The sample containing Tc-99 is mixed with Tc-95m added as a gamma-emitting tracer. The two
isotopes of Tc are brought to an isotopic equilibrium and separated from other elements by ferrous and ferric
hydroxide coprecipitation. The precipitate is dissolved with dilute nitric acid and passed through a commercially
available resin column (TEVA® resin) which is highly specific for Tc in the pertechnetate form. The resin is washed
with dilute nitric acid to remove possible interferences and then it is extruded directly into a suitable liquid scintillation
cocktail.
Analysis Time (Counts): The sample is typically counted for one hour to simultaneously determine Tc-99 activity and
the Tc-95m radiochemical yield. Quench/efficiency calibration curves need to be established for the liquid scintillation
spectrometer for both Tc-95m and Tc-99.
Other: Tritium may follow technetium due to the absorption of some tritium-labeled compounds by the resin. Possible
tritium interferences are eliminated by setting the Tc counting window above the maximum energy of tritium beta
particles.
Rapid Screening and Preliminary Identification Techniques and Methods
2-10
September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Alpha and Beta Emitters cont.
Technetium-99
Air Filters
Soil and
Sediment
Surface Wipes
Liquid
Scintillation
ORISE Method
APS
Emission Energies: 84.6 keV
Expected Identifiable Concentration: The expected identifiable concentration depends on sample size, counting
system characteristics, background, and counting time
Sample Preparation: Solid samples are leached with dilute nitric acid. The leachates are passed through a
commercially-available resin column (TEVA® resin) which is highly specific for Tc in the pertechnetate form. The Tc
is absorbed onto the extraction resin. The resin is added to a scintillation vial containing an appropriate cocktail and
counted using a liquid scintillation analyzer. Most interfering beta emitting radionuclides (including C-14, P-32, S-35,
Sr-90, Y-90, and Th-234) are effectively removed using TEVA® resin under the conditions in this procedure.
Analysis Time (Counts): The sample is typically counted for one hour to determine the Tc-99 activity.
Quench/efficiency calibration curve needs to be established for the liquid scintillation spectrometer for Tc-99.
Other: Tritium may follow technetium due to the absorption of some tritium-labeled compounds by the resin. Possible
tritium interferences are eliminated by setting the Tc counting window above the maximum energy of tritium beta
particles.
Tritium
(Hydrogen-3)
Aqueous/Liquid
Drinking Water
Liquid
Scintillation
EPA Method
906.0
Emission Energies: 18.59 keV
Expected Identifiable Concentration: The expected identifiable concentration depends on sample size, counting
system characteristics, background, and counting time
Sample Preparation: An unpreserved 100-mL aliquot of a drinking water sample is distilled after adjusting pH with a
small amount of sodium hydroxide and adding potassium permanganate. The alkaline treatment prevents other
radionuclides, such as radioiodine and radiocarbon, from distilling with the tritium. The permanganate treatment
oxidizes trace organics that may be present in the sample and prevents their appearance in the distillate. To
determine the concentration of tritium, the middle fraction of the distillate is used, because the early and late fractions
are more apt to contain materials interfering with the liquid scintillation counting process. A portion of this collected
fraction is added to a liquid scintillator cocktail, and the solution is mixed, dark adapted, and counted for beta particle
activity. The efficiency of the system can be determined by the use of prepared tritiated water standards having the
same density and color as the sample.
Analysis Time (Counts): The sample is typically counted for one hour using a liquid scintillation spectrometer.
Increased counting time will increase detection sensitivity.
Other: Other beta emitters may follow tritium during the distillation process and interfere with the measurement.
Possible interferences are eliminated by setting the tritium counting window below the energies of the interfering beta
particles from C-14, Tc-99, etc.
Rapid Screening and Preliminary Identification Techniques and Methods
2-11
September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Alpha and Beta Emitters cont.
Tritium
(Hydrogen-3)
(cont.)
Beta and
Gamma
Emitters
Cobalt-60
Cesium-137
Europium-154
lodine-131
lridium-192
Molybdenum-99
Ruthenium-103
Ruthenium-106
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Liquid
Scintillation
Gamma
Spectrometry
Analysis and
Gross Beta
ORISE Method
AP2
EPA Method
900.0
EPA EMSL
Method
LV 0539 17
ORISE Method
AP1
Emission Enerqies: 18.59 keV
Expected Identifiable Concentration: The expected identifiable concentration depends on sample size, countina
system characteristics, background, and counting time
Sample Preparation: For solid samples, an appropriate volume of water is added to facilitate distillation. Certain solid
samples may be refluxed to ensure distribution of any tritium that may be in the sample. The sample may be spiked
with a standard tritium solution to evaluate quenching and counting efficiency. After the sample has been distilled, an
aliquot of the distillate is added to a scintillation cocktail and the sample is counted using a liquid scintillation
analyzer.
Analysis Time (Counts): The sample is typically counted for 90 minutes usina a liquid scintillation spectrometer.
Increased counting time will increase detection sensitivity.
Other: Other volatile radionuclides such as iodine and carbon isotopes may interfere and may require that the
sample be made alkaline using solid sodium hydroxide before distillation. Organic impurities may interfere and may
require the addition of an oxidizing agent to the sample as well as spiking the samples with a standard tritium
solution. The addition of a standard tritium solution to each sample allows for counting efficiencies to be calculated
for each individual sample.
Emission Eneraies: Refer to specific aamma-emittina radionuclides for isotope-specific emission eneraies
Expected Identifiable Concentration (with 20% efficiency p-tvpe):
8 pCi/L for aqueous and drinking water samples (NBS Handbook, Edition 69, Strontium-90)
30 pCi/L for aqueous liquids and drinking water samples (NBS Handbook, Edition 69, Ruthenium-106)
5 pCi/g for soils and sediments (CERCLA, Ra-226 limit)
6 E-12 |jCi/mL for air filter sample (10 CFR 20 Subpart O, Appendix B, Table 2 based on most conservative value for
effluent concentrations, Strontium-90)
220 pCi/swipe for swipe sample (49 CFR 1 173.443)
Sample Preparation: See sample preparation for Gamma Emitters, General
Analysis Time (Counts): See analysis time (counts) for Gamma Emitters, General
Rapid Screening and Preliminary Identification Techniques and Methods
2-12
September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Alpha Emitters
Alpha Emitters,
General
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Alpha
Spectrometry
Analysis
EPA Method
907.0
EPA Method
EMSL-19
ASTM Method
D3084-05
Emission Energies: Refer to specific alpha-emitting radionuclides for isotope-specific emission energies
Expected Identifiable Concentration: The expected identifiable concentration depends on sample size, counting
system characteristics, background, and counting time. See specific alpha-emitting radionuclides for expected
identifiable concentrations.
Sample Preparation: Depending on the sample matrix, pretreatment (e.g., grinding, sieving) may be necessary to
obtain a homogeneous sample. The sample is processed by various chemical separation methods (e.g., acid
digestion, chemical fusion, co-precipitation, liquid-liquid extraction, ion exchange), along with method-specific
radioisotopic tracers, to isolate and extract the radioisotope(s) in their purest form. The radioisotope(s) extract is 1)
mounted as a thin layer on an appropriate alpha spectrometry counting geometry (depending on the separation
method used) by electrodeposition, evaporation of organic solvent, or fluoride precipitation, or 2) extracted into liquid
scintillation cocktail and counted by PERALS® spectrometry system.
Analysis Time (Counts): Samples are counted, depending on the sample activity, for a sufficient length of time
(generally one to eight hours) to provide clear delineation of the target nuclide(s) and/or tracer, and to ensure good
alpha peak resolution (Full Width Half-Maximum) of approximately: 20 - 50 keV for electrodeposited and organically
evaporated samples by alpha spectrometry, 25 - 200 keV for precipitated samples by alpha spectrometry, and 400 -
500 keVfor liquid scintillation counted samples. Sample count may be stopped at anytime if clear evidence is
obtained as to the isotope or tracer present in the sample with well-resolved peak(s); increased counting time will
increase detection sensitivity.
Other: Perform alpha spectrometry upon positive identification of gross alpha at greater than 30 pCi/L (water), 5
pCi/g (soil or sediment), or 2.0 E-8 |jCi/ml_ (air filter or wipe). Requires experience in determination of multiple peak
alpha analysis. It is assumed that if only one isotope is present, it will be apparent. Any sample that produces multiple
peaks and has multiple isotopes identified should have the spectrum sent to EPA ORIA or a designated laboratory
for definitive examination.
Americium-241
(alpha emitter)
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Alpha
Spectrometry
Analysis
EPA Method
907.0
EPA Method
EMSL-19
ASTM Method
D3084-05
Emission Energies: 5.486 MeV (85%) and 5.443 MeV (13%)
Expected Identifiable Concentration: The expected identifiable concentration to which this method is applicable
depends on sample size, counting system characteristics, background, and counting time
Sample Preparation: See Sample Preparation for Alpha Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Alpha Emitters, General
Rapid Screening and Preliminary Identification Techniques and Methods
2-13
September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Alpha Emitters (cont.)
Californium-252
(alpha emitter)
Curium-244
(alpha emitter)
Plutonium-238
(alpha emitter)
Plutonium-239
(alpha emitter)
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Alpha
Spectrometry
Analysis
Alpha
Spectrometry
Analysis
Alpha
Spectrometry
Analysis
Alpha
Spectrometry
Analysis
EPA Method
907.0
EPA Method
EMSL-19
ASTM Method
D3084-05
EPA Method
907.0
EPA Method
EMSL-19
ASTM Method
D3084-05
EPA Method
907.0
EPA Method
EMSL-19
ASTM Method
D3084-05
EPA Method
907.0
EPA Method
EMSL-19
ASTM Method
D3084-05
Emission Eneraies: 6.1 18 MeV (84%) and 6.076 MeV (16%)
Expected Identifiable Concentration: The expected identifiable concentration to which this method is applicable
depends on sample size, counting system characteristics, background, and counting time
Sample Preparation: See Sample Preparation for Alpha Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Alpha Emitters, General
Emission Eneraies: 5.805 MeV (76%) and 5.763 MeV (24%)
Expected Identifiable Concentration: The expected identifiable concentration to which this method is applicable
depends on sample size, counting system characteristics, background, and counting time
Sample Preparation: See Sample Preparation for Alpha Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Alpha Emitters, General
Emission Eneraies: 5.499 MeV (72%) and 5.456 MeV (28%)
Expected Identifiable Concentration: The expected identifiable concentration to which this method is applicable
depends on sample size, counting system characteristics, background, and counting time
Sample Preparation: See Sample Preparation for Alpha Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Alpha Emitters, General
Emission Eneraies: 5.156 MeV (71%), 5.143 MeV (17%), and 5.105 MeV (12%)
Expected Identifiable Concentration: The expected identifiable concentration to which this method is applicable
depends on sample size, counting system characteristics, background, and counting time
Sample Preparation: See Sample Preparation for Alpha Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Alpha Emitters, General
Rapid Screening and Preliminary Identification Techniques and Methods
2-14
September 2010
-------
Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Alpha Emitters (cont.)
Polonium-210
(alpha emitter)
Radium-226
(alpha emitter)
Uranium-234
(alpha emitter)
Uranium-235
(alpha emitter)
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Alpha
Spectrometry
Analysis
Alpha
Spectrometry
Analysis
Alpha
Spectrometry
Analysis
Alpha
Spectrometry
Analysis
HASL-300
Method
Po-02-RC
EPA Method 1 1 1
ORISE Method
AP7
EPA Method
EMSL-19
ASTM Method
D3084-05
EPA Method
907.0
EPA Method
EMSL-19
ASTM Method
D3084-05
EPA Method
907.0
EPA Method
EMSL-19
ASTM Method
D3084-05
Emission Enerqies: 5.305 MeV
Expected Identifiable Concentration: The expected identifiable concentration to which this method is applicable
depends on sample size, counting system characteristics, background, and counting time
Sample Preparation: See Sample Preparation for Alpha Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Alpha Emitters, General
Emission Eneraies: 4.782 MeV (95%) and 4.599 MeV (5%)
Expected Identifiable Concentration: The expected identifiable concentration to which this method is applicable
depends on sample size, counting system characteristics, background, and counting time
Sample Preparation: See Sample Preparation for Alpha Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Alpha Emitters, General
Emission Eneraies: 4.774 MeV (71%) and 4.722 MeV (28%)
Expected Identifiable Concentration: The expected identifiable concentration to which this method is applicable
depends on sample size, counting system characteristics, background, and counting time
Sample Preparation: See Sample Preparation for Alpha Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Alpha Emitters, General
Emission Eneraies: 4.397 MeV (55%), 4.366 MeV (17%), 4.214 MeV (6%), and 4.596 MeV (5%)
Expected Identifiable Concentration: The expected identifiable concentration to which this method is applicable
depends on sample size, counting system characteristics, background, and counting time
Sample Preparation: See Sample Preparation for Alpha Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Alpha Emitters, General
Rapid Screening and Preliminary Identification Techniques and Methods
2-15
September 2010
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Table 2: Rapid Screening and Preliminary Identification Techniques and Methods for the Radiochemical Analytes Listed in SAM (cont.)
Analyte
Matrix
Technique
Reference
Source *
Comments
Alpha Emitters cont.
Uranium-238
(alpha emitter)
Air Filters
Aqueous/Liquid
Drinking Water
Soil and
Sediment
Surface Wipes
Alpha
Spectrometry
Analysis
EPA Method
907.0
EPA Method
EMSL-19
ASTM Method
D3084-05
Emission Eneraies: 4.200 MeV (77%) and 4.1 15 MeV (23%)
Expected Identifiable Concentration: The expected identifiable concentration to which this method is applicable
depends on sample size, counting system characteristics, background, and counting time
Sample Preparation: See Sample Preparation for Alpha Emitters, General
Analysis Time (Counts): See Analysis Time (Counts) for Alpha Emitters, General
*SAM methods listed in this column can be located using the U.S. Environmental Protection Agency, National Homeland Security Research Center's (NHSRC), Standardized Analytical
Methods for Environmental Restoration Following Homeland Security Events (www.epa.gov/sam). SAM is intended to be used concurrently with this Rapid Screening and Preliminary
Identification Techniques and Methods document. Full citations for references not accessible through SAM are provided in Section 3.0 of this document.
Rapid Screening and Preliminary Identification Techniques and Methods
2-16
September 2010
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United States
Environmental Protection
Agency
PRESORTED STANDARD
POSTAGE & FEES PAID
EPA
PERMIT NO. G-35
Office of Research and Development
National Homeland Security Research Center
Cincinnati, OH 45268
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