United States
Environmental Protection
Agency
Office of
Solid Waste and
Emergency Response
OSWER Document 9200.5-171-FS
EPA Publication 540-FS-07-001
August 2007
Multi-Media, Multi-Concentration,
Organic Analytical Service for
Superfund (SOM01.2)
Office of Superfund Remediation and Technology Innovation (OSRTI)
Analytical Services Branch (ASB) (5203P)
Quick Reference Fact Sheet
Under the legislative authority granted to the U.S. Environmental Protection Agency (EPA) under the Comprehensive
Environmental Response, Compensation, and Liability Act of 1980 (CERCLA) and the Superfund Amendments and
Reauthorization Act of 1986 (SARA), EPA develops standardized analytical methods for the measurement of various
pollutants in environmental samples from known or suspected hazardous waste sites. Among the pollutants that are of
concern to the EPA at such sites are a series of volatile, semivolatile, pesticide, and Aroclor compounds that are analyzed
using gas chromatography coupled with mass spectrometry (GC/MS) and gas chromatography with an electron capture
detector (GC/ECD). The Analytical Services Branch (ASB) of the Office of Superfund Remediation and Technology
Innovation (OSRTI) offers an analytical service that provides data from the analysis of water and soil/sediment samples for
organic compounds for use in the Superfund decision-making process. Through a series of standardized procedures and a
strict chain-of-custody, the organic analytical service produces data of known and documented quality. This service is
available through the Superfund Contract Laboratory Program (CLP).
DESCRIPTION OF SERVICES
This new organic analytical service provides a technical
and contractual framework for laboratories to apply
EPA/CLP analytical methods for the isolation, detection,
and quantitative measurement of 52 volatile, 67
semivolatile, 21 pesticide, and 9 Aroclor target
compounds in water and soil/sediment environmental
samples. The CLP provides the methods to be used and
the specific technical, reporting, and contractual
requirements, including Quality Assurance (QA), Quality
Control (QC), and Standard Operating Procedures
(SOPs), by which EPA evaluates the data. This service
uses GC/MS and GC/ECD methods to analyze the target
compounds.
Three data delivery turnarounds are available to CLP
customers: 7-day, 14-day, and 21-day turnaround after
laboratory receipt of the last sample in the set. In addition,
there are 48-hour (for trace volatiles and volatiles) and
72-hour (for semivolatiles, pesticides, and Aroclors)
preliminary data submission options available. Options
under this service include a closed system purge-and-trap
method for low-level volatile soil analysis and methanol
preservation for medium-level volatile soil analysis. In
addition, data users may request modifications to the
SOW that may include, but are not limited to, additional
compounds, sample matrices other than soil/sediment or
water, lower quantitation limits, and other requirements to
enhance method performance.
DATA USES
This analytical service provides data which EPA uses for
a variety of purposes, such as determining the nature and
extent of contamination at a hazardous waste site,
assessing priorities for response based on risks to human
health and the environment, determining appropriate
cleanup actions, and determining when remedial actions
are complete. The data may be used in all stages in the
investigation of a hazardous waste site including, but not
limited to: site inspections; Hazard Ranking System
(HRS) scoring; remedial investigations/Feasibility Studies
(FSs); remedial design; treatability studies; and removal
actions. In addition, this service provides data that will be
available for use in Superfund enforcement/litigation
activities.
TARGET COMPOUNDS
Table 1 lists the compounds for which this service is
applicable and the corresponding quantitation limits.
Specific quantitation limits are highly matrix-dependent.
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Table 1. Target Compound List (TCL) and Contract Required Quantitation Limits (CRQLs) for SOM01.2*
VOLATILES
1 . Dichlorodifluoromethane
2. Chloromethane
3. Vinyl Chloride
4. Bromomethane
5. Chloroethane
6. Trichlorofluoromethane
7. 1,1-Dicholoroethene
8. l,l,2-Trichloro-l,2,2-tnfluoroethane
9. Acetone
10. Carbon Disulfide
1 1 . Methyl acetate
12. Methylene chloride
13. trans-l,2-Dichloroethene
14. Methyl tert-butyl ether
15. 1,1-Dichloroethane
16. cis-l,2-Dichloroethene
17. 2-Butanone
18. Bromochloromethane
19. Chloroform
20. 1,1,1-Tnchloroethane
21. Cyclohexane
22. Carbon tetrachloride
23. Benzene
24. 1 ,2-Dichloroethane
25. 1,4-Dioxane
26. Trichloroethene
27. Methylcyclohexane
28. 1 ,2-Dichloropropane
29. Bromodichloromethane
30. cis-l,3-Dichloropropene
31. 4-Methyl-2-pentanone
32. Toluene
33. trans-l,3-Dichloropropene
34. 1,1,2-Tnchloroethane
35. Tetrachloroethene
36. 2-Hexanone
37. Dibromochloromethane
38. 1,2-Dibromoethane
39. Chlorobenzene
Quantitation Limits
Trace
Water
by Trace
SIM Water
(Ug/L) (ug/L)
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
5.0
0.50
0.50
0.50
0.50
0.50
0.50
0.50
5.0
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
5.0
0.50
0.50
0.50
0.50
5.0
0.50
0.050 0.50
0.50
Low
Water
(«g/L)
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
10
5.0
5.0
5.0
5.0
5.0
5.0
5.0
10
5.0
5.0
5.0
5.0
5.0
5.0
5.0
100
5.0
5.0
5.0
5.0
5.0
10
5.0
5.0
5.0
5.0
10
5.0
5.0
5.0
*For volatiles, quantitation limits for medium soils are approximately 50 times
quantitation limits for low soils.
Low
Soil
(ug/kg)
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
10
5.0
5.0
5.0
5.0
5.0
5.0
5.0
10
5.0
5.0
5.0
5.0
5.0
5.0
5.0
100
5.0
5.0
5.0
5.0
5.0
10
5.0
5.0
5.0
5.0
10
5.0
5.0
5.0
Med.
Soil
(ug/kg)
250
250
250
250
250
250
250
250
500
250
250
250
250
250
250
250
500
250
250
250
250
250
250
250
5000
250
250
250
250
250
500
250
250
250
250
500
250
250
250
Quantitation Limits
VOLATILES (CON'T)
40. Ethylbenzene
41 . o-Xylene
42. m, p-Xylene
43. Styrene
44. Bromoform
45. Isopropylbenzene
46. 1,1,2,2-Tetrachloroethane
47. 1,3-Dichlorobenzene
48. 1 ,4-Dichlorobenzene
49. 1 ,2-Dichlorobenzene
50. l,2-Dibromo-3-chloropropane
51. 1 ,2,4-Trichlorobenzene
52. 1,2,3-Trichlorobenzene
SEMIVOLATILES
53. Benzaldehyde
54. Phenol
55. bis-(2-chloroethyl) ether
56. 2-Chlorophenol
57. 2-Methylphenol
58. 2,2'-Oxybis (1 -chloropropane)
59. Acetophenone
60. 4-Methylphenol
61. N-Nitroso-di-n propylamine
62. Hexachloroethane
63. Nitrobenzene
64. Isophorone
65. 2-Nitrophenol
66. 2,4-Dimethylphenol
67. Bis (2-chloroethoxy) methane
68. 2,4-Dichlorophenol
69. Napthalene
70. 4-Chloroamlme
71 . Hexachlorobutadiene
72. Caprolactam
73. 4-Chloro-3-methylphenol
74. 2-Methylnapthalene
75. Hexachlorocyclo-pentadiene
76. 2,4,6-Trichlorophenol
77. 2,4,5-Tnchlorophenol
Trace
Water
by
SIM
("g/L)
0.050
Low
Water
by
SIM
("g/L)
0.10
0.10
Trace
Water
(Mg/L)
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
Low
Water
(Mg/L)
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
the quantitation limits for low soils. For semivolatile medium soils, quantitation
Low
Water
(Mg/L)
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
Low
Soil by
SIM
(Hi/kg)
3.3
3.3
Low
Soil
(fig/kg)
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
Low
Soil
(fig/kg)
170
170
170
170
170
170
170
170
170
170
170
170
170
170
170
170
170
170
170
170
170
170
170
170
170
limits are approximately
Med.
Soil
(Mg/kg)
250
250
250
250
250
250
250
250
250
250
250
250
250
Med.
Soil
(Mg/kg)
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
30 times the
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Table 1. Target Compound List (TCL) and Contract Required Quantitation Limits (CRQLs) for SOM01.2* (Con't)
Quantitation Limits
SEMIVOLATILES fCON'Tl
78. l.l'-Brphenyl
79. 2-Chloronapthalene
80. 2-Nitroaniline
81. Dimethylphthalate
82. 2,6-Dinitrotoluene
83. Acenaphthylene
84. 3-Nitroaniline
85. Acenaphthene
86. 2,4-Dinitrophenol
87. 4-Nitrophenol
88. Dibenzofuran
89. 2,4-Dimtrotoluene
90. Diethylphthalate
91. Fluorene
92. 4-Chlorophenyl-phenyl ether
93. 4-Nitroaniline
94. 4,6-Dinitro-2-methylphenol
95. N-Nitrosodiphenylamine
96. 1,2,4,5-Tetrachlorobenzene
97. 4-Bromophenyl-phenylether
98. Hexachlorobenzene
99. Atrazine
100. Pentachlorophenol
101. Phenanthrene
102. Anthracene
103. Carbazole
104. Di-n-butylphthalate
105. Fluoranthene
106. Pyrene
107. Butylbenzylphthalate
108. 3,3'-Dichlorobenzidme
109. Benzo (a) anthracene
110. Chrysene
1 1 1 . Bis (2-ethylhexyl) phthalate
112. Di-n-octylphthalate
113. Benzo (b) fluoroanthene
114. Benzo (k) fluoroanthene
* For volatiles, quantitation limits
quantitation limits for low soils.
Low
Water
by
SIM
(«g/L)
0.10
0.10
0.10
0.20
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.10
for medium soils are
Low
Water
("g/L)
5.0
5.0
10
5.0
5.0
5.0
10
5.0
10
10
5.0
5.0
5.0
5.0
5.0
10
10
5.0
5.0
5.0
5.0
5.0
10
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
approx
Low
Soil by Low
SIM Soil
(ug/kg) (ug/kg)
170
170
330
170
170
3.3 170
330
3.3 170
330
330
170
170
170
3.3 170
170
330
330
170
170
170
170
170
6.7 330
3.3 170
3.3 170
170
170
3.3 170
3.3 170
170
170
3.3 170
3.3 170
170
170
3.3 170
3.3 170
Med.
Soil
("g/kg)
5000
5000
10000
5000
5000
5000
10000
5000
10000
10000
5000
5000
5000
5000
5000
10000
10000
5000
5000
5000
5000
5000
10000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
5000
Quantitation Limits
SEMIVOLATILES fCON'Tl
115. Benzo (a) pyrene
116. Indeno (l,2,3-cd)-pyrene
117. Dibenzo (a,h)-anthracene
118. Benzo (g,h,i) perylene
119. 2,3,4,6-Tetrachlorophenol
PESTICIDES
120. alpha-BHC
121.beta-BHC
122. delta-BHC
123. gamma-BHC (Lmdane)
124. Heptachlor
125. Aldrm
126. Heptachlor epoxide
127. Endosulfan I
128. Dieldrm
129. 4,4'-DDE
130. Endrm
131. Endosulfan II
132. 4-4'-DDD
133. Endosulfan sulfate
134. 4-4'-DDT
135. Methoxychlor
136. Endrinketone
137. Endrin aldehyde
138. alpha-Chlordane
139. gamma-Chlordane
140. Toxaphene
AROCLORS
141. Aroclor-1016
142. Aroclor-1221
143. Aroclor-1232
144. Aroclor-1242
145. Aroclor-1248
146. Aroclor-1254
147. Aroclor-1260
148. Aroclor-1262
149. Aroclor-1268
Low
Water
by Low
SIM Water
(ug/L) (ug/L)
0.10 5.0
0.10 5.0
0.10 5.0
0.10 5.0
5.0
Water (ug/L)
0.050
0.050
0.050
0.050
0.050
0.050
0.050
0.050
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.50
0.10
0.10
0.050
0.050
5.0
Water (ug/L)
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
mately 50 times the quantitation limits for low soils. For semivolatile medium soils, quantitation
Low
Soil by Low
SIM Soil
(ug/kg) (ug/kg)
3.3 170
3.3 170
3.3 170
3.3 170
170
Soil (ug/kg)
1.7
1.7
1.7
1.7
1.7
1.7
1.7
1.7
3.3
3.3
3.3
3.3
3.3
3.3
3.3
17
3.3
3.3
1.7
1.7
170
Soil (ug/kg)
33
33
33
33
33
33
33
33
33
limits are approximately 30
Med.
Soil
("g/kg)
5000
5000
5000
5000
5000
times the
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The TCL for this service was originally derived from the
EPA Priority Pollutant List of 129 compounds. In the
years since the inception of the CLP, compounds have
been added to and removed from the TCL, based on
advances in analytical methods, evaluation of method
performance data, and the needs of the Superfund
program. The SOM analytical service combines the
previous OLM and OLC services into one method. For
example, drinking water and ground water type samples
may be analyzed using the Trace Volatiles method in
SOM.
METHODS AND INSTRUMENTATION
For trace volatile water samples, 25 mL of water sample
is added to a purge-and-trap device and purged with an
inert gas at room temperature. For low/medium volatile
water samples, 5 mL of water sample is added to a
purge-and-trap device and purged with an inert gas at
room temperature. Higher purge temperatures may be
used for both trace and low/medium volatile analyses if
all technical acceptance criteria is met for all standards,
samples, and blanks. For low-level volatile soil samples,
organic compounds are generally determined by
analyzing approximately 5 g of sample in a closed-
system purge-and-trap device at 40 °C. For a medium-
level soil sample, a soil sample of 5 g is collected,
preserved, and/or extracted with methanol and an aliquot
of methanol extract is added to 5 mL reagent water and
purged at room temperature. For water and soil samples,
the volatiles purged from the sample are trapped on a
solid sorbent. The purged volatiles are subsequently
desorbed by rapidly heating and backflushing with
helium, and then introduced into a GC/MS system.
For semivolatile, pesticide, and Aroclor water samples, a
1 L aliquot of sample is extracted with methylene
chloride using a continuous liquid-liquid extractor or
separatory funnel (for pesticides and Aroclors only). For
low-level semivolatile, pesticide, and Aroclor soil
samples, a 30 g soil/sediment sample is extracted with
methylene chloride/acetone using sonication, automated
Soxhlet/Dean-Stark (SDS) extraction, or pressurized
fluid extraction techniques. For medium-level
semivolatile soil samples, a Ig aliquot is extracted with
methylene chloride using the techniques mentioned
above for low-level soil samples. For both water and soil
samples, the extract is concentrated, subjected to
fraction-specific cleanup procedures, and analyzed by
GC/MS for semivolatiles or GC/ECD for pesticides and
Aroclors. Table 2 summarizes the methods and
instruments used in this analytical service.
DATA DELIVERABLES
Data deliverables for this service include hardcopy data
reporting forms and supporting raw data. In addition to
the hardcopy deliverable, contract laboratories must also
submit the same data electronically. The laboratory must
submit data to EPA within 7, 14, or 21-days after
laboratory receipt of the last sample in set [or
preliminary data within 48 hours (for trace volatiles and
volatiles) or 72 hours (for semivolatiles, pesticides, and
Aroclors)] after laboratory receipt of each sample. EPA
then processes the data through an automated Data
Assessment Tool (DAT). DAT provides EPA Regions
with PC-compatible reports, spreadsheets, and electronic
files within 24-48 hours from the receipt of the data for
use in data validation. This automated tool also facilitates
the transfer of analytical data into Regional databases. In
addition to the Regional electronic reports, the CLP
laboratories are provided with a data assessment report
that documents the instances of noncompliance. The
laboratory has 6 business days to reconcile defective data
and resubmit the data to EPA. EPA then reviews the data
for noncompliance and sends a final data assessment
report to the CLP laboratory and the Region.
QUALITY ASSURANCE (QA)
The QA process consists of management review and
oversight at the planning, implementation, and
completion stages of the environmental data collection
activity. This process ensures that the data provided are
of known and documented quality.
During the implementation of the data collection effort,
QA activities ensure that the Quality Control (QC)
system is functioning effectively and that the deficiencies
uncovered by the QC system are corrected. After
environmental data are collected, QA activities focus on
assessing the quality of data to determine its suitability to
support enforcement or remedial decisions.
Each contract laboratory prepares a Quality Assurance
Plan (QAP) with the objective of providing sound
analytical chemical measurements. The QAP must
specify the policies, organization, objectives, and
functional guidelines, as well as the QA and QC
activities designed to achieve the data quality
requirements in the contract.
QUALITY CONTROL (QC)
The QC process includes those activities required during
analytical data collection to produce data of known and
documented quality. The analytical data acquired from
QC procedures are used to estimate and evaluate the
analytical results and to determine the necessity for, or
the effect of, corrective action procedures. The QC
procedures required for this analytical service are
provided in Table 3.
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Table 2. Methods and Instruments
Fraction
Trace Volatiles
Volatiles
Semivolatiles
Pesticides
Aroclors
Water
Purge-and-trap followed by GC/MS analysis
Purge-and-trap followed by GC/MS analysis
Continuous liquid-liquid extraction (CLLE)
followed by GC/MS analysis
CLLE or separatory funnel extraction
followed by dual column GC/ECD analysis
CLLE or separatory funnel extraction
followed by dual column GC/ECD analysis
Soil
N/A
Purge-and-trap or closed-system purge-and-trap
followed by GC/MS analysis
Sonication, automated SDS extraction, or pressurized
fluid extraction followed by GC/MS analysis
Sonication, automated SDS extraction or pressurized
fluid extraction followed by dual column GC/ECD
analysis
Sonication, automated SDS extraction or pressurized
fluid extraction followed by dual column GC/ECD
analysis
Table 3. Quality Control (QC)
QC Operation
Deuterated Monitoring Compounds (DMCs)
(trace volatiles, volatiles, and semivolatiles)
Surrogates
(pesticides and Aroclors)
Method Blanks
(trace volatiles and volatiles)
Method Blanks
(semivolatiles, pesticides, and Aroclors)
Instrument Blank
(trace volatiles and volatiles)
Instrument Blank
(pesticides and Aroclors)
Storage Blanks
(trace volatiles and volatiles)
GC/MS Mass Calibration and Ion Abundance
Patterns (trace volatiles, volatiles, and
semivolatiles)
GC Resolution Check
(pesticides)
Initial Calibration
Continuing Calibration
Internal Standards
(trace volatiles, volatiles, and semivolatiles)
Matrix Spike and Matrix Spike Duplicate
(MS/MSD)
Laboratory Control Samples (LCSs)
(pesticides and Aroclors)
Method Detection Limit (MDL)
Frequency
Added to each sample, standard, and blank
Added to each sample, standard, and blank
Analyzed at least every 12 hours for each matrix and level
Prepared with each group of 20 samples or less of same matrix and
level, or each time samples are extracted by the same procedure
Analyzed after a sample which contains compounds at concentrations
greater than the calibration range
Every 12 hours on each GC column used for analysis
Prepared and stored with each set of samples
Every 12 hours for each instrument used for analysis
Prior to initial calibration, on each instrument used for analysis
Upon initial set up of each instrument, and each time continuing
calibration fails to meet the acceptance criteria
Every 12 hours for each instrument used for analysis
Added to each sample, standard, and blank
Once every 20 or fewer samples of same fraction, matrix, and level in a
Sample Delivery Group (SDG)
Once every 20 or fewer samples of same fraction, matrix, and level in
an SDG
Determined annually, per matrix and level
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PERFORMANCE MONITORING ACTIVITIES
Laboratory performance monitoring activities are
provided primarily by ASB and the Regions to ensure
that contract laboratories are producing data of the
appropriate quality. EPA performs on-site laboratory
audits, data package audits, GC/MS and/or GC/ECD tape
audits, and evaluates laboratory performance through the
use of blind Performance Evaluation (PE) samples.
CONTACTING EPA
For more information, or for suggestions to improve this
analytical service, please contact:
Phil Cocuzza
Organic Program Manager
USEPA/ASB
Ariel Rios Building (5203P)
1200 Pennsylvania Avenue, NW
Washington, DC 20460
732-632-4765
FAX: 732-906-6843
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