United States
Environmental Protection
Agency
Office of
Solid Waste and
Emergency Response
OSWER Document 540-F-05-008
EPA Publication 9240.1-50FS
January 2006
Multi-Media, Multi-Concentration,
Organic Analytical Service for
Superfund (SOM01.1)
Office of Superfund Remediation and Technology Innovation (OSRTI)
Analytical Services Branch (ASB) (5102G)
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. Changes to the organic method include the
separation of pesticide and Aroclor methods, the
inclusion of Selected Ion Monitoring (SDVI) analysis,
and the incorporation of the Staged Electronic Data
Deliverable (SEDD) requirement for Electronic Data
Deliverables (EDDs) in Extensible Markup Language
(XML) format. 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
foravariety of purposes, suchas 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 SOM01.1*
VOLATILES
1 . Dichlorodifiuoromethane
2. Chloromethane
3. Vinyl Chloride
4. Bromomethane
5. Chloroethane
6. Trichlorofiuoromethane
7. 1,1-Dicholoroethene
8. l,l,2-Trichloro-l,2,2-trifiuoroethane
9. Acetone
10. Carbon Disulfide
1 1 . Methyl acetate
12. Methylene chloride
13. trans- 1,2-Dichloroethene
14. Methyl tert-butyl ether
15. 1,1 -Di chloroethane
16. cis- 1,2-Dichloroethene
17. 2-Butanone
18. Bromochloromethane
19. Chloroform
20. 1,1,1-Tnchloroethane
21. Cyclohexane
22. Carbon tetrachloride
23. Benzene
24. 1,2-Di chloroethane
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-Trichloroethane
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
2.0 20
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
(M6/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
Low
Soil
("g/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
("g/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. 1 ,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-Chloroaniline
71. Hexachlorobutadiene
72. Caprolactam
73. 4-Chloro-3-methylphenol
74. 2-Methylnapthalene
75. Hexachlorocyclopentadiene
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
(MS/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
(«g/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
Low
Water
("g/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
(fig/kg)
3.3
3.3
Low
Soil
(^g/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
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
Med.
Soil
(^g/kg)
250
250
250
250
250
250
250
250
250
250
250
250
250
Med.
Soil
(fig/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
* For volatiles, quantitation limits for medium soils are approximately 50 times the quantitation limits for low soils. For semivolatile medium soils, quantitation limits are approximately 50 times the
quantitation limits for low soils.
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Table 1. Target Compound List (TCL) and Contract Required Quantitation Limits (CRQLs) for SOM01.1* (Con't)
Quantitation Limits
Low
Water
by
SIM
(M6/L
SEMIVOLATILES (CON'T)
78. l.l'-Brphenyl
79. 2-Chloronapthalene
80. 2-Nitroamlme
Sl.Dimethylphthalate
82. 2,6-Dinitrotoluene
83. Acenaphthylene 0.10
84. 3-Nitroaniline
85. Acenaphthene 0.10
86. 2,4-Dinitrophenol
87. 4-Nitrophenol
88. Dibenzofuran
89. 2,4-Dimtrotoluene
90. Diethylphthalate
91.Fluorene 0.10
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 phenyl ether
98. Hexachlorobenzene
99. Atrazine
100. Pentachlorophenol 0.20
101. Phenanthrene 0.10
102. Anthracene 0.10
103. Carbazole
104. Di-n-butylphthalate
105. Fluoranthene 0.10
106. Pyrene 0.10
107. Butylbenzylphthalate
108. 3,3'-Dichlorobenzidine
109. Benzo(a)anthracene 0.10
110. Chrysene 0.10
111. Bis(2-ethylhexyl)phthalate
112. Di-n-octylphthalate
113. Benzo(b)fiuoroanthene 0.10
114. Benzo(k)fluoroanthene 0.10
* For volatiles, quantitation limits for medium soils
quantitation limits for low soils.
Low
Low Soil by
Water SIM
(Ug/L) (fig/kg)
5.0
5.0
10
5.0
5.0
5.0 3.3
10
5.0 3.3
10
10
5.0
5.0
5.0
5.0 3.3
5.0
10
10
5.0
5.0
5.0
5.0
5.0
10 6.7
5.0 3.3
5.0 3.3
5.0
5.0
5.0 3.3
5.0 3.3
5.0
5.0
5.0 3.3
5.0 3.3
5.0
5.0
5.0 3.3
5.0 3.3
Low
Soil
("g/kg)
170
170
330
170
170
170
330
170
330
330
170
170
170
170
170
330
330
170
170
170
170
170
330
170
170
170
170
170
170
170
170
170
170
170
170
170
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
SEMIVOLATILES (CON'T)
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. EndosulfanI
128. Dieldrm
129. 4,4-DDE
130. Endrin
131.EndosulfanII
132. 4-4'-DDD
133. Endosulfan sulfate
134. 4-4'-DDT
135. Methoxychlor
136. Endrin ketone
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
Quantitation Limits
Low
Water Low
by Low Soil by
SIM Water SIM
(ug/L) (ug/L) (fig/kg)
0.10 5.0 3.3
0.10 5.0 3.3
0.10 5.0 3.3
0.10 5.0 3.3
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
Low
Soil
(^g/kg)
170
170
170
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
Med.
Soil
(^g/kg)
5000
5000
5000
5000
5000
are approximately 50 times the quantitation limits for low soils. For semivolatile medium soils, quantitation limits are approximately 30 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 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 uncoveredby 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:
Anand Mudambi
Organic Program Manager
USEPA/ASB
Ariel Rios Building (5102G)
1200 Pennsylvania Avenue, NW
Washington, DC 20460
703-603-8796
FAX: 703-603-9116
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