United States
Environmental Protection
Agency
Office of
Solid Waste and
Emergency Response
OSWER Document 9240.1-42-FSD
EPA Publication 540-F-03-005
August 2003
o-EPA
Multi-Media, Multi-Concentration,
Organic Analytical Service for
Superfund (OLM04.3)
Office of Superfund Remediation and Technology Innovations
Analytical Operations/Data Quality Center (5204G)
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 forthe measurement of various pollutants
in environmental samples fromknownor suspected hazardous waste sites. Among the pollutants that are of concern to the EPA
at such sites, are a series of volatile, semivolatile, and pesticide/Aroclor (pesticide/PCB) compounds that are analyzed using
Gas Chromatography coupled with Mass Spectrometry (GC/MS) and Gas Chromatography with Electron Capture (GC/EC).
The Analytical Operations/Data Quality Center (AOC) of the Office of Superfund Remediation and Technology Innovations
(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
The new organic analytical service is available as of March
2003. It provides a technical and contractual frame work
for laboratories to apply EPA/CLP analytical methods for
the isolation, detection, and quantitative measurement of 48
volatile, 65 semivolatile, and 28 pesticide/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 OperatingProcedures (SOPs),
by which EPA evaluates the data. This service uses
GC/MS and GC/EC methods to analyze the target
compounds. Three data delivery turnarounds are available
to CLP customers: 7, 14, and 21-day turnaround after
laboratory receipt of the last sample in the set. hi addition,
there are 48 (for volatiles) and 72-hour (or semivolatiles
and pesticides/Aroclors) preliminary data submission
options available. The data associated with these
Preliminary Results is due within the specified time after
receipt of each sample at the laboratory. Options under
this service include a closed systempurge-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, modified quantitation limits (e.g., lower
volatile limits), additional cleanup options, 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 contaminationatahazardous 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 site inspections, Hazard
Ranking System scoring, remedial investigations/feasibility
studies, remedial design, treatability studies, and removal
actions, hi addition, this service provides data that will be
available for use in Superfund enforcement/litigation
activities.
TARGET COMPOUNDS
The compounds for which this service is applicable and the
corresponding quantitation limits are listedin Table 1. For
water samples, the lowest reportable quantitation limits are
10 ppb for the volatile compounds, 10 ppb for the
semivolatile compounds, and 0.05 ppb for the
pesticide/Aroclor compounds. For soil samples, the
lowest reportable quantitation limits are 10 ppb for the
volatile compounds, 330 ppb for the semivolatile
compounds, and 1.7 ppb for the pesticide/Aroclor
compounds. Specific sample quantitation limits will be
highly matrix-dependent. Compounds identified with
concentrations belowthe quantitationlimitwillbe reported
as estimated concentration values.
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Table 1. Target Compound List and Contract Required Quantitation Limits (CRQLs) For OLM04.3*
Quantitation Limits
VOLATILES
1. Dichlorodifluoromethane
2. Chloromethane
3. Vinyl Chloride
4. Bromomethane
5. Chloroethane
6. Trichlorofluoromethane
7. 1,1-Dichloroethene
8. 1,1,2-Trichloro-
1,2,2-trifluoroethane
9. Acetone
10. Carbon Disulfide
11. Methyl Acetate
12. Methylene Chloride
13. trans- 1,2-Dichloroethene
14. Methyl tert-Butyl Ether
15. 1,1-Dichloroethane
16. cis-l,2-Dichloroethene
17. 2-Butanone
18. Chloroform
19. 1,1,1-Trichloroethane
20. Cyclohexane
21. Carbon Tetrachloride
22. Benzene
23. 1,2-Dichloroethane
24. Trichloroethene
25. Methylcyclohexane
26. 1,2-Dichloropropane
27. Bromodichloromethane
28. cis-l,3-Dichloropropene
29. 4-Methyl-2-pentanone
30. Toluene
31.trans-l,3-
Dichloropropene
32. 1,1,2-Trichloroethane
33. Tetrachloroethene
34. 2-Hexanone
35. Dibromochloromethane
36. 1,2-Dibromoethane
37. Chlorobenzene
38. Ethylbenzene
39. Xylenes (Total)
40. Styrene
41. Bromoform
42. Isopropylbenzene
43. 1,1,2,2-Tetrachloroethane
44. 1,3-Dichlorobenzene
45. 1,4-Dichlorobenzene
46. 1,2-Dichlorobenzene
47. 1,2-Dibromo-
3-chloropropane
48. 1,2,4-Triclorobenzene
Low
Water Soil
(ug/L) (ug/Kg)
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
10 10
Modified
Cat1
Levels
(ug/L)
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
10
0.50
0.50
0.50
0.50
0.50
0.50
0.50
10
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
0.50
10
0.50
0.50
0.50
0.50
0.50
10
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
Quantitation Limits
SEMIVOLATILES
49. Benzaldehyde
50. Phenol
51. bis-(2-Chloroethyl)ether
52. 2-Chlorophenol
53. 2-Methylphenol
54. 2,2'-oxybis
(1-Chloropropane)
55. Acetophenone
56. 4-Methylphenol
57. N-Nitroso-di-n-
propylamine
58. Hexachloroethane
59. Nitrobenzene
60. Isophorone
61. 2-Nitrophenol
62. 2,4-Dimethylphenol
63. bis-(2-Chloroethoxy) methane
64. 2,4-Dichlorophenol
65. Naphthalene
66. 4-Chloroaniline
67. Hexachlorobutadiene
68. Caprolactam
69. 4-Chloro-3-methylphenol
70. 2-Methylnaphthalene
71. Hexachlorocyclo-pentadiene
72. 2,4,6-Trichlorophenol
73. 2,4,5-Trichlorophenol
74. U'-Biphenyl
75. 2-Chloronaphthalene
76. 2-Nitroaniline
77. Dimethylphthalate
78. 2,6-Dinitrotoluene
79. Acenaphthylene
80. 3-Nitroaniline
81. Acenaphthene
82. 2,4-Dinitrophenol
83. 4-Nitrophenol
84. Dibenzofuran
85. 2,4-Dinitrotoluene
86. Diethylphthalate
87. Fluorene
88. 4-Chlorophenyl-phenyl ether
89. 4-Nitroaniline
90. 4,6-Dinitro-2-methylphenol
91. N-Nitrosodiphenylamine
92. 4-Bromophenyl-phenylether
93. Hexachlorobenzene
94. Atrazine
95. Pentachlorophenol
96. Phenanthrene
97. Anthracene
Water
(ug/L)
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
25
10
10
25
10
10
10
25
10
25
25
10
10
10
10
10
25
25
10
10
10
10
25
10
10
Low
Son
(Hg/Kg)
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
830
330
330
830
330
330
330
830
330
830
830
330
330
330
330
830
830
830
330
330
330
330
830
330
330
Quantitation Limits
98. Carbazole
99. Di-n-butylphthalate
100. Fluoranthene
101. Pyrene
102. Butylbenzylphthalate
103. 3,3'-Dichlorobenzidine
104. Benzo(a)anthracene
105. Chrysene
106. bis-(2-
Ethylhexyl)phthalate
107. Di-n-octylphthalate
108. Benzo(b)fluoranthene
109. Benzo(k)fluoranthene
110. Benzo(a)pyrene
111. Indeno(l,2,3-cd)pyrene
112. Dibenz(a,h)anthracene
113. Benzo(g,h,i)perylene
PESTICIDES/AROCLORS
(PESTICIDES/PCBs)
114. alpha-BHC
115.beta-BHC
116. delta-BHC
1 17. gamma-BHC (Lindane)
118. Heptachlor
119. Aldrin
120. Heptachlor epoxide
m.Endosulfanl
122. Dieldrin
123. 4,4'-DDE
124. Endrin
125. Endosulfan II
126. 4,4'-DDD
127. Endosulfan sulfate
128. 4,4'-DDT
129. Methoxychlor
130. Endrin ketone
131. Endrin aldehyde
132. alpha-Chlordane
133. gamma-Chlordane
134. Toxaphene
135. Aroclor-1016
136. Aroclor-1221
137. Aroclor- 1232
138. Aroclor- 1242
139. Aroclor- 1248
140. Aroclor- 1254
141. Aroclor-1260
Water
(ug/L)
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
Water
(Ug/L)
0.05
0.05
0.05
0.05
0.05
0.05
0.05
0.05
0.10
0.10
0.10
0.10
0.10
0.10
0.10
0.50
0.10
0.10
0.05
0.05
5.0
1.0
2.0
1.0
1.0
1.0
1.0
1.0
Low
Son
(ug/Kg)
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
330
Son
(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
33
67
33
33
33
33
33
*For volatiles, quantitation limits for medium soils are approximately 130 times the quantitation limits for low soils. For semivolatile medium soils,
quantitation limits are approximately 30 times the quantitation limits for low soils.
'Modified quantitation limits are available under the Flexibility Clause.
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The list of target compounds 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
Target Compound List (TCL), based on advances in
analytical methods, evaluation of method performance
data, and the needs of the Superfund program.
For drinking water and groundwater type samples, use of
the low concentration organic analytical service is
recommended.
METHODS AND INSTRUMENTATION
For 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. For volatile low-level soil samples, a
5 g aliquot of soil is added to a purge and trap device with
5 mL of reagent water then purged with an inert gas at
40°C; or a 5 g aliquot (pre-weighed in the field) is purged
from a closed-system purge and trap device at 40°C. For
volatile medium-level soil samples, a measured amount is
collected/extracted with methanol and an aliquot of the
methanol extract is added to reagent water and purged at
room temperature. For both water and soil samples, the
volatiles purged from the sample are trapped on a solid
sorbent. They are subsequently desorbed by rapidly
heating the sorbent and then introduced into a GC/MS
system.
For semivolatile and pesticide/Aroclor water samples, a
1 L aliquot is extracted with methylene chloride using a
continuous liquid-liquid extractor or separatory funnel [for
pesticides/Aroclors only]. For low-level semivolatile soil
and pesticide/Aroclor soil samples, a 30 g soil/sediment
sample is extracted with methylene chloride/acetone using
sonication, automated soxhlet, or pressurized fluid
extraction techniques. For medium-level semivolatile soil
samples, a 1 g 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/EC for pesticides/Aroclors. Table 2 summarizes the
methods and instruments used in this analytical service.
PRESERVATION OF VOLATILE SOIL SAMPLES
All soil sample containers that are not chemically
preserved should be frozen upon receipt at the laboratory.
This includes closed-system vials received from the
sampler; closed-system vials generated by the laboratory;
low headspace vials containing sample for moisture
determination (or for analysis by the old Method 5030
protocol); and all QC samples.
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 the set. Preliminary
data must be submitted within 48 hours (forvolatiles) or 72
hours (for semivolatiles and pesticides/Aroclors) after
receipt of each sample at the laboratory. EPA then
processes the data through an automated Data Assessment
Tool (DAT). DAT is a complete CLP data assessment
package. DAT incorporates Contract Compliance
Screening (CCS) and Computer-Aided Data Review and
Evaluation (CADRE) to provide EPA Regions with PC-
compatible reports, spreadsheets, and electronic files
within 24 to 48 hours from the receipt of the data. This
automated tool 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 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
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 the quality
required.
During the implementation of the data collection effort,
QA activities ensure that the 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 for this analytical
service.
QUALITY CONTROL
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 shown in Table 3.
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Table 2. Methods and Instruments
Fraction
Volatiles
Semivolatiles
Pesticides/Aroclors
Water
Purge-and-trap followed by GC/MS analysis.
Continuous liquid-liquid extraction followed
by GC/MS analysis.
Continuous liquid-liquid or separatory funnel
extraction followed by dual column GC/EC
analysis.
Soil
Purge-and-trap or closed-system
purge-and-trap followed by GC/MS
analysis.
Sonication, automated soxhlet, or
pressurized fluid extraction followed
by GC/MS analysis.
Sonication, automated soxhlet, or
pressurized fluid extraction followed
by dual column GC/EC analysis.
Table 3. Quality Control
QC Operation
System Monitoring Compounds (volatiles)
Surrogates (for Semivolatiles and pesticides/Aroclors)
Method Blanks (volatiles)
Method Blanks (semivolatiles and pesticides/Aroclors)
Instrument Blank (volatiles)
Instrument Blank (pesticides/Aroclors)
Storage Blanks (volatiles)
GC/MS Mass Calibration and Ion Abundance Patterns
(volatiles and semivolatiles)
GC Resolution Check (pesticides/Aroclors)
Initial Calibration
Continuing Calibration
Internal Standards (volatiles and semivolatiles)
Matrix Spike and Matrix Spike Duplicate
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 that 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, whenever
instrument maintenance/modification has been performed,
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 an SDG.
PERFORMANCE MONITORING ACTIVITIES
Laboratory performance monitoring activities are provided
primarily by AOC 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/EC tape audits, and evaluates
laboratory performance through the use of blind
performance evaluation samples.
For more information, or for suggestions to improve this
analytical service, please contact:
Terry Smith
Organic Program Manager
EPA/AOC
Ariel Rios Building (5204G)
1200 Pennsylvania Avenue, NW
Washington, DC 20460
703-603-8849
FAX: 703-603-9112
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