United States
Environmental Protection
Agency
Office of
Solid Waste and
Emergency Response
EPA540-F-01-013
Publication 9240.0-37FS
June 2001
Low Concentration Organic Analytical
Service for Superfund (Water Matrix)
(OLC03.2)
Office of Emergency and Remedial Response
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 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, and pesticide/Aroclor (pesticide/PCB) 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 Operations/Data Quality Center (AOC) of the Office of
Emergency and Remedial Response (OERR) offers an analytical service that provides data from the analysis of water
samples for low concentration organic compounds for use in the Superfund decision-making process. Through a series
of standardized procedures and a strict chain-of-custody, the low concentration 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 low concentration organic analytical service
provides a contractual framework for laboratories to
apply EPA/CLP analytical methods for the isolation,
detection, and quantitative measurement of 50 volatile,
65 semivolatile, and 28 pesticide/Aroclor
(pesticide/PCB) target compounds in water samples.
The analytical service provides the methods to be used
and the specific contractual requirements, by which
EPA evaluates the data. The options for data
turnaround time for this contract are 7, 14, or 21 days
after laboratory receipt of the last sample in the Sample
Delivery Group (SDG). This service uses Gas
Chromatography/Mass Spectrometry (GC/MS) and Gas
Chromatography with Electron Capture Detector
(GC/ECD) techniques to analyze the target compounds.
DATA USES
This analytical service provides data that 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
at all stages in the investigation of hazardous waste
sites including: site inspections; Hazard Ranking
System (HRS) scoring; remedial investigation/
feasibility studies; remedial design; treatability studies;
and removal actions. In addition, this service provides
data that are available for use in Superfund
enforcement/litigation activities.
TARGET COMPOUNDS
The compounds and quantitation limits for which this
service is applicable are listed in Table 1. The lowest
reportable quantitation limits are 0.50 ng/L for the
volatile compounds, 5.0 ng/L for the semivolatile
compounds, and 0.01 ng/L for the pesticide/Aroclor
compounds. The list of target compounds 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 deleted from the Target Compound List (TCL),
based on advances in analytical methods, evaluation of
method performance data, and the needs of the
Superfund program.
METHODS AND INSTRUMENTATION
For volatiles, 25 mL of sample is added to a purge-and-
trap device. A solution of 14 Deuterated Monitoring
Compounds (DMCs) and a solution of internal
standards are added to the sample which is then purged
with an inert gas at room temperature.
-------
Table 1. Target Compound List and Contract Required Quantitation Limits (CRQLs) in ug/L (OLC03.2)
VOLATILES
Quantitation Limits
Ug/L
1. Dichlorodifluoromethane
2. Chloromethane
3. Vinyl Chloride
4. Bromomethane
5. Chloroethane
6. Trichlorofluoromethane .
7. 1,1-Dichloroethene
.... 0.5
.... 0.5
.... 0.5
.... 0.5
.... 0.5
.... 0.5
.... 0.5
8. l,l,2-Trichloro-l,2,2-trifluoroethane 0.5
9. Acetone 5
10. Carbon Bisulfide 0.5
11. Methyl Acetate 0.5
12. Methylene Chloride 0.5
13. trans-1,2-Dichloroethene 0.5
14. Methyl tert-Butyl Ether 0.5
15. 1,1-Dichloroethane 0.5
16. cis-l,2-Dichloroethene 0.5
17. 2-Butanone 5
18. Bromochloromethane 0.5
19. Chloroform 0.5
20. 1,1,1-Trichloroethane 0.5
21. Cyclohexane 0.5
22. Carbon Tetrachloride 0.5
23. Benzene 0.5
24. 1,2-Dichloroethane 0.5
25. Trichloroethene 0.5
26. Methylcyclohexane 0.5
27. 1,2-Dichloropropane 0.5
28. Bromodichloromethane 0.5
29. cis-l,3-Dichloropropene 0.5
30. 4-Methyl-2-pentanone 5
31. Toluene 0.5
32. trans-l,3-Dichloropropene 0.5
33. 1,1,2-Trichloroethane 0.5
34. Tetrachloroethene 0.5
35. 2-Hexanone 5
36. Dibromochloromethane 0.5
37. 1,2-Dibromoethane 0.5
38. Chlorobenzene 0.5
39. Ethylbenzene 0.5
40. Xylenes (total) 0.5
41. Styrene 0.5
42. Bromoform 0.5
43. Isopropylbenzene 0.5
44. 1,1,2,2-Tetrachloroethane 0.5
45. 1,3-Dichlorobenzene 0.5
46. 1,4-Dichlorobenzene 0.5
47. 1,2-Dichlorobenzene 0.5
48. l,2-Dibromo-3-chloropropane 0.5
49. 1,2,4-Trichlorobenzene 0.5
50. 1,2,3-Trichlorobenzene 0.5
SEMIVOLATILES
Quantitation Limits
Ug/L
51. Benzaldehyde
52. Phenol
53. bis-(2-Chloroethyl) ether
54. 2-Chlorophenol
55. 2-Methylphenol
. . 5
. . 5
. . 5
. . 5
. . 5
56. 2,2'-oxybis (1-Chloropropane)1 . 5
57. Acetophenone 5
58. 4-Methylphenol 5
59. N-Nitroso-di-n-propylamine ... 5
60. Hexachloroethane 5
61. Nitrobenzene 5
62. Isophorone 5
63. 2-Nitrophenol 5
64. 2,4-Dimethylphenol 5
65. bis (2-Chloroethoxy) methane .. 5
66. 2,4-Dichlorophenol 5
67. Naphthalene 5
68. 4-Chloroaniline 5
69. Hexachlorobutadiene 5
70. Caprolactam 5
71. 4-Chloro-3-methylphenol 5
72. 2-Methylnaphthalene 5
73. Hexachlorocyclopentadiene .... 5
74. 2,4,6-Trichlorophenol 5
75. 2,4,5-Trichlorophenol 20
76. U'-Biphenyl 5
77. 2-Chloronaphthalene 5
78. 2-Nitroaniline 20
79. Dimethylphthalate 5
80. 2,6-Dinitrotoluene 5
81. Acenaphthylene 5
82. 3-Nitroaniline 20
83. Acenaphthene 5
84. 2,4-Dinitrophenol 20
85. 4-Nitrophenol 20
86. Dibenzofuran 5
87. 2,4-Dinitrotoluene 5
88. Diethylphthalate 5
89. Fluorene 5
90. 4-Chlorophenyl-phenylether ... 5
91. 4-Nitroaniline 20
92. 4,6-Dinitro-2-methylphenol ... 20
93. N-Nitrosodiphenylamine 5
94. 1,2,4,5 Tetrachlorobenzene .... 5
95. 4-Bromophenyl-phenylether ... 5
96. Hexachlorobenzene 5
97. Atrazine 5
98. Pentachlorophenol 5
99. Phenanthrene 5
100. Anthracene 5
Quantitation Limits
Ug/L
101. Di-n-butylphthalate 5
102. Fluoranthene 5
103. Pyrene 5
104. Butylbenzylphthalate 5
105. 3,3'-Dichlorobenzidine 5
106. Benzo(a)anthracene 5
107. Chrysene 5
108. bis-(2-Ethylhexyl) phthalate 5
109. Di-n-octylphthalate 5
110. Benzo(b)fluoranthene 5
111. Benzo(k)fluoranthene 5
112. Benzo(a)pyrene 5
113. Indeno(l,2,3-cd)pyrene 5
114. Dibenzo(a,h)anthracene 5
115. Benzo(g,h,i)perylene 5
PESTICIDES/AROCLORS
(PESTICIDES/PCBs)
116. alpha-BHC 0.01
117. beta-BHC 0.01
118. delta-BHC 0.01
119. gamma-BHC (Lindane) 0.01
120. Heptachlor 0.01
121. Aldrin 0.01
122. Heptachlor epoxide2 0.01
123. Endosulfan I 0.01
124. Dieldrin 0.02
125. 4,4'-DDE 0.02
126. Endrin 0.02
127. Endosulfan II 0.02
128. 4,4'-DDD 0.02
129. Endosulfan sulfate 0.02
130. 4,4'-DDT 0.02
131. Methoxychlor 0.10
132. Endrin ketone 0.02
133. Endrin aldehyde 0.02
134. alpha-Chlordane 0.01
135. gamma-Chlordane 0.01
136. Toxaphene 1.0
137. Aroclor-1016 0.20
138. Aroclor-1221 0.40
139. Aroclor-1232 0.20
140. Aroclor-1242 0.20
141. Aroclor-1248 0.20
142. Aroclor-1254 0.20
143. Aroclor-1260 0.20
'Previously known by the name bis (2-chloroisopropyl) ether.
2Only the exo-epoxy isomer (isomer B) of heptachlor epoxide is reported on the data reporting forms.
The volatiles purged from the sample are trapped on a
solid sorbent. They are subsequently desorbed into a
GC/MS system.
For semivolatile and pesticide/Aroclor water samples,
a 1 -L aliquot is extracted with methylene chloride using
continuous liquid-liquid extraction or a separatory
funnel (for pesticides/Aroclors only). For
pesticide/Aroclors, the aliquot is spiked with a solution
of two surrogate compounds before extraction. The
extract is dried, concentrated, and subjected to cleanup
prior to GC/ECD analysis. For semivolatiles, the
aliquot is acidified to a pH of 2.0 and a solution of 16
DMCs is added before extraction. The extract is dried
and concentrated, internal standards are added, and then
it is analyzed by GC/MS. Table 2 summarizes the
preparation methods and instruments used in this
analytical service.
-------
DATA DELIVERABLES
Data deliverables for this service include hardcopy data
reporting forms, supporting raw data, and electronic
data on diskette or other means specified by EPA. The
laboratory must submit data to EPA within 7, 14, or 21
days after laboratory receipt of the last sample in the
SDG. EPA then checks the data for compliance with
contract requirements. A report of instances of
noncompliance is distributed to the laboratory and the
Region within 7 days from the receipt of the data. The
laboratory has 7 days from receipt of the report to
reconcile defective data and resubmit the data to EPA.
EPA then screens the data and sends a final data
assessment report to the laboratory and the Region.
QUALITY ASSURANCE
The Quality Assurance (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 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/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 requirements for this analytical
service are shown in Table 3.
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, and GC/MS tape audits,
and evaluates laboratory performance through the use
of blind PE samples.
Table 2. Methods and Instruments
Fraction
Volatiles
Semivolatiles
Pesticides/ Aroclors
(Pesticides/PCBs)
Preparation Method
Purge-and-trap
Continuous liquid-liquid extraction
Continuous liquid-liquid or separately funnel
extraction
Analytical Instrument
GC/MS analysis
GC/MS analysis
GC/ECD analysis
Table 3. Quality Control
QC Operation
Deuterated Monitoring Compounds (DMCs) (volatiles
and semivolatiles)
Method Blanks (volatiles)
Method Blanks [semivolatiles and pesticides/ Aroclors
(pesticides/PCBs)]
Instrument Blank (volatiles)
Instrument Blank [pesticides/ Aroclors (pesticides/PCBs)]
Surrogates [pesticides/ Aroclors (pesticides/PCBs)l
Frequency
Added to each sample, standard, and blank.
Analyzed at least every 12 hours.
Prepared with each group of 20 field samples or less, or
each time samples are extracted.
Analyzed after a sample that contains compounds at
concentrations greater than the calibration range.
Every 12 hours and preceding all groups of acceptable
sample analysis.
Added to each sample, standard, and blank.
-------
Table 3. Quality Control (Continued)
QC Operation
Storage Blank (volatiles)
Instrument Performance Check (volatiles and
semivolatiles)
GC Resolution Check [pesticides/ Aroclors
(pesticides/PCBs)]
Initial Calibration
Continuing Calibration (volatiles and semivolatiles)
Calibration Verification [pesiticides/Aroclor
(pesticides/PCBs)l
Internal Standards (volatiles and semivolatiles)
Laboratory Control Sample (LCS) [pesticides/ Aroclor
(pesticides/PCBs)]
Performance Evaluation (PE) Sample
Matrix Spike/Matrix Spike Duplicate (MS/MSD)
Method Detection Limit (MDL)
Sulfur Cleanup Blank [pesticides/Aroclor
(pesticides/PCBs)]
Sample Cleanup by Florisil Cartridge
Florisil Cartridge Performance Check [pesticides/Aroclor
(pesticides/PCBs)]
Frequency
Prepared and stored with each group of samples.
Analyzed after all samples in the SDG have been
analyzed.
Prior to any analysis and every 12 hours.
Prior to initial calibration on each GC column used for
analysis.
Upon initial set up of each instrument, after major
instrument maintenance or modification, and each time
continuing calibration fails to meet the acceptance
criteria.
Every 12 hours for each instrument used for analysis.
Beginning and end of each 12-hour data collection period.
Added to each sample, standard, and blank.
Prepared and analyzed once per SDG.
Prepared and analyzed (if provided) with every 20 field
samples in an SDG or for each SDG, whichever is most
frequent.
Performed only when requested by Region. Performed
with every 20 field samples in an SDG or for each SDG,
whichever is most frequent.
Run before any samples analyzed under contract (annually
thereafter) and after major instrument maintenance.
Only when part of a set of samples extracted together
requires sulfur removal.
Performed on all sample extracts and method blank
extracts.
Performed at least once on each lot of cartridges used for
sample cleanup or every 6 months, whichever is most
frequent.
For more information, or for suggestions to improve this
analytical service, please contact:
Terry Smith
Organic Program Manager
USEPA/AOC
Ariel Rios Building, (5204G)
1200 Pennsylvania Avenue, NW
Washington, DC 20460
703-603-8849
FAX: 703-603-9112
------- |