United States
Environmental Protection
Agency
Office of
Solid Waste and
Emergency Response
OSWER Document 9240.1-48FS
EPA Publication 540-F-05-002
Draft Final - September 2005
Multi-Media, Multi-Concentration
Chlorinated Biphenyl Congeners
Analytical Service for Superfund
(CBC01.0)
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 Chlorinated Biphenyl (CB) Congeners that are analyzed using High
Resolution Gas Chromatography/HighResolutionMass Spectrometry (HRGC/HRMS). The Analytical Services Branch
(ASB) of EPA's Office of Superfund Remediation and Technology Innovation (OSRTI) offers an analytical service that
provides data from the analysis of water, soil, sediment, sludge, non-human tissue, ash, oil, and oily matrices for use in
the Superfund decision-making process. Through a series of standardized procedures and a strict chain-of-custody, the
CB congeners analytical service produces data of known and documented quality.
DESCRIPTION OF SERVICES
The CB congeners analytical service provides a flexible
contractual framework for laboratories to apply EPA
analytical methods for the isolation, detection, and
quantitative measurement of 209 2,2',3,3',4,4',5,5',6,6'-
substituted mono- through deca- CB congeners in
water, soil, sediment, sludge, non-human tissue, ash,
oil, and oily matrices. EPA ASB has prequalified
laboratories that use the CB congeners Statement of
Work (SOW) CBC01.0 to provide this service. The
standard data Turnaround Time (TAT) for this service
is 35 days after laboratory receipt of the last sample in
the Sample Delivery Group (SDG). This TAT can be
changed to meet project-specific requirements.
REQUESTING THIS FLEXIBLE SERVICE
The CB congeners analytical service can be requested
by EPA Regions and other interested parties by
submitting a Task Order (TO) to EPA ASB. These TOs
can modify the SOW to meet project-specific
requirements [e.g., changes in TAT, detection limits, or
Target Compound Lists (TCLs)]. The CB congeners
SOW can be accessed at:
http://www.epa.gov/superfund/programs/clp/nonroutine.htm
DATA USES
The CB congeners analytical service provides data that
EPA uses for a variety 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 clean-up actions; and determining when
remedial actions are complete. The data may be used
in 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 applicable target compounds and Contract
Required Quantitation Limits (CRQLs) for this service
are listed in Table 1. For water samples, the lowest
reportable CRQL is 10 pg/L. For soil and tissue
samples, the lowest reportable CRQL is 1.0 ng/kg. For
extracts, the lowest reportable CRQL is 0.5 pg/uL. The
specific CRQLs are highly matrix-dependent. The
CRQLs listed herein are provided for guidance and may
not always be achievable.
-------
METHODS AND INSTRUMENTATION
For water samples, the stable isotopically-labeled
analogs of the Toxics and labeled Level of Chlorination
(LOG) CB congeners are spiked into a 1L sample. The
sample is extracted using solid-phase extraction (SPE),
separately funnel extraction (SFE), or continuous
liquid/liquid extraction (CLLE).
For soil/sediment samples, the labeled compounds are
spiked into a sample containing 10 g (dry weight) of
solids and extracted for 16-24 hours with toluene in a
Soxhlet/Dean-Stark (SDS) extractor. The extract is
concentrated for cleanup.
For non-human tissue samples, a 20 g aliquot of a
sample is homogenized, and a 10 g aliquot is spiked
with the labeled compounds. The sample is mixed with
anhydrous sodium sulfate, allowed to dry for 12-24
hours, and extracted for 18-24 hours using methylene
chloride in an SDS extractor. The extract is evaporated
to near dryness, and the lipid content is determined.
For all samples, the extracts are cleaned and
concentrated to 20 uL. Labeled internal standards are
added to each extract and an aliquot of the extract is
injected into the High Resolution Gas Chromotograph
(HRGC). The analytes are separated by the HRGC and
detected by a High Resolution Mass Spectrometer
(HRMS). Table 2 summarizes the methods and
instruments used in this analytical service.
DATA DELIVERABLES
Data deliverables for the CB congeners analytical
service include the hardcopy data reporting forms and
supporting raw data. Certain TOs may require the use
of the Electronic Data Deliverable (EDD) format. The
EDD reporting requirements will be outlined in the TO.
The laboratory must submit data to EPA within 3 5 days
after laboratory receipt of the last sample in the SDG,
or as stated in the TO. The EPA Regions then review
the data, based on project-specific requirements.
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 the quality required.
During the planning of an environmental data
collection program, QA activities focus on defining
data quality criteria and designing a Quality Control
(QC) system to measure the quality of data being
generated. During the implementation of the data
collection effort, QA activities ensure that the QC
system is functioning effectively, and 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 (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
analysis are shown in Table 3. A number of optional
cleanup procedures are available for the CB congeners
SOW.
-------
Table 1. Target Compound List (TCP and
Estimated Contract Required Ouantitation Limits (CROLs)
CB Congener1
IUPAC
Number
Water (pg/L)
Other (ng/kg)
Extract (pg/uL)
Monochlorobiphenyls
2-MoCB
3-MoCB
4-MoCB
1
2
3
200
10
200
20
1
20
10
0.5
10
Dichlorobiphenyls
2,2'-DiCB
2,3-DiCB
2,3'-DiCB
2,4-DiCB
2,4'-DiCB2
2,5-DiCB
2,6-DiCB
3,3'-DiCB
3,4-DiCB
3,4'-DiCB
3,5-DiCB
4,4'-DiCB
4
5
6
7
8
9
10
11
12
13
14
15
500
50
50
50
500
50
50
200
100
100
100
500
50
5
5
5
50
5
5
20
10
10
10
50
25
2
2
2
25
2
2
10
5
5
5
25
Trichlorobiphenyls
2,2',3-TrCB
2,2',4-TrCB
2,2',5-TrCB2
2,2',6-TrCB
2,3,3'-TrCB
2,3,4-TrCB
2,3,4'-TrCB
2,3,5-TrCB
2,3,6-TrCB
2,3',4-TrCB
2,3',5-TrCB
2,3',6-TrCB
2,4,4'-TrCB2
2,4,5-TrCB
2,4,6-TrCB
2,4',5-TrCB
2,4',6-TrCB
2',3,4-TrCB
2'3,5-TrCB
3,3',4-TrCB
3,3',5-TrCB
3,4,4'-TrCB
3,4,5-TrCB
3,4',5-TrCB
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
100
200
500
100
500
200
200
200
200
200
200
200
500
200
500
500
200
200
200
200
200
500
200
200
10
20
50
10
50
20
20
20
20
20
20
20
50
20
50
50
20
20
20
20
20
50
20
20
5
10
25
5
25
10
10
10
10
10
10
10
25
10
25
25
10
10
10
10
10
25
10
10
Tetrachlorobiphenyls
2,2',3,3'-TeCB
2,2',3,4-TeCB
2,2',3,4'-TeCB
2,2',3,5-TeCB
2,2',3,5'-TeCB2
2,2',3,6-TeCB
2,2',3,6'-TeCB
40
41
42
43
44
45
46
500
500
200
200
500
200
200
50
50
20
20
50
20
20
25
25
10
10
25
10
10
-------
Table 1. Target Compound List (TCP and
Contract Required Ouantitation Limits (CROLs) Con't
CB Congener1
2,2',4,4'-TeCB
2,2',4,5-TeCB
2,2',4,5'-TeCB
2,2',4,6-TeCB
2,2',4,6'-TeCB
2,2',5,5'-TeCB2
2,2',5,6'-TeCB
2,2',6,6'-TeCB
2,3,3',4'-TeCB
2,3,3',4'-TeCB
2,3,3',5-TeCB
2,3,3',5'-TeCB
2,3,3',6-TeCB
2,3,4,4'-TeCB
2,3,4,5-TeCB
2,3,4,6-TeCB
2,3,4',5-TeCB
2,3,4',6-TeCB
2,3,5,6-TeCB
2,3',4,4'-TeCB2
2,3',4,5-TeCB
2,3',4,5'-TeCB
2,3',4,6-TeCB
2,3',4',5-TeCB
2,3',4',6-TeCB
2,3',5,5'-TeCB
2,3',5',6-TeCB
2,4,4',5-TeCB
2,4,4',6-TeCB
2',3,4,5-TeCB
3,3',4,4'-TeCB2'3
3,3',4,5-TeCB
3,3',4,5'-TeCB
3,3',5,5'-TeCB
3,4,4',5-TeCB3
IUPAC
Number
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
80
81
Water (pg/L)
500
200
500
200
200
500
200
500
500
200
500
500
200
500
500
200
500
200
500
500
500
500
500
500
500
500
500
500
200
500
500
500
500
500
500
Other (ng/kg)
50
20
50
20
20
50
20
50
50
20
50
50
20
50
50
20
50
20
50
50
50
50
50
50
50
50
50
50
20
50
50
50
50
50
50
Extract (pg/uL)
25
10
25
10
10
25
10
25
25
10
25
25
10
25
25
10
25
10
25
25
25
25
25
25
25
25
25
25
10
25
25
25
25
25
25
Pentachlorobiphenyls
2,2',3,3',4-PeCB
2,2',3,3',5-PeCB
2,2',3,3',6-PeCB
2,2',3,4,4'-PeCB
2,2',3,4,5-PeCB
2,2',3,4,5'-PeCB
2,2',3,4,6-PeCB
2,2',3,4,6'-PeCB
2,2',3,4',5-PeCB
2,2',3,4',6-PeCB
2,2',3,5,5'-PeCB
2,2',3,5,6-PeCB
2,2',3,5,6'-PeCB
82
83
84
85
86
87
88
89
90
91
92
93
94
500
500
500
200
500
500
500
500
1000
500
500
500
500
50
50
50
20
50
50
50
50
100
50
50
50
50
25
25
25
10
25
25
25
25
50
25
25
25
25
-------
Table 1. Target Compound List (TCP and
Contract Required Ouantitation Limits (CROLs) Con't
CB Congener1
2,2',3,5',6-PeCB
2,2',3,6,6'-PeCB
2,2',3',4,5-PeCB
2,2',3',4,6-PeCB
2,2',4,4',5-PeCB
2,2',4,4',6-PeCB
2,2',4,5,5'-PeCB2
2,2',4,5,6'-PeCB
2,2',4,5,'6-PeCB
2,2',4,6,6'-PeCB
2,3,3',4,4'-PeCB2-3
2,3,3',4,5-PeCB
2,3,3',4',5-PeCB
2,3,3',4,5'-PeCB
2,3,3',4,6-PeCB
2,3,3',4',6-PeCB
2,3,3',5,5'-PeCB
2,3,3',5,6-PeCB
2,3,3',5',6-PeCB
2,3,4,4',5-PeCB3
2,3,4,4',6-PeCB
2,3,4,5,6-PeCB
2,3,4',5,6-PeCB
2,3',4,4',5-PeCB2'3
2,3',4,4',6-PeCB
2,3',4,5,5'-PeCB
2,3',4,5,'6-PeCB
2',3,3',4,5-PeCB
2',3,4,4',5-PeCB3
2',3,4,5,5'-PeCB
2',3,4,5,6'-PeCB
3,3',4,4',5-PeCB2'3
3,3',4,5,5'-PeCB
IUPAC
Number
95
96
97
98
99
100
101
102
103
104
105
106
107
108
109
110
111
112
113
114
115
116
117
118
119
120
121
122
123
124
125
126
127
Water (pg/L)
500
500
500
500
500
500
1000
500
500
500
200
500
1000
500
200
1000
1000
1000
1000
500
1000
200
200
500
500
500
500
500
500
1000
500
500
1000
Other (ng/kg)
50
50
50
50
50
50
100
50
50
50
20
50
100
50
20
100
100
100
100
50
100
20
20
50
50
50
50
50
50
100
50
50
100
Extract (pg/fiL)
25
25
25
25
25
25
50
25
25
25
10
25
50
25
10
50
50
50
50
25
50
10
10
25
25
25
25
25
25
50
25
25
50
Hexachlorobiphenyls
2,2',3,3',4,4'-HxCB2
2,2',3,3',4,5-HxCB
2,2',3,3',4,5'-HxCB
2,2',3,3',4,6-HxCB
2,2',3,3',4,6'-HxCB
2,2',3,3',5,5'-HxCB
2,2',3,3',5,6-HxCB
2,2',3,3',5,6'-HxCB
2,2',3,3',6,6'-HxCB
2,2',3,4,4',5-HxCB
2,2',3,4,4',5'-HxCB2
2,2',3,4,4',6-HxCB
2,2',3,4,4',6'-HxCB
2,2',3,4,5,5'-HxCB
2,2',3,4,5,6-HxCB
2,2',3,4,5,6'-HxCB
2,2',3,4,5',6-HxCB
128
129
130
131
132
133
134
135
136
137
138
139
140
141
142
143
144
500
500
500
500
500
500
500
500
200
1000
500
500
500
200
1000
500
500
50
50
50
50
50
50
50
50
20
100
50
50
50
20
100
50
50
25
25
25
25
25
25
25
25
10
50
25
25
25
10
50
25
25
-------
Table 1. Target Compound List (TCP and
Contract Required Ouantitation Limits (CROLs) Con't
CB Congener1
2,2',3,4,6,6'-HxCB
2,2',3,4',5,5'-HxCB
2,2',3,4',5,6-HxCB
2,2',3,4',5,6',-HxCB
2,2',3,4',5',6-HxCB
2,2',3,4',6,6'-HxCB
2,2',3,5,5',6-HxCB
2,2',3,5,6,6'-HxCB
2,2',4,4',5,5'-HxCB2
2,2',4,4',5',6-HxCB
2,2',4,4',6,6'-HxCB
2,3,3',4,4',5-HxCBJ
2,3,3',4,4',5'-HxCB3
2,3,3',4,4',6-HxCB
2,3,3',4,5,5'-HxCB
2,3,3',4,5,6-HxCB
2,3,3',4,5',6-HxCB
2,3,3',4',5,5'-HxCB
2,3,3',4',5,6-HxCB
2,3,3',4',5',6-HxCB
2,3,3',5,5',6-HxCB
2,3,4,4',5,6-HxCB
2,3',4,4',5,5'-HxCB3
2,3',4,4',5',6-HxCB
3,3',4,4',5,5'-HxCB2'3
Heptachlorobiphenyls
2,2',3,3',4,4',5-HpCB2
2,2'3,3',4,4',6-HpCB
2,2',3,3',4,5,5'-HpCB
2,2',3,3',4,5,6-HpCB
2,2',3,3',4,5,6'-HpCB
2,2',3,3',4,5',6-HpCB
2,2',3,3',4,6,6'-HpCB
2,2',3,3',4',5,6-HpCB
2,2',3,3',5,5',6-HpCB
2,2',3,3',5,6,6'-HpCB
2,2',3,4,4',5,5'-HpCB2
2,2',3,4,4',5,6-HpCB
2,2',3,4,4',5,6'-HpCB
2,2',3,4,4',5',6-HpCB
2,2',3,4,4',6,6'-HpCB
2,2',3,4,5,5',6-HpCB
2,2',3,4,5,6,6'-HpCB
2,2',3,4',5,5',6-HpCB2
2,2',3,4',5,6,6'-HpCB
2,3,3',4,4',5,5'-HpCB3
2,3,3',4,4',5,6-HpCB
2,3,3',4,4',5',6-HpCB
2,3,3',4,5,5',6-HpCB
2,3,3',4',5,5',6-HpCB
IUPAC
Number
145
146
147
148
149
150
151
152
153
154
155
156
157
158
159
160
161
162
163
164
165
166
167
168
169
170
171
172
173
174
175
176
177
178
179
180
181
182
183
184
185
186
187
188
189
190
191
192
193
Water (pg/L)
1000
500
500
1000
500
1000
500
1000
500
500
1000
500
500
200
1000
500
1000
1000
500
500
1000
500
500
500
500
500
1000
1000
1000
500
1000
1000
500
500
500
500
1000
1000
1000
1000
1000
1000
500
500
500
500
1000
1000
500
Other (ng/kg)
100
50
50
100
50
100
50
100
50
50
100
50
50
20
100
50
100
100
50
50
100
50
50
50
50
50
100
100
100
50
100
100
50
50
50
50
100
100
100
100
100
100
50
50
50
50
100
100
50
Extract (pg/fiL)
50
25
25
50
25
50
25
50
25
25
50
25
25
10
50
25
50
50
25
25
50
25
25
25
25
25
50
50
50
25
50
50
25
25
25
25
50
50
50
50
50
50
25
25
25
25
50
50
25
-------
Table 1. Target Compound List (TCP and
Contract Required Ouantitation Limits (CROLs) Con't
CB Congener1
Octachlorobiphenyls
2,2',3,3',4,4',5,5'-OcCB
2,2',3,3',4,4',5,6-OcCB2
2,2',3,3',4,4',5,6'-OcCB
2,2',3,3',4,4',6,6'-OcCB
2,2',3,3',4,5,5',6-OcCB
2,2',3,3',4,5,5',6'-OcCB
2,2',3,3',4,5,6,6'-OcCB
2,2',3,3',4,5',6,6'-OcCB
2,2',3,3',5,5',6,6'-OcCB
2,2',3,4,4',5,5',6-OcCB
2,2',3,4,4',5,6,6'-OcCB
2,3,3',4,4',5,5',6-OcCB
Nonachlorobiphenyls
2,2',3,3',4,4',5,5',6-NoCB2
2,2',3,3',4,4',5,6,6'-NoCB
2,2',3,3',4,5,5',6,6'-NoCB
Decachlorobiphenyls
DeCB2
IUPAC
Number
194
195
196
197
198
199
200
201
202
203
204
205
206
207
208
209
Water (pg/L)
500
1000
1000
1000
500
500
1000
1000
1000
1000
1000
1000
1000
1000
1000
500
Other (ng/kg)
50
100
100
100
50
50
100
100
100
100
100
100
100
100
100
50
Extract (pg/uL)
25
50
50
50
25
25
50
50
50
50
50
50
50
50
50
25
'Abbreviations for chlorination levels:
MoCB = monochlorobiphenyl
DiCB = dichlorobiphenyl
TrCB = trichlorobiphenyl
TeCB = tetrachlorbiphenyl
PeCB = pentachlorobiphenyl
HxCB = hexachlorobiphenyl
HpCB = heptachlorobiphenyl
OcCB = octachlorobiphenyl
NoCB = nonachlorobiphenyl
DeCB = decachlorobiphenyl
National Oceanic and Atmospheric Administration (NOAA) Congener of Interest.
3World Health Organization (WHO) Toxic Congener.
NOTE: The values in these tables are quantitation limits, not absolute detection limits. The amount of material necessary to
produce a detector response that can be identified and reliably quantified is greater than that needed to be simply
detected above the background noise. The quantitation limits in these tables are set at the concentrations in the sample
equivalent to the concentration of the lowest calibration standard analyzed for each analyte.
Specific quantitation limits are highly matrix-dependent. The quantitation limits listed herein are provided for guidance and may
not always be achievable.
These CRQL values are based on the analysis of samples according to the specifications given in the CB congeners SOW. Sample
data are reported on a dry weight basis for all non-aqueous samples [except tissues which are reported on a wet weight basis, along
with their Percent Lipid (% Lipid) content].
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Table 2. Methods and Instruments
Matrix
Water
Soil/Sediment
Non-Human Tissue
Preparation Method
Using Solid-Phase Extraction (SPE):
Vacuum-filtered through glass fiber on top of
an SPE disk; fiber and disk extraction.
Using Separatory Funnel Extraction
(SFE): Filtrate extraction with methylene
chloride using a separatory funnel.
Using Continuous Liquid-Liquid
Extraction (CLLE): Filtrate extraction with
methylene chloride using a continuous
liquid-liquid extractor.
Extraction with toluene in a Soxhlet/Dean-
Stark (SDS) extractor.
Extraction with methylene chloride using an
SDS extractor for 18-24 hours.
Analytical Instrument
HRGC/HRMS analysis
HRGC/HRMS analysis
HRGC/HRMS analysis
Table 3. Quality Control (PC)
QC Operation
Frequency
ANALYSES
High Resolution Mass Spectrometry (HRMS) System
Tune
Window-Defining Mixture (WDM)
Initial Calibration
Continuing Calibration Verification (CCV):
Mid-Point Calibration Standard (CSS) Relative
Response (RR) and Relative Response Factor (RRF)
Prior to the analysis of calibration standards, Initial
Precision and Recovery (IPR) standards, samples, and
blanks within each 12-hour period.
Following the HRMS system tune and at the beginning
of each 12-hour period for each instrument used for
analysis during which standards or samples are
analyzed; precedes initial calibration, continuing
calibration, and whenever adjustments or instrument
maintenance activities are performed that may affect
Retention Times (RTs).
Upon contract award, during initial setup of each
instrument used prior to analysis of samples and
required blanks, and each time calibration verification
fails to meet the technical acceptance criteria.
At the beginning of each 12-hour period after the
HRMS system tune during which sample data are
collected and at the end of each 12-hour period.
STANDARDS
Internal Standards
Clean-Up Standard
Labeled Toxic and Level of Chlorination (LOG)
Chlorinated Biphenyls (CBs)
Added to all extracts prior to analysis.
Added to all extracts prior to cleanup.
Added to all samples including blanks, LCSs, and PE
samples prior to extraction.
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Table 3. Quality Control (QC) Con't
QC Operation
Frequency
BLANKS
Performance Evaluation (PE) Samples
Laboratory Control Sample (LCS)
Method Blank
Prepared and analyzed (if provided) with each group of
20 field samples or less.
Prepared and analyzed with each group of 20 field
samples or less of a similar matrix in an SDG.
Prepared and analyzed with each group of 20 field
samples or less, or each time samples are extracted.
INSTRUMENT CALIBRATION
Gel Permeation Chromatography (GPC) Calibration
NOTE: Optional for water extracts only; should be
used for soil/sediment and non-human tissue
Verified after every 20 extracts.
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
evaluations, electronic data audits, data package audits,
HRGC/HRMS tape audits, and evaluates laboratory
performance through the use of blind Performance
Evaluation (PE) samples.
CONTACTING EPA
For more information, or to submit suggestions to
improve this analytical service, please contact:
Elizabeth Holman
EPA/ASB
Ariel Rios Building (5102G)
1200 Pennsylvania Ave, N.W.
Washington, DC 20460
703-603-8761
FAX: 703-603-9116
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