United States Office of
Environmental Protection Solid Waste and
Agency Emergency Response
OSWER Document 9200.3-72FS
Publication EPA-540-FS-11-03
November 2011
&EPA Multi-Media, Multi-Concentration
Chlorinated Biphenyl Congeners
Analytical Service for Superfund
(CBC01.2)
Office of Superfund Remediation and Technology Innovation (OSRTI)
Analytical Services Branch (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 Chlorinated Biphenyl (CB)
Congeners that are analyzed using High Resolution Gas Chromatography/High Resolution Mass 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) CBC01.2 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. go v/superfund/programs/clp/cbc 1. htm
DATA USES
The CB congeners 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 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
CRQL is 20 pg/L. For solids and tissue samples, the
CRQL is 2.0 ng/kg. For extracts, the CRQL is 1.0
pg/uL. The specific CRQLs are highly matrix-
dependent. The CRQLs listed herein are provided for
guidance and may not always be achievable.
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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 1
L 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 HRGC. The analytes are separated
by the HRGC and detected by an HRMS. 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.
Laboratories must also submit the data electronically,
referred to as an Electronic Data Deliverable (EDD),
within the contract required TAT. Additional
information about EDD requirements are provided in
Exhibit H of the SOW, located at:
http://www.epa.gov/superfund/programs/clp/cbcl.htm.
EPA then processes the EDD through a web-based
data assessment tool - the Electronic Data exchange
and Evaluation System (EXES). EXES provides data
users with electronic data assessment/usability
reports and spreadsheets within 24 to 48 hours of data
receipt. EXES reports also facilitate the transfer of
analytical data into client databases. In addition to the
data assessment/usability reports, laboratories are
provided with a data assessment report documenting
instances of noncompliance.
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
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 in the SOW.
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CB Congener1
2,4'-DiCB2
2,2',5-TrCB2
2,4,4'-TrCB2
2,2',3,5'-TeCB2
2,2',5,5'-TeCB2
2,3',4,4'-TeCB2
3,3',4,4'-TeCB2'3
3,4,4',5-TeCB3
2,2',4,5,5'-PeCB2
2,3,3',4,4'-PeCB2'3
2,3,4,4',5-PeCB3
2,3',4,4',5-PeCB2'3
2',3,4,4',5-PeCB3
3,3',4,4',5-PeCB2'3
2,2',3,3',4,4'-HxCB2
2,2',3,4,4',5'-HxCB2
2,2',4,4',5,5'-HxCB2
2,3,3',4,4',5-HxCB3
2,3,3',4,4',5'-HxCB3
2,3',4,4',5,5'-HxCB3
3,3',4,4',5,5'-HxCB2'3
2,2',3,3',4,4',5-HpCB2
2,2',3,4,4',5,5'-HpCB2
2,2',3,4',5,5',6-HpCB2
2,3,3',4,4',5,5'-HpCB3
2,2',3,3',4,4',5,6-OcCB2
2,2',3,3',4,4',5,5',6-NoCB2
DeCB2
All other non-dioxin-like congeners
Congener Number
PCB-8
PCB-18
PCB-28
PCB-44
PCB-52
PCB-66
PCB-77
PCB-8 1
PCB-101
PCB-105
PCB-114
PCB-118
PCB-123
PCB-126
PCB-128
PCB-138
PCB-153
PCB-156
PCB-157
PCB-167
PCB-169
PCB-170
PCB-180
PCB-187
PCB-189
PCB-195
PCB-206
PCB-209
-
CAS Number
34883-43-7
37680-65-2
7012-37-5
41464-39-5
35693-99-3
32598-10-0
32598-13-3
70362-50-4
37680-73-2
32598-14-4
74472-37-0
31508-00-6
65510-44-3
57465-28-8
38380-07-3
35065-28-2
35065-27-1
38380-08-4
69782-90-7
52663-72-6
32774-16-6
35065-30-6
35065-29-3
52663-68-0
39635-31-9
52663-78-2
40186-72-9
2051-24-3
-
Water
(PS/L)
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
20
CRQL4
Other
(ng/kg)
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
Extract
(pg/uL)
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
1.0
Abbreviations for chlorination levels:
MoCB = monochlorobiphenyl
DiCB = dichlorobiphenyl
TrCB = trichlorobiphenyl
TeCB = tetrachlorbiphenyl
PeCB = pentachlorobiphenyl
HxCB = hexachlorobiphenyl
HpCB = heptachlorobiphenyl
OcCB = octachlorobiphenyl
NoCB = nonachlorobiphenyl
DeCB = decachlorobiphenyl
2. National Oceanic and Atmospheric Administration (NCAA) Congener of Interest.
3. World Health Organization (WHO) Toxic Congener.
4. The CRQLs in this table are equivalent to the concentration of the low calibration (CS1) standard, assuming that all
sample weight, volumes, and cleanup procedures are performed according to Exhibit D of this SOW.
Specific quantitation limits are highly matrix-dependent. The quantitation limit listed herein is 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 Exhibit D. 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 Separately Funnel Extraction (SFE):
Filtrate extraction with methylene chloride using a
separately 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
HRGC/HRMS
HRGC/HRMS
Table 3. Quality Control (QC)
QC
Frequency
ANALYSES
HRMS System Tune
Window-Defining Mixture (WDM)
Prior to the analysis of calibration 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).
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Table 3. Quality Control (QC) (Con'f)
QC Operation
Initial Calibration
Continuing Calibration Verification (CCV): Mid-Point
Calibration Standard (CSS) Relative Response (RR) and
Relative Response Factor (RRF)
Frequency
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
Labeled Toxic and Level of Chlorination (LOG) Chlorinated
Biphenyls (CBs)
Cleanup Standards
Internal Standards
Added to all samples including blanks, LCSs, and PE
samples prior to extraction.
Added to all extracts prior to cleanup.
Added to all extracts prior to analysis.
BLANKS
Performance Evaluation (PE) Samples
Laboratory Control Sample (LCS)
Method Blank
Prepared and analyzed (if provided) with each set of 20 field
samples.
Prepared and analyzed with each group of 20 field samples
or less of a similar matrix in an SDG. LCS analysis precedes
analysis of samples from the same SDG.
Prepared and analyzed with each group of 20 field samples
or less, or each time samples are extracted to determine the
level of contamination associated with the processing and
analysis of samples. Method Blank analysis precedes
analysis of samples from the same SDG.
INSTRUMENT CALIBRATION
Gel Permeation Chromatography (GPC) Calibration
(optional)
Upon contract award, upon initial setup of instruments, when
the Gas Chromatography (GC) column is changed, when
channeling occurs, and once every 7 days when samples are
cleaned using GPC.
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:
Charlie Appleby
USEPA, OSWER/OSRTI/TIFSD/ASB
Ariel Rios Building (5203P)
1200 Pennsylvania Ave, N.W.
Washington, DC 20460
Phone (ASB): 703-347-0266
Phone (mobile): 703-405-0057
FAX: 703-603-9135
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