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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