Polychlorinated Biphenyls (PCBs)

Detection and Site Characterization

PCB analysis can be performed in the field or at a fixed laboratory using a variety of techniques. PCB immunoassay kits utilize analyte-specific antibodies to bind and remove PCBs from complex sample matrices. The process is colorimetric in nature with the change in color indicting approximate concentrations. The color change can be measured using an instrument (e.g., spectrophotometer) or visual color card. Soil samples require an extraction step that can be difficult with very fine-grained materials. The kits are generally calibrated against a specific Aroclor standard (e.g., 1254) but are not able to differentiate between Aroclors. Also, some Aroclors respond better than others. The test can be used as a screening tool during cleanups where a specific cleanup goal such as 1 ppm or 10 ppm has been set and analysis is done to determine whether the contaminant level is above or below the goal. Analysis time varies but can take over 30 minutes per sample.

Ion-specific analysis uses a chloride-specific electrode to measure the amount of chlorine in a sample extract that has been treated with sodium to strip the chlorine from the biphenyl compound. It is a screening tool and does not differentiate between Aroclors. Greater accuracy is obtained when the target Aroclor is known before using the electrode system.

Gas chromatography (GC) is an accepted technique (SW-846, Method 8082) for quantitatively determining both congeners and Aroclor types. It is the most sensitive of the available methods with method detection limits ranging from 0.054 to 0.9 µg/L for water and 57 to 70 µg/kg for soil. When used in a screening mode (i.e., less rigorous QA/QC than required in Method 8082), a portable GC in the field can run 30 to 40 samples a day; however, the microextraction techniques usually employed in the field sampling will result in slightly higher detection limits.

Gas chromatography coupled with mass spectrometry (GC/MS) also can be used to quantitatively determine both congeners and Aroclor types but with somewhat higher detection levels than those provided by GC alone. While GC/MS equipment generally is associated with fixed laboratory facilities, it can be deployed to the field in a mobile laboratory, and portable equipment also is available. Throughput for standard GC/MS instruments deployed in the field generally is 13 to 16 samples per day.

Adapted from:

SW 846: Test Methods for Evaluating Solid Wastes: Physical/Chemical Methods, 3rd Edition

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Field Analysis

Case Study of the Triad Approach: Expedited Characterization of Petroleum Constituents and PCBs Using Test Kits and a Mobile Chromatography Laboratory at the Former Cos Cob Power Plant Site
U.S. EPA, Brownfields Technology Support Center, in cooperation with Region 1 and Metcalf & Eddy.
EPA 542-R-04-008, 116 pp, June 2004.

Field Analytical Screening Program: PCB Method Innovative Technology Evaluation Report
U.S. EPA, Office of Research and Development.
EPA 540-R-95-521, 47 pp, 1995.

Field Screening Method for Polychlorinated Biphenyl Compounds in Water
U.S. EPA, Office of Research and Development.
EPA 540-R-94-519, 34 pp, Oct 1994

Innovations in Site Characterization: Case Study: Dexsil L2000 PCB/Chloride Analyzer for Drum Surfaces
U.S. EPA, Technology Innovation Office.
EPA 542-R-99-003, 48 pp, May 1999

Method 4020: Screening for Polychlorinated Biphenyls by Immunoassay
Test Methods for Evaluating Solid Wastes: Physical/Chemical Methods, 3rd Edition SW-846.
U.S. EPA, Office of Solid Waste.

U.S. EPA Environmental Technology Verification (ETV) Program Verifications

Contact: Teresa Harten, harten.teresa@epa.gov or Eric Koglin, koglin.eric@epa.gov

Laboratory Analysis

40 CFR 136—Guidelines Establishing Test Procedures for the Analysis of Pollutants, Appendix A Code of Federal Regulations.

Method 608—Organochlorine Pesticides And PCBs
Method 625—Base/Neutrals and Acids

Method 1668, Revision A: Chlorinated Biphenyl Congeners in Water, Soil, Sediment, and Tissue by HRGC/HRMS
U.S. EPA, Office of Water.
EPA 821-R-00-002, 133 pp, 1999.

NIOSH Manual of Analytical Methods (NMAM®), 4th Edition
National Institute for Occupational Safety and Health, Publication 94-113, 1994.
Contact: Paula Fey O'Connor, pfo1@cdc.gov

Method 5503: Polychlorinated Biphenyls

Method TO-10A: Determination of Pesticides and Polychlorinated Biphenyls in Ambient Air Using Low Volume Polyurethane Foam (PUF) Sampling Followed by Gas Chromatographic/Multi-Detector Detection (GC/MD)
Compendium of Methods for the Determination of Toxic Organic Compounds in Ambient Air, Second Edition.
U.S. EPA, Office of Research and Development.
EPA 625-R-96-010b, 37 pp, 1999.

Polychlorinated Biphenyls (PCB) Training Tool
U.S. Navy, Naval Facilities Engineering Command, Environmental Restoration Technology Transfer, Multimedia Training Tools website, 34 pp.

This PCB Training Tool is a multimedia desktop primer designed to give remedial project managers information on PCBs. Topics addressed in this training include the history of PCBs, environmental fate and transport, nomenclature, laboratory test methods, data objectives, and questions to ask the laboratory. Knowing the project's data and information needs, data quality objectives, and the capabilities of a particular laboratory will enable the project manager to choose the right PCB analysis for a site. The entire primer takes about 30 minutes to complete, but individual topics of interest can selected for viewing.

Polychlorinated Biphenyls (PCB) Training Tool Data Sheet
U.S. Navy, Naval Facilities Engineering Command, Environmental Restoration Technology Transfer, Multimedia Training Tools website, 4 pp.

The PCB Training Tool is an interactive, Web-based resource prepared by the Naval Facilities Engineering Command. This brief data sheet is designed to familiarize the user with PCB history and nomenclature and to provide information about cost and data quality differences among PCB analyses.

Test Methods for Evaluating Solid Wastes: Physical/Chemical Methods, 3rd Edition
U.S. EPA, SW-846.

This is the main webpage for SW 846. Section 3000 contains sample preparation methods for semi-volatile organics. The ones identified below specifically describe PCBs. Other 3000 preparation methods for semi-volatile organics also may be applicable to PCBs. Section 4000 contains immunoassay techniques and section 8000 contains the more conventional test methods.

Method 3535: A Solid Phase Extraction
Method 3562: Supercritical Fluid Extraction
Method 4020: Screening for Polychlorinated Biphenyls by Immunoassay
Method 4425: Screening Extracts of Environmental Samples for Planar Organic Compounds (PAHs, PCBs, PCDDs/PCDFs) by a Reporter Gene On a Human Cell Line
Method 8082a : Polychlorinated Biphenyls (PCBs) by Gas Chromatography Method 8270d: Semivolatile Organic Compounds by Gas Chromatography/Mass Spectrometry (GC/MS)
Method 8275a: Semivolatile Organic Compounds (PAHs and PCBs) in Soils/sludges and Solid Wastes Using Thermal Extraction/gas Chromatography/mass Spectrometry (TE/GC/MS)

Update on the Benefits of PCB Congener-Specific Analyses
Burkhard, L., EPA Office of Research and Development Ecological Risk Assessment Support Center (ERASC), EPA-600-R-21-237, 30 pp, 2021.

In April 2020, the Ecological Risk Assessment Forum submitted a request to the ERASC to review the ERASC Memorandum: Response to Ecological Risk Assessment Forum Request for Information on The Benefits of PCB Congener-Specific Analyses was developed in March 2005. Specifically, a review was needed to 1) ensure that the memorandum reflects the latest state of the science and 2) update the information as needed. Results of analyses for PCB contamination on environmental matrices may be expressed in terms of PCB congener-specific, total PCB, and Aroclor equivalent concentrations. The cost ramifications, potential overlap in results from each analysis, and whether reporting results of all three types of analyses should be the standard approach are discussed. The update is designed to assist risk assessment practitioners in choosing cost-effective analyses that meet the objectives of the assessment.

USEPA Contract Laboratory Program Statement of Work for Organics Analysis Multi-Media, Multi-Concentration SOM01.2
U.S. EPA, 2007.

USEPA Contract Laboratory Program Statement of Work for Organics Exhibit D Analytical Method for the Analysis of Aroclors
U.S. EPA, 66 pp, 2005

Sampling

Cross Validation of Two Partitioning-Based Sampling Approaches in Mesocosms Containing PCB Contaminated Field Sediment, Biota, and Activated Carbon Amendment
Schmidt, S., A. Wang, P. Gidley, A. Wooley, G. Lotufo, R. Burgess, U. Ghosh, L. Fernandez, and P. Mayer. Environmental Science & Technology 51(17):9996-10004(2017) [Abstract]

This study compared two passive sampling-based approaches—(1) ex situ equilibrium sampling with multiple thicknesses of silicone and (2) in situ pre-equilibrium sampling with LDPE loaded with performance reference compounds—for measuring the bioavailable concentrations of PCBs in contaminated sediments. The study demonstrated that the two methods generated similar results. This information provides environmental managers with the ability to select between these two methods (depending on the circumstances) and know that the results will be comparable.

Validation Studies on Activated Carbon Fiber Passive Sampler for PCDD/FS and PCBs in Water
Cerasa, M., P. Benedetti, A. De Stefanis, E. Guerriero, S. Mosca, A. Bacaloni, and M. Rotatori.
Chemosphere 239:124666(2020) [Abstract]

A characterization and validation study was conducted on activated carbon filters (ACF) to monitor for PCBs, polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) in water. The validity of using the ACF as solid-phase extraction and as passive sampler was evaluated by the percentage recovery (R %) of ¹³C₁₂-labeled standards of PCDD/Fs and PCBs added in a known volume of water. When compared to the R% of liquid-liquid extraction, the authors suggest the method has a better reproducibility of results and is capable of satisfying the extraction requirements of EPA reference methods.

Other

Analysis of PCB Congeners vs. Arcolors [sic] in Ecological Risk Assessment
T. Bernhard and S. Petron, Depart of Defense, 7 pp, 2001.

Determination of Polychlorinated Biphenyls (PCBs) in Sediment and Biota
Webster, L., P. Roose, P. Bersuder, M. Kotterman, M. Haarich, and K. Vorkamp.
ICES Techniques in Marine Environmental Sciences, No. 53, 23 pp, 2013

The determination of PCBs in sediment and biota generally involves extraction with organic solvents, cleanup, and gas chromatographic separation with electron capture detection or mass spectrometry. Due to the low concentrations of non-ortho-substituted PCBs compared to those of other PCBs, their determination may require an additional separation step. All stages of the procedure are susceptible to insufficient recovery and/or contamination; therefore, quality control procedures are important in order to check method performance.

Environmental Forensics: Contaminant-Specific Guide
Robert D. Morrison and Brian Murphy.
Elsevier Academic Press, Boston. ISBN: 0125077513, 576 pp, 2006

Environmental forensics is the application of scientific techniques for the purpose of identifying the source and age of a contaminant. This book discusses the following contaminants and contaminant groups: mercury, asbestos, lead, chromium, methane, radioactive compounds, pesticides, perchlorate, polychlorinated biphenyls, arsenic, chlorinated solvents, polyaromatic hydrocarbons, crude oil, gasoline, microbes, and compounds found in sewage.

Evaluation of Dredged Material Proposed for Discharge in Waters of the U.S.: Testing Manual (The Inland Testing Manual)
U.S. EPA, Office of Water, and U.S. Army Corps of Engineers.
EPA 823-B-98-004, 571 pp, 1998.

Evaluation of Dredged Material Proposed for Ocean Disposal Testing Manual
U.S. EPA, Office of Water, and U.S. Army Corps of Engineers.
EPA 503/8-91/001, 214 pp, 1991.

A Handbook for Determining the Sources of PCB Contamination in Sediments
NAVFAC Engineering and Expeditionary Warfare Center.
TR-NAVFAC EXWC-EV-1302, 164 pp, 2012

This guide to conducting environmental forensic investigations for PCBs at sediment sites covers the following topics: (1) the general forensic approach, including relevant background information; (2) technical methods used in a PCB environmental forensics investigation; and (3) application of the procedures in two demonstration case studies.

Integrated Forensics Approach to Fingerprint PCB Sources in Sediments using Rapid Sediment Characterization (RSC) and Advanced Chemical Fingerprinting (ACF)
Leather, J., G. Durell, G. Johnson, and M. Mills.
ESTCP Project ER-200826, SPAWAR Technical Document 3262, 228 pp, 2012

An integrated approach to fingerprinting PCB contamination combines sediment screening technologies on a large number of field samples followed by detailed PCB congener analysis in conjunction with advanced chemical fingerprinting data interpretation on a subset of selected laboratory samples. All the techniques discussed in this report are commercially available from multiple sources. See also the ESTCP Cost and Performance Report ; PAH/PCB Fingerprinting Tool

PCB Method Comparison of High and Low Resolution Sediment Analysis
Coots, R.
Washington Dept. of Ecology, Publication 14-03-009 , 72 pp, 2014

Ten archived marine and freshwater sediment samples from cleanup projects with known PCB concentrations were split three ways and analyzed by congeners (high resolution), homologs (low resolution), and Aroclor methods. Detection limits varied between methods, with estimated sample detection limits for congeners averaging about 50 times lower than those reported for homologs and over 400 times lower than Aroclors. A strong statistical relationship was noted for total PCBs determined by congener analysis compared to either the homolog analysis or the same dataset Kaplan and Meier adjusted to account for nondetects. When total PCB Aroclors were compared to high resolution congeners, a weaker yet still strong relationship was reported.

QA/QC Guidance for Sampling and Analysis of Sediments Water and Tissue for Dredged Material Evaluation, Phase I: Chemical Evaluations
U.S. EPA, Office of Water.
EPA 823-B-95-001, 269 pp, 1995.

Performance-Based, Cost- and Time-Effective PCB Analytical Methodology
Alvarado, J., Argonne National Laboratory, 12 pp, 1998.
Contact: Jorge S. Alvarado, JAlvarado@anl.gov

Protocol for Sampling and Testing at PCB Storage Sites in Ontario
Ontario Ministry of the Environment, 27 pp, 2000.

Analytical Methods
ATSDR Toxicological Profile for Polychlorinated Biphenyls (PCBs), Chapter 7, 2000.
Agency for Toxic Substances and Disease Registry.

U.S. EPA Region 4 Technical Services Section Issue Paper for Polychlorinated Biphenyl Characterization at Region 4 Superfund and RCRA Sites: Technical Services Section Issue
Wischkaemper, H.K., A.F. Beliveau, and R.W. Henderson.
U.S. EPA Region 4, 78 pp, 2013

This issue paper helps the site project manager begin the process of planning the site characterization using appropriate analytical procedures on adequate samples, with the endpoint being that defensible data are available to support sound decision-making at complicated PCB-contaminated sites. Characterization of groundwater, soil, and sediment for PCBs is unique because of the varied site conceptual models for PCB and PCB mixture migration and the specific analytical requirements to evaluate the presence and extent of PCB contamination.

Verification of PCB Spill Cleanup by Sampling and Analysis
U.S. EPA, Office of Toxic Substances.
EPA 560-5-85-026, 74 pp, 1985.
Contact: John Smith, smith.johnh@epa.gov

Toxicity

Generating the Right PCB Data: Determination of Aroclors Versus PCB Congeners
Narquis, C.T., J.E. Hyatt, and A.L. Prignano.
HNF-34789-FP, 13 pp, 2007

PCBs can be analyzed and quantified either as Aroclor mixtures or as individual congeners. In general, most cleanup regulations pertaining to PCBs are based on total PCB concentrations using Aroclor analyses. Congener analysis is relatively new to environmental cleanup and restoration due to both technical issues and associated cost. This paper defines Aroclors and congeners and compares the current application and usefulness of the two analytical methods for environmental restoration and cleanup and includes a strategy for the best use of the two methods to optimize overall characterization cost.

Methods for Measuring the Toxicity and Bioaccumulation of Sediment-Associated Contaminants with Freshwater Invertebrates, Second Ed.
U.S. EPA, Office or Research and Development and Office of Water.
EPA 600-R-99-064, 212 pp, 2000.

Methods for Assessing the Toxicity of Sediment-Associated Contaminants with Estuarine and Marine Amphipods
U.S. EPA, Office of Research and Development.
EPA 600-R-94-025, 156 pp, 1994.

Short-Term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Water to Freshwater Organisms, Third Ed.
U.S. EPA, Office of Research and Development.
EPA 600-4-91-002, 334 pp, 1994.

Short-Term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Water to Marine and Estuarine Organisms, Second Ed.
U.S. EPA, Office of Research and Development.
EPA 600-4-91-003, 516 pp, 1994.

Literature References

Measurement and Monitoring Technologies for the 21st Century Initiative (21M²) Literature Search
Through the Measurement and Monitoring Technologies for the 21st Century initiative, EPA's Office of Solid Waste and Emergency Response (OSWER) will identify and deploy promising measurement and monitoring technologies in response to waste management and site cleanup program needs by matching existing and emerging technologies with OSWER program and client needs.

U.S. EPA Contaminated Site Cleanup Information (CLU-IN)

Polychlorinated Biphenyls (PCBs)

Detection and Site Characterization