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


U.S. Environmental Protection Agency
U.S. EPA Technology Innovation and Field Services Division

Sediments

Site Characterization

Analytical Methods

Generally, the analyses of sediment and water samples conform to standard laboratory procedures, such those found in SW-846 or the Contract Laboratory Statement of Work. A list of methods that are specific to many of the contaminants of concern in sediments can be found in the detection and characterization sections of Contaminant Focus. Some sediment characteristics, such as marine salinity, may require modification of the analytical or preparation methods.

A comprehensive list of laboratory methods, many of which pertain to sediment and biota analysis, can be found at the US Fish and Wildlife Analytical Control Facility Web site.


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Sediment Testing for Physical/Chemical Properties | Biota Analysis | Chemical Analysis | Toxicity Analyses

Sediment Testing for Physical/Chemical Properties

Adobe PDF LogoEvaluation of Dredged Material Proposed For Discharge in Waters of the U.S. - Testing Manual. Inland Testing Manual
USACE/USEPA, Office of Water, EPA-823/B-98/004, 571 pp, 1998

This manual describes laboratory techniques, test species, procedures, detection limits, and evaluation protocols representing the state of knowledge at publication. The document has a tiered approach to testing that is designed to provide the information needed to determine the potential for contaminant related impacts of proposed dredging discharges without necessitating unnecessary testing and evaluation.

Biota Analysis

Standard laboratory methods, such as those found in SW 846, may be used to analyze biota tissues for the presence of contaminants. Sample preparation procedures for biota tissues differ from those used for water and sediment sample analysis.

Adobe PDF LogoExtraction, Cleanup, and Gas Chromatography/Mass Spectrometry Analysis of Sediments and Tissues for Organic Contaminants
Sloan, C.A., D.W. Brown, R.W. Pearce, R.H. Boyer, J.L. Bolton, D.G. Burrows, D.P. Herman, and M.M. Krahn.
NOAA Tech. Memo. NMFS-NWFSC-59, 47 p, 2004.

Adobe PDF LogoReview of Field Validation Studies of Sediment Bioassays for the Regulatory Evaluation of Dredged Material
U.S. Army Corps of Engineers, ERDC TN-DOER-C23, 19 pp, 2001

Chemical Analysis

Field

Adobe PDF LogoAn In Situ Laser-Induced Fluorescence System for Polycylic Aromatic Hydrocarbon-Contaminated Sediments
Aldstadt, J., R.S. Germain, T. Grundl, and R. Schweitzer
USEPA, Great Lakes National Program Office, 54 pp, 2002

Adobe PDF LogoIntegrated Field-Screening for Rapid Sediment Characterization
ESTCP, Space and Naval Warfare Systems Center, San Diego, ESTCP Project #9717, 122 pp, 2000

This document provides an evaluation of the use of field portable X-ray fluorescence, UV fluorescence spectroscopy, and Quiksed for evaluating metals, the presence of PAHs, and sediment toxicity, respectively.

Laboratory

Adobe PDF Logo 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.

Adobe PDF LogoPassive PE Sampling in Support of In Situ Remediation of Contaminated Sediments: Standard Operating Procedure for PE Analysis
Gschwend, P., J. MacFarlane, K. Palaia, S. Reichenbacher, and D. Gouveia.
ESTCP Project ER-200915, 7 pp, 2012

This method describes procedures for chemical analysis of contaminants contained in polyethylene (PE) as deployed in polyethylene devices (PEDs) to sample hydrophobic organic compounds in aquatic and sediment environments. The procedure generates extracts suitable for high-resolution GC/MS analysis and is applicable to lab- or field-exposed PEDs.

Adobe PDF LogoPCB 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.

Adobe PDF LogoSW 846 Method 4430 Screening for Polychlorinated Dibenzo-P-Dioxins and Furans (PCDD/Fs) by Aryl Hydrocarbon-Receptor PCR Assay
USEPA, Office of Solid Waste, SW 846 Method 4430, 21 pp, 2007

Adobe PDF LogoSW-846 Method 8261A: Volatile Organic Compounds by Vacuum Distillation in Combination with Gas Chromatography/Mass Spectrometry (VD/GC/MS)
USEPA, Office of Solid Waste, 99 pp, 2006

This recommended version, which reflects an update of a previous version of this method, incorporates the latest available vacuum distillation equipment and is consistent with Method 8260C. The revised method is based on a vacuum distillation and cryogenic trapping procedure (Method 5032) and gas chromatography/mass spectrometry. It incorporates an internal standard-based matrix correction, involving the analysis of multiple internal standards to predict matrix effects. Normalization of the matrix effects makes Method 8261 analyses matrix independent and allows multiple matrices to be analyzed within a sample batch. As a result, the calculations involved are specific to this method and may not be used with data generated by another method. The method includes all of the necessary steps from sample preparation through instrumental analysis.

This method is used to determine the concentrations of volatile organic compounds, and some low-boiling semivolatile organic compounds, in nearly all matrices, including water, soil, sediment, sludge, oil, and animal tissue. Unlike Method 5032/8260, this method uses internal standards to measure matrix effects and compensates analyte responses for matrix effects. This method should be considered for samples where matrix effects are anticipated to severely impact analytical results.

Adobe PDF LogoSW-846 Method 8272: Parent and Alkyl Polycyclic Aromatics in Sediment Pore Water by Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry in Selected Ion Monitoring Mode
USEPA, Office of Solid Waste, 34 pp, 2007

EPA's narcosis model for benthic organisms in sediments contaminated with PAHs is based on the concentrations of dissolved PAHs in the interstitial water or pore water of the sediment. Method 8272 covers the separation of pore water from PAH-impacted sediment samples, the removal of colloids, and the subsequent measurement of dissolved concentrations of the 10-parent PAHs and two alkylated daughter PAHs in the pore water samples. This method directly determines the concentrations of dissolved PAHs in environmental sediment pore water, groundwater, and other water samples using solid-phase microextraction for static sample collection followed by desorption into a gas chromatograph equipped with a mass spectrometric detector operated in the selected ion monitoring mode for analyte identification and quantitation.

Toxicity Analyses

Field

Adobe PDF LogoIntegrated Field-Screening for Rapid Sediment Characterization
ESTCP, Space and Naval Warfare Systems Center, San Diego, ESTCP Project #9717, 122 pp, 2000

This document evaluates the use of field portable X-ray fluorescence, UV fluorescence spectroscopy, and Quiksed for evaluating metals, the presence of PAHs, and sediment toxicity, respectively.

Adobe PDF LogoUse of Sediment Quality Guidelines and Related Tools for the Assessment of Contaminated Sediments Executive Summary Booklet of a SETAC Pellston Workshop
Wenning, R.J. and C.G. Ingersoll (eds.)
SETAC, 48 pp, 2002

This workshop focused on the evaluation of the scientific foundations supporting different chemically-based numeric sediment quality guidelines (SQGs) and methods to improve the integration of SQGs into different sediment quality assessment frameworks that include information derived from multiple chemical and biological lines of evidence.

Laboratory

Adobe PDF LogoConfounding Factors in Sediment Toxicology
Lapota, D., D. Duckworth, and J.Q. Word
SPAWAR, 19 pp, 2000

Bioassays, which are often required as part of an ecological risk assessment, often demonstrate toxicity that could lead to inaccurate conclusions and subsequently expensive remedial actions. Evidence of toxicity in sediments can often be caused by natural factors termed "false positives" or "confounding factors," such as ammonia, sulfide, or grain size, rather than actual contaminants of concern. The objective of this issue paper is to evaluate the natural factors that cause toxicity or false positives; identify, discuss, and optimize methods to measure or eliminate these factors; and identify and discuss standard and new cost-effective sediment toxicity bioassays.

Adobe PDF LogoThe Determination of Sediment Polycyclic Aromatic Hydrocarbon (PAH) Bioavailability Using Direct Pore Water Analysis by Solid-Phase Microextraction (SPME)
Geiger, S.C.
ESTCP Project ER-200709, 483 pp, 2010

Direct determination of PAH concentrations in dissolved sediment pore water using EPA method SW-8272 and ASTM provisional method D-7363-07 utilizes SPME on a very small sample of sediment (20 ml to <40 ml) to provide PAH concentration data. PAHs in sediments at the Washington Navy Yard, Washington, DC, were targeted for a demonstration of the SPME analytical method and the developed PAHs bioavailability assessment protocol.

Adobe PDF LogoDevelopment of Sediment Extracts for Rapid Assessment of Organic Contaminant Bioavailability
Price, C., et al.
USACE, ERDC/TN EEDP 02-31, 10 pp, 2003

This technical note describes the development of sediment extraction procedures for evaluating the bioaccumulation potential of non-polar organic contaminants from dredged material.

Adobe PDF LogoDevelopment of Marine Sediment Toxicity for Ordnance Compounds and Toxicity Identification Evaluation Studies at Select Naval Facilities
NAVFAC, NFESC Contract Report CR 01-002-ENV, 205 pp, 2000

Adobe PDF LogoDevelopment of a Rapid, Inexpensive Bioassay for Screening Contaminant Bioavailability in Sediment Using mRNA Profiling
Perkins, E., H. Fredrickson, and G. Lotufo
USACE, ERDC/TN EEDP-04-35, 8 pp, 2002

Adobe PDF LogoDredged Material Analysis Tools; Performance of Acute and Chronic Sediment Toxicity Methods
Steevens, Jeffery, Alan Kennedy, Daniel Farrar, Cory McNemar, Mark R. Reiss, Kropp, R.K., J. Doi, and T. Bridges
USACE, ERDC/EL TR-08-16, 73 pp, 2008

Adobe PDF LogoMethod for Assessing the Chronic Toxicity of Marine and Estuarine Sediment-associated Contaminants with Amphipod Leptocheirus plumulosus
USEPA and USACE, EPA/600/R-01/020, 130 pp, 2001

Adobe PDF LogoMethods for Measuring the Toxicity and Bioaccumulation of Sediment-Associated Contaminants with Freshwater Invertebrates, Second Edition
USEPA, Office of Research and Development and Office of Water, EPA/600/R-99/064, 212 pp, 2000

Adobe PDF LogoSW 846 Method 4435: Method for Toxic Equivalents (TEQS) Determinations for Dioxin-Like Chemical Activity with the CALUX® Bioassay
USEPA, Office of Solid Waste, 58 pp



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