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5.1 Solvent extraction of soils and sediments can provide information on the availability of petroleum hydrocarbons to leaching, water quality changes, or other site conditions.5.2 Rapid heating, in combination with temperatures in excess of the atmospheric boiling point of acetone/hexane, reduces sample preparation or extraction times.5.3 Reduced amounts of solvents are required and solvent loss due to boiling and evaporation are eliminated by use of closed extraction vessels.1.1 This practice covers the solvent extraction of total petroleum hydrocarbon (TPH) from soils and sediments, using closed vessel microwave heating, for subsequent determination by gravimetric or gas chromatographic techniques.1.2 This practice is recommended only for solid samples that can pass through a ten mesh screen (approximately 2 mm openings).1.3 The solvent extract obtained by this practice may be analyzed for total or specific nonvolatile and semivolatile petroleum hydrocarbons but may require sample clean-up procedures prior to specific compound analysis.1.4 This practice is limited to solvents that are recommended for use in microwave solvent extraction systems.1.5 The values stated in SI units are to be regarded as standard.1.5.1 Exception—The inch-pound values given for units of pressure are to be regarded as standard; SI unit conversions are shown in parentheses.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 9.

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4.1 Partial extraction of soils and sediments can provide information on the availability of elements to leeching, water quality changes, or other site conditions.4.2 Rapid heating, in combination with temperatures in excess of the atmospheric boiling point of nitric acid, reduces sample preparation or reaction times.4.3 Little or no acids are lost to boiling or evaporation in the closed digestion vessel so additional portions of acid may not be required. Increased blank corrections from trace impurities in acid are minimized.1.1 This practice covers the digestion of soils and sediments for subsequent determination of acid-extractable concentrations of certain elements by such techniques as atomic absorption and atomic emission spectroscopy.1.1.1 Concentrations of arsenic, cadmium, copper, lead, magnesium, manganese, nickel, and zinc can be extracted from the preceding materials. Other elements may be determined using this practice.1.2 The analytical sample is arbitrarily defined as that which passes a 10-mesh (approximately 2 mm openings) screen and is prepared according to Practice D3974.1.3 Actual element quantitation can be accomplished by following the various test methods under other appropriate ASTM standards for element(s) of interest.1.4 The detection limit and linear concentration range for each element is dependent on the atomic absorption or emission spectrophotometric technique employed and may be found in the manual accompanying the instrument used.1.5 Before selecting a digestion technique, the user should consult the appropriate quantitation standard(s) for any special analytical considerations, and Practice D3974 for any special preparatory considerations.1.6 The extent of extraction of elements from soils and sediments by this method is dependent upon the physical and mineralogic characteristics of the prepared sample.1.7 The values stated in both inch-pound and SI units are to be regarded separately as the standard. The values given in parentheses are for information purposes only.1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 Sediment toxicity evaluations are a critical component of environmental quality and ecosystem impact assessments, and are used to meet a variety of research and regulatory objectives. The manner in which the sediments are collected, stored, characterized, and manipulated can influence the results of any sediment quality or process evaluation greatly. Addressing these variables in a systematic and uniform manner will aid the interpretations of sediment toxicity or bioaccumulation results and may allow comparisons between studies.5.2 Sediment quality assessment is an important component of water quality protection. Sediment assessments commonly include physicochemical characterization, toxicity tests or bioaccumulation tests, as well as benthic community analyses. The use of consistent sediment collection, manipulation, and storage methods will help provide high quality samples with which accurate data can be obtained for the national inventory and for other programs to prevent, remediate, and manage contaminated sediment.5.3 It is now widely known that the methods used in sample collection, transport, handling, storage, and manipulation of sediments and interstitial waters can influence the physicochemical properties and the results of chemical, toxicity, and bioaccumulation analyses. Addressing these variables in an appropriate and systematic manner will provide more accurate sediment quality data and facilitate comparisons among sediment studies.5.4 This standard provides current information and recommendations for collecting and handling sediments for physicochemical characterization and biological testing, using procedures that are most likely to maintain in situ conditions, most accurately represent the sediment in question, or satisfy particular needs, to help generate consistent, high quality data collection.5.5 This standard is intended to provide technical support to those who design or perform sediment quality studies under a variety of regulatory and non-regulatory programs. Information is provided concerning general sampling design considerations, field and laboratory facilities needed, safety, sampling equipment, sample storage and transport procedures, and sample manipulation issues common to chemical or toxicological analyses. Information contained in this standard reflects the knowledge and experience of several internationally-known sources including the Puget Sound Estuary Program (PSEP), Washington State Department of Ecology (WDE), United States Environmental Protection Agency (USEPA), US Army Corps of Engineers (USACE), National Oceanic and Atmospheric Administration (NOAA), and Environment Canada. This standard attempts to present a coherent set of recommendations on field sampling techniques and sediment or interstitial water sample processing based on the above sources, as well as extensive information in the peer-reviewed literature.5.6 As the scope of this standard is broad, it is impossible to adequately present detailed information on every aspect of sediment sampling and processing for all situations. Nor is such detailed guidance warranted because much of this information (for example, how to operate a particular sampling device or how to use a Geographical Positioning System (GPS) device) already exists in other published materials referenced in this standard.5.7 Given the above constraints, this standard: (1) presents a discussion of activities involved in sediment sampling and sample processing; (2) alerts the user to important issues that should be considered within each activity; and (3) gives recommendations on how to best address the issues raised such that appropriate samples are collected and analyzed. An attempt is made to alert the user to different considerations pertaining to sampling and sample processing depending on the objectives of the study (for example, remediation, dredged material evaluations or status and trends monitoring).5.8 The organization of this standard reflects the desire to give field personnel and managers a useful tool for choosing appropriate sampling locations, characterize those locations, collect and store samples, and manipulate those samples for analyses. Each section of this standard is written so that the reader can obtain information on only one activity or set of activities (for example, subsampling or sample processing), if desired, without necessarily reading the entire standard. Many sections are cross-referenced so that the reader is alerted to relevant issues that might be covered elsewhere in the standard. This is particularly important for certain chemical or toxicological applications in which appropriate sample processing or laboratory procedures are associated with specific field sampling procedures.5.9 The methods contained in this standard are widely applicable to any entity wishing to collect consistent, high quality sediment data. This standard does not provide guidance on how to implement any specific regulatory requirement, or design a particular sediment quality assessment, but rather it is a compilation of technical methods on how to best collect environmental samples that most appropriately address common sampling objectives.5.10 The information presented in this standard should not be viewed as the final statement on all the recommended procedures. Many of the topics addressed in this standard (for example, sediment holding time, formulated sediment composition, interstitial water collection and processing) are the subject of ongoing research. As data from sediment monitoring and research becomes available in the future, this standard will be updated as necessary.1.1 This guide covers procedures for obtaining, storing, characterizing, and manipulating marine, estuarine, and freshwater sediments, for use in laboratory sediment toxicity evaluations and describes samplers that can be used to collect sediment and benthic invertebrates (Annex A1). This standard is not meant to provide detailed guidance for all aspects of sediment assessments, such as chemical analyses or monitoring, geophysical characterization, or extractable phase and fractionation analyses. However, some of this information might have applications for some of these activities. A variety of methods are reviewed in this guide. A statement on the consensus approach then follows this review of the methods. This consensus approach has been included in order to foster consistency among studies. It is anticipated that recommended methods and this guide will be updated routinely to reflect progress in our understanding of sediments and how to best study them. This version of the standard is based primarily on a document developed by USEPA (2001 (1))2 and by Environment Canada (1994 (2)) as well as an earlier version of this standard.1.2 Protecting sediment quality is an important part of restoring and maintaining the biological integrity of our natural resources as well as protecting aquatic life, wildlife, and human health. Sediment is an integral component of aquatic ecosystems, providing habitat, feeding, spawning, and rearing areas for many aquatic organisms (MacDonald and Ingersoll 2002 a, b (3)(4)). Sediment also serves as a reservoir for contaminants in sediment and therefore a potential source of contaminants to the water column, organisms, and ultimately human consumers of those organisms. These contaminants can arise from a number of sources, including municipal and industrial discharges, urban and agricultural runoff, atmospheric deposition, and port operations.1.3 Contaminated sediment can cause lethal and sublethal effects in benthic (sediment-dwelling) and other sediment-associated organisms. In addition, natural and human disturbances can release contaminants to the overlying water, where pelagic (water column) organisms can be exposed. Sediment-associated contaminants can reduce or eliminate species of recreational, commercial, or ecological importance, either through direct effects or by affecting the food supply that sustainable populations require. Furthermore, some contaminants in sediment can bioaccumulate through the food chain and pose health risks to wildlife and human consumers even when sediment-dwelling organisms are not themselves impacted (Test Method E1706).1.4 There are several regulatory guidance documents concerned with sediment collection and characterization procedures that might be important for individuals performing federal or state agency-related work. Discussion of some of the principles and current thoughts on these approaches can be found in Dickson, et al. Ingersoll et al. (1997 (5)), and Wenning and Ingersoll (2002 (6)).1.5 This guide is arranged as follows:  Section  1Referenced Documents  2Terminology  3Summary of Guide  4  5Interferences  6Apparatus  7Safety Hazards  8Sediment Monitoring and Assessment Plans  9Collection of Whole Sediment Samples 10Field Sample Processing, Transport, and Storage of Sediments 11Sample Manipulations 12Collection of Interstitial Water 13Physico-chemical Characterization of Sediment Samples 14Quality Assurance 15Report 16Keywords 17Description of Samplers Used to Collect Sediment or Benthic Invertebrates Annex A11.6 Field-collected sediments might contain potentially toxic materials and should thus be treated with caution to minimize occupational exposure to workers. Worker safety must also be considered when working with spiked sediments containing various organic, inorganic, or radiolabeled contaminants, or some combination thereof. Careful consideration should be given to those chemicals that might biodegrade, volatilize, oxidize, or photolyze during the exposure.1.7 The values stated in either SI or inch-pound units are to be regarded as the standard. The values given in parentheses are for information only.1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.Specific hazards statements are given in Section 8.1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 This test method is meant to allow for a rapid (24 h) index of a geomedia's sorption affinity for given solutes in environmental waters or leachates. A large number of samples may be run in parallel using this test method to determine a comparative ranking of those samples, based upon the amount of solute sorbed by the geomedia, or by various geomedia or leachate constituents. The 24 h time is used to make the test convenient and also to minimize microbial, light, or hydrolytic degradation which may be a problem in longer timed procedures. While Kd values are directly applicable for screening and comparative ranking purposes, their use in predictive field applications generally requires the assumption that Kd be a fixed value.5.2 While this test method may be useful in determining 24 h Kd values for nonvolatile organic constituents, interlaboratory testing has been carried out only for the nonvolatile inorganic species arsenic and cadmium (see Section 12). However, the procedure has been tested for single-laboratory precision with polychlorinated biphenyls (PCBs) and is believed to be useful for all stable and nonvolatile inorganic and organic constituents. This test method is not considered appropriate for volatile constituents.5.3 The 24 h time limit may be sufficient to reach a steady-state Kd; however, the calculated Kd value should be considered a non-equilibrium measurement unless steady-state has been determined. To report this determination as a steady-state Kd, this test method should be conducted for intermediate times (for example, 12, 18, and 22 h) to ensure that the soluble concentrations in the solution have reached a steady state by 24 h. If a test duration of greater than 24 h is required, refer to Test Method D4319 for an alternate procedure of longer duration.1.1 This test method describes a procedure for determining the sorption affinity of waste solutes by unconsolidated geologic material in aqueous suspension. The waste solute may be derived from a variety of sources such as wells, underdrain systems, or laboratory solutions such as those produced by waste extraction tests like the Practice D3987 shake extraction method.1.2 This test method is applicable in screening and providing relative rankings of a large number of geomedia samples for their sorption affinity in aqueous leachate/geomedia suspensions. This test method may not simulate sorption characteristics that would occur in unperturbed geologic settings.1.3 While this procedure may be applicable to both organic and inorganic constituents, care must be taken with respect to the stability of the particular constituents and their possible losses from solution by such processes as degradation by microbes, light, hydrolysis, or sorption to material surfaces. This test method should not be used for volatile chemical constituents (see 6.1).1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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Sediment in insulating oil may deposit on transformer parts and interfere with heat transfer and may choke oil ducts; thus hindering oil circulation and heat dissipation. Inorganic sediment usually indicates contamination of some type and organic sediment indicates either deterioration of the oil or contamination.Soluble sludge indicates deterioration of the oil, presence of contaminants, or both. It serves as a warning that formation of sediment may be imminent.The determination of sediment and soluble sludge in a used insulating oil assists in deciding whether the oil may continue to be used in its existing condition or should be replaced, reclaimed, or reconditioned.1.1 This test method covers the determination of sediment and soluble sludge in service-aged insulating oils of petroleum origin. Also, provision is made for determining organic and inorganic content of the sediment. The method is intended primarily for oils of comparatively low viscosity; for example 5.7 to 13.0 cSt (mm2/s) at 40°C (104°F). Suitability for high viscosity oils have not been determined.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

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6.1 Contaminated sediments may affect natural populations of aquatic organisms adversely. Sediment-dwelling organisms may be exposed directly to contaminants by the ingestion of sediments and by the uptake of sediment-associated contaminants from interstitial and overlying water. Contaminated sediments may affect water column species directly by serving as a source of contaminants to overlying waters or a sink for contaminants from overlying waters. Organisms may also be affected when contaminated sediments are suspended in the water column by natural or human activities. Water column species and nonaquatic species may also be affected indirectly by contaminated sediments by the transfer of contaminants through ecosystems (7, 8).6.2 The procedures described in this guide may be used and adapted for incorporation in basic and applied research to determine the ecological effects of contaminated sediments. These same methods may also be used in the development and implementation of monitoring and regulatory programs designed to prevent and manage sediment contamination.6.3 Sediment tests with aquatic organisms can be used to quantify the acute and chronic toxicity and the bioavailability of new and presently used materials. Sediment toxicity may also result from environmental processes such as ammonia generation, pH shifts, or dissolved oxygen fluctuation. In many cases, consideration of the adverse effects of sediment-associated contaminants is only one part of a complete hazard assessment of manufactured compounds that are applied directly to the environment (for example, pesticides) and those released (for example, through wastewater effluents) as by-products from the manufacturing process or from municipalities (7).6.4 Sediment tests can be used to develop exposure-response relationships for individual toxicants by spiking clean sediments with varying concentrations of a test chemical and determining the concentration that elicits the target response in the test organism (Guide E1391). Sediment tests can also be designed to determine the effects that the physical and chemical properties of sediments have on the bioavailability and toxicity of compounds.6.5 Sediment tests can provide valuable information for making decisions regarding the management of contaminated sediments from hazardous waste sites and other contaminated areas. Biological tests with sediments can also be used to make defensible management decisions on the dredging and disposal of potentially contaminated sediments from rivers and harbors. ((7, 8), Test Method E1706.)1.1 As the contamination of freshwater and saltwater ecosystems continues to be reduced through the implementation of regulations governing both point and non-point source discharges, there is a growing emphasis and concern regarding historical inputs and their influence on water and sediment quality. Many locations in urban areas exhibit significant sediment contamination, which poses a continual and long-term threat to the functional condition of benthic communities and other species inhabiting these areas (1).2 Benthic communities are an important component of many ecosystems and alterations of these communities may affect water-column and nonaquatic species.1.2 Biological tests with sediments are an efficient means for evaluating sediment contamination because they provide information complementary to chemical characterizations and ecological surveys (2). Acute sediment toxicity tests can be used as screening tools in the early phase of an assessment hierarchy that ultimately could include chemical measurements or bioaccumulation and chronic toxicity tests. Sediment tests have been applied in both saltwater and freshwater environments (2-6). Sediment tests have been used for dredge material permitting, site ranking for remediation, recovery studies following management actions, and trend monitoring. A particularly important application is for establishing contaminant-specific effects and the processes controlling contaminant bioavailability(7).1.3 This guide is arranged as follows:  SectionReferenced Documents  2Terminology  3Application  4Summary of Guide  5  6Hazards  7Sediment Test Types  8Biological Responses  9Test Organisms 10Experimental Design Considerations 11Data Interpretation 12Keywords 131.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 7.1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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