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ASTM D5765-05

(Practice)

Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating

Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating

SIGNIFICANCE AND USE
Solvent extraction of soils and sediments can provide information on the availability of petroleum hydrocarbons to leaching, water quality changes, or other site conditions.
Rapid heating, in combination with temperatures in excess of the atmospheric boiling point of acetone/hexane, reduces sample preparation or extraction times.
Reduced amounts of solvents are required and solvent loss due to boiling and evaporation are eliminated by use of closed extraction vessels.
SCOPE
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 pounds per square inch (psi) are to be regarded as the standard. The SI units given in parentheses are for information only.  
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 8.

General Information

Status
Historical
Publication Date
14-Aug-2005
ICS
13.080.10 - Chemical characteristics of soils
Technical Committee
D19 - Water
Drafting Committee
D19.07 - Sediments, Geomorphology, and Open-Channel Flow
Current Stage
Ref Project

Relations

Replaces
ASTM D5765-95(2001) - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
Effective Date
15-Aug-2005
Replaced By
ASTM D5765-05(2010) - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
Effective Date
15-Jun-2010
Referred By
ASTM D7876-13(2018) - Standard Practice for Practice for Sample Decomposition Using Microwave Heating (With or Without Prior Ashing) for Atomic Spectroscopic Elemental Determination in Petroleum Products and Lubricants
Effective Date
15-Aug-2005

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ASTM D5765-05 - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave HeatingASTM D5765-05 - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
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ASTM D5765-05 - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D5765–05
Standard Practice for
Solvent Extraction of Total Petroleum Hydrocarbons from
Soils and Sediments Using Closed Vessel Microwave
1
Heating
This standard is issued under the fixed designation D5765; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D3694 Practices for Preparation of Sample Containers and
for Preservation of Organic Constituents
1.1 This practice covers the solvent extraction of total
D3856 Guide for Good Laboratory Practices in Laborato-
petroleum hydrocarbon (TPH) from soils and sediments, using
ries Engaged in Sampling and Analysis of Water
closedvesselmicrowaveheating,forsubsequentdetermination
D3974 Practices for Extraction of Trace Elements from
by gravimetric or gas chromatographic techniques.
Sediments
1.2 This practice is recommended only for solid samples
D3976 Practice for Preparation of Sediment Samples for
that can pass through a ten mesh screen (approximately 2-mm
Chemical Analysis
openings).
D5368 Test Methods for Gravimetric Determination of
1.3 The solvent extract obtained by this practice may be
Total Solvent Extractable Content (TSEC) of Solid Waste
analyzed for total or specific nonvolatile and semivolatile
Samples
petroleum hydrocarbons but may require sample clean-up
2.2 Federal Standard:
procedures prior to specific compound analysis.
Code of Federal Regulations, Title 21, Part 1030, and Title
1.4 This practice is limited to solvents that are recom-
3
47, Part 18
mended for use in microwave solvent extraction systems.
1.5 The values stated in pounds per square inch (psi) are to
3. Summary of Practice
be regarded as the standard. The SI units given in parentheses
3.1 The chemical portion of this practice involves solvent
are for information only.
extraction to dissociate petroleum hydrocarbons from the
1.6 This standard does not purport to address all of the
matrix.
safety concerns, if any, associated with its use. It is the
3.2 The sample is extracted with acetone/hexane in a sealed
responsibility of the user of this standard to establish appro-
microwave transparent vessel using microwave heating to an
priate safety and health practices and determine the applica-
internal temperature of 150°C.
bility of regulatory limitations prior to use. Specific hazard
3.3 This practice provides a sample suitable for analysis by
statements are given in Section 8.
gas chromatography or gravimetric measurements.
2. Referenced Documents
4. Significance and Use
2
2.1 ASTM Standards:
4.1 Solvent extraction of soils and sediments can provide
information on the availability of petroleum hydrocarbons to
1
This practice is under the jurisdiction of ASTM Committee D19 on Water and
leaching, water quality changes, or other site conditions.
is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology,
4.2 Rapid heating, in combination with temperatures in
and Open-Channel Flow.
excess of the atmospheric boiling point of acetone/hexane,
Current edition approved Aug. 15, 2005. Published August 2005. Originally
approved in 1995. Last previous edition approved in 2001 as D5765 – 95 (2001).
reduces sample preparation or extraction times.
DOI: 10.1520/D5765-05.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
3
the ASTM website. Available from the U.S. Government Printing Office, Washington, DC.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D5765–05
TABLE 1 Extraction Heating Parameters
4.3 Reduced amounts of solvents are required and solvent
loss due to boiling and evaporation are eliminated by use of Microwave power 100 %
Vessels pressure 200 psi
closed extraction vessels.
Vessels temperature 150°C
Heating time at 150°C 15 min
5. Interferences
5.1 No interferences to the extraction of soils and sediments
tee onAnalytical Reagents of theAmerican Chemical Society,
using microwave heating have been observed.
4
where such specifications are available.
5.2 Precautions should be exercised to avoid those interfer-
7.2 Acetone, HPLC grade.
ences normally associated with the final determination of total
7.3 Hexane, HPLC grade.
petroleum hydrocarbons using gas chromatography or gravi-
7.4 Sodium Sulfate—Reagent grade, granular, anhydrous,
metric techniques.
prepared by heating at 400°C for a minimum of 4 h.
7.5 Ashless Filter Paper.
6. Apparatus
8. Hazards
...

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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.  
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ASTM D7363-13A(2021)e1(Test Method)
Standard Test Method for Determination of Parent and Alkyl Polycyclic Aromatics in Sediment Pore Water Using Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry in Selected Ion Monitoring Mode

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5.1 This method directly determines the concentrations of dissolved PAH concentrations in environmental sediment pore water samples. The method is important from an environmental regulatory perspective because it can achieve the analytical sensitivities to meet the goals of the USEPA narcosis model for protecting benthic organisms in PAH contaminated sediments. Regulatory methods using solvent extraction have not achieved the wide calibration ranges from nanograms to milligrams per litre and the required levels of detection in the nanogram-per-litre range. In addition, conventional solvent extraction methods require large aliquot volumes (litre or larger), use of large volumes of organic solvents, and filtration to generate the pore water. This approach entails the storage and processing of large volumes of sediment samples and loss of low molecular weight PAHs in the filtration and solvent evaporation steps.  
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1.1 The U.S. Environmental Protection Agency (USEPA) narcosis model for benthic organisms in sediments contaminated with polycyclic aromatic hydrocarbons (PAHs) is based on the concentrations of dissolved PAHs in the interstitial water or “pore water” in sediment. This test method covers the separation of pore water from PAH-impacted sediment samples, the removal of colloids, and the subsequent measurement of dissolved concentrations of the required 10 parent PAHs and 14 groups of alkylated daughter PAHs in the pore water samples. The “24 PAHs” are determined using solid-phase microextraction (SPME) followed by Gas Chromatography/Mass Spectrometry (GC/MS) analysis in selected ion monitoring (SIM) mode. Isotopically labeled analogs of the target compounds are introduced prior to the extraction, and are used as quantification references.  
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SIGNIFICANCE AND USE
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.  
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5.2 PFAS are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFAS have been reported to exhibit developmental toxicity, hepatotoxicity, immunotoxicity, and hormone disturbance. A draft Toxicological Profile for Perfluoroalkyls from the U.S. Department of Health and Human Services is available.7 PFAS have been detected in soils, sludges, and surface and drinking waters. Hence, there is a need for a quick, easy, and robust method to determine these compounds at trace levels in various soil matrices for understanding of the sources and pathways of exposure.  
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5.1 This practice is a screening procedure for determining the presence of fuels containing aromatic compounds in soils. If a sample of the contaminant fuel is available for use in calibration, the approximate concentration of the fuel in the soil can be calculated. If the fuel type is known but a sample of the contaminant fuel is not available for calibration, an estimate of the contaminant fuel concentration can be calculated using average response factors based on composition of the fuel in the soil. If the composition of the contaminant fuel is unknown, a contaminant concentration cannot be calculated, and this practice can only be used only to indicate the presence or absence of fuel contamination.  
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SCOPE
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1.1 This test method covers a procedure for determining the pH of a soil in corrosion evaluations. The principle use of the test is to supplement soil resistivity measurements and thereby identify conditions under which the corrosion of metals in soil may be accentuated (see G57 – 78 (2012)).  
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5.1 Where sulfates are suspected, subgrade soils should be tested as an integral part of a geotechnical evaluation because the possibility that sulfate induced heave may occur if calcium containing stabilizers are used to improve the soils and sulfate reactions may also cause deterioration in concrete structures. When planning to treat a soil used in construction with lime, testing the soil for water soluble sulfates prior to treatment becomes very important (Note 2).  
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SCOPE
1.1 These methods determine the water soluble sulfate content of cohesive soils used in construction by using the colorimetric technique. Two methods are presented in this standard. Method A is for use in the field and Method B is for use in the laboratory. The colorimetric technique involves measuring the scattering of a light beam through a solution that contains suspended particulate matter. Measurements of sulfate concentrations in construction soils can be used to guide professionals in the selection of appropriate stabilization methods and to assist in assessment of potential deterioration in concrete structures.
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1.3 Ion chromatography is also an acceptable alternative method that can be used to evaluate results, however, it is outside the scope of this standard.  
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 All observed and calculated values shall conform to the guidelines for significant digits and rounding established in Practice D6026, unless superseded by this test method.  
1.5.1 The procedures used to specify how data are collected/recorded and calculated in the standard are regarded as the industry standard. In addition, they are representative of the significant digits that generally should be retained. The procedures used do not consider material variation, purpose for obtaining the data, special purpose studies, or any considerations for the user’s objectives; and it is common practice to increase or reduce significant digits of reported data to be commensurate with these considerations. It is beyond the scope of these test methods to consider significant digits used in analysis methods for engineering data.  
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Standard Test Method for Specific Gravity of Soil Solids by Gas Pycnometer

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SCOPE
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1.3 All observed and calculated values shall conform to the guidelines for significant digits and rounding established in Practice D6026.  
1.3.1 For purposes of comparing a measured or calculated value(s) with specified limits, the measured or calculated value(s) shall be rounded to the nearest decimal or significant digits in the specified limits.  
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1.4 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses are provided for information only and are not considered standard.  
1.4.1 The gravitational system of inch-pound units is used when dealing with inch-pound units. In this system, the pound (lbf) represents a unit of force (weight), while the unit for mass is slugs. The converted slug unit is not given, un...

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SCOPE
1.1 This guide is intended to serve as a reference for laboratories wishing to perform 99Tc analyses in soil. Several options are given for selection of a tracer and for the method of extracting the Tc from the soil matrix. Separation of Tc from the sample matrix is performed using an extraction chromatography resin. Options are then given for the determination of the 99Tc activity in the original sample. It is up to the user to determine which options are appropriate for use, and to generate acceptance data to support the chosen procedure.  
1.2 Due to the various extraction methods available, various tracers used, variable detection methods used, and lack of certified reference materials for 99Tc in soil, there is insufficient data to support a single method written as a standard method.  
1.3 The values stated in SI units are to be regarded as standard, except where the non-SI unit of molar, M, is used for the concentration of chemicals and reagents. The values given in parentheses after SI units are provided for information only and are not considered standard.  
1.4 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.  
1.5 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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ASTM
ASTM D4542-22(Test Method)
Standard Test Methods for Pore Water Extraction and Determination of the Soluble Salt Content of Soils by Refractometer

SIGNIFICANCE AND USE
4.1 The soluble salt content may be used to correct the index properties of soils such as water content, void ratio, specific gravity, degree of saturation, and dry density.
Note 1: The quality of the result produced by this standard is dependent on the competence of the personnel performing it, and the suitability of the equipment and facilities used. Agencies that meet the criteria of Practice D3740 are generally considered capable of competent and objective testing/sampling/inspection/etc. Users of this standard are cautioned that compliance with Practice D3740 does not in itself assure reliable results. Reliable results depend on many factors; Practice D3740 provides a means of evaluating some of those factors.
SCOPE
1.1 These test methods cover a rapid procedure for squeezing pore water from fine-grained soils for the purpose of determining the amount of soluble salts present in the extracted pore water.  
1.2 These test methods were developed for soils having a water content equal to or greater than approximately 14 %, for example, marine soils. An extensive summary of procedures for extracting pore water from soils has been presented by Kriukov and Manheim (1).2  
1.3 These test methods are not generally applicable for determining the soluble salt content of the pore water extracted from coarse-grained soils, such as clean sands and gravels.  
1.4 Test Method A provides a procedure using a refractometer with a refraction index scale; Test Method B provides a procedure using a refractometer with a parts per thousand (ppt) scale.  
1.5 Units—The values stated in SI units are to be regarded as the standard.  
1.6 All observed and calculated values shall conform to the guidelines for significant digits and rounding established in Practice D6026 unless superseded by these test methods.  
1.6.1 The procedures used to specify how data are collected/recorded and calculated in the standard are regarded as the industry standard. In addition, they are representative of the significant digits that generally should be retained. The procedures used do not consider material variation, purpose for obtaining the data, special purpose studies, or any considerations for the user’s objectives; and it is common practice to increase or reduce significant digits of reported data to be commensurate with these considerations. It is beyond the scope of these test methods to consider significant digits used in analysis methods for engineering data.  
1.7 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.  
1.8 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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  • Standard
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