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ASTM D5765-95(2001)

(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

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
31-Dec-2000
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 - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
Effective Date
01-Jan-2001
Replaced By
ASTM D5765-05 - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
Effective Date
15-Aug-2005
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
01-Jan-2001

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ASTM D5765-95(2001) - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave HeatingASTM D5765-95(2001) - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
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ASTM D5765-95(2001) - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
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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
An American National Standard
Designation:D 5765–95 (Reapproved 2001)
Standard Practice for
Solvent Extraction of Total Petroleum Hydrocarbons from
Soils and Sediments Using Closed Vessel Microwave
Heating
This standard is issued under the fixed designation D 5765; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope Total Solvent Extractable Content (TSEC) of Solid Waste
Samples
1.1 This practice covers the solvent extraction of total
2.2 Federal Standard:
petroleum hydrocarbon (TPH) from soils and sediments, using
Code of Federal Regulations, Title 21, Part 1030, and Title
closedvesselmicrowaveheating,forsubsequentdetermination
47, Part 18
by gravimetric or gas chromatographic techniques.
1.2 This practice is recommended only for solid samples
3. Summary of Practice
that can pass through a ten mesh screen (approximately 2-mm
3.1 The chemical portion of this practice involves solvent
openings).
extraction to dissociate petroleum hydrocarbons from the
1.3 The solvent extract obtained by this practice may be
matrix.
analyzed for total or specific nonvolatile and semivolatile
3.2 The sample is extracted with acetone/hexane in a sealed
petroleum hydrocarbons but may require sample clean-up
microwave transparent vessel using microwave heating to an
procedures prior to specific compound analysis.
internal temperature of 150°C.
1.4 This practice is limited to solvents that are recom-
3.3 This practice provides a sample suitable for analysis by
mended for use in microwave solvent extraction systems.
gas chromatography or gravimetric measurements.
1.5 The values stated in pounds per square inch (psi) are to
be regarded as the standard. The SI units given in parentheses
4. Significance and Use
are for information only.
4.1 Solvent extraction of soils and sediments can provide
1.6 This standard does not purport to address all of the
information on the availability of petroleum hydrocarbons to
safety concerns, if any, associated with its use. It is the
leaching, water quality changes, or other site conditions.
responsibility of the user of this standard to establish appro-
4.2 Rapid heating, in combination with temperatures in
priate safety and health practices and determine the applica-
excess of the atmospheric boiling point of acetone/hexane,
bility of regulatory limitations prior to use. Specific hazard
reduces sample preparation or extraction times.
statements are given in Section 8.
4.3 Reduced amounts of solvents are required and solvent
loss due to boiling and evaporation are eliminated by use of
2. Referenced Documents
closed extraction vessels.
2.1 ASTM Standards:
D 3694 Practices for Preparation of Sample Containers and
5. Interferences
for Preservation of Organic Constituents
5.1 No interferences to the extraction of soils and sediments
D 3856 Guide for Good Laboratory Practices in Laborato-
using microwave heating have been observed.
ries Engaged in Sampling and Analysis of Water
5.2 Precautions should be exercised to avoid those interfer-
D 3974 Practice for Extraction of Trace Elements from
2 ences normally associated with the final determination of total
Sediments
petroleum hydrocarbons using gas chromatography or gravi-
D 3976 Practice for Preparation of Sediment Samples for
2 metric techniques.
Chemical Analysis
D 5368 Test Method for the Gravimetric Determination of
6. Apparatus
6.1 Microwave Heating System—A laboratory microwave
heating system capable of delivering a minimum of 900 W of
This practice is under the jurisdiction ofASTM Committee D-19 on Water and
microwave energy. The system should be capable of 1 %
is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology,
and Open-Channel Flow.
Current edition approved Aug. 15, 1995. Published October 1995.
2 4
Annual Book of ASTM Standards, Vol 11.02. Annual Book of ASTM Standards, Vol 11.04.
3 5
Annual Book of ASTM Standards, Vol 11.01. 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.
D 5765–95 (2001)
power adjustments and 1-s time adjustment. The microwave 8. Hazards
cavity should be constructed so as to prevent any possible
8.1 Themicrowavesystemshallbeoperatedandmaintained
metal to metal arcing from occurring within the cavity. The
in accordance with the manufacturer’s recommended safety
oven cavity should be equipped with an exhaust ventilation
precautions.
sufficient to provide ten chamber exchanges per minute. The
8.2 The extraction vessels shall be used and maintained in
ventilation exhaust should contain a solvent sensor capable of
accordance with the manufacturer’s recommended safety pre-
detecting solvent concentrations below their lower explosive
cautions.
limits and shutting the microwave source off. The cavity shall
8.3 Use only microwave systems and vessels approved for
have a 360° oscillating turntable to ensure even sample
solvent use.
heating, and be capable of removing contained vessel vented
solvents. Safety interlocks, to shut off magnetron power output
9. Sampling
shall be contained in the cavity door opening mechanism. The
9.1 Collect a soil or sediment sample using an appropriate
system shall comply with Department of Health and Human
sampling technique.
ServicesStandardsundertheCodeofFederalRegulations,Part
9.2 Prepare the soil or sediment sample in accordance with
1030.10, Subparts (c) (1), (c) (2), and (c)
...

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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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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.  
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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.  
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5.1 This practice provides procedures to generate and document QC data for ensuring that an XRF is operating within acceptable tolerances throughout the testing period when being used to collect lead results during a lead-based paint (LBP) inspection for the purposes of generating lead classification results.  
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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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1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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5.2 Fuels containing aromatic compounds, such as diesel fuel and gasoline, as well as other aromatic-containing hydrocarbon materials, such as crude oil, coal oil, and motor oil, can be determined by this practice. The quantitation limit for diesel fuel is about 75 mg/kg. Approximate quantitation limits for other aromatic-containing hydrocarbon materials that can be determined by this screening practice are given in Table 1. Quantitation limits for highly aliphatic materials, such as aviation gasoline and synthetic motor oil, are much higher than those for more aromatic materials, such as coal oil and diesel fuel.  
Note 1: The quantitation limits listed in Table 1 are estimated values because in this practice, the quantitation limit can be influenced by the particular fuel type and soil background. For information on how the values given in Table 1 were determined, see Appendix X1. Data generated during the development of this screening practice and other information pertaining to this practice can be found in the referenced research reports (1, 2).3  
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SCOPE
1.1 This practice is a screening procedure for assessing the presence of fuels containing aromatic compounds in soils. If a sample of the contaminant fuel is available, the concentration of the fuel in the soil can be determined. If the contaminant fuel type is known but a sample of the contaminant fuel is not available, an estimate of the concentration of the fuel in the soil can be made using average response factors based on composition of the fuel in the soil. If the kind of contaminant fuel is unknown, this screening method can be used to identify the presence of contamination.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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1.4 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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4.1 Information on pH of soil is used as an aid in evaluating the corrosivity of a soil environment. Some metals are more sensitive to the pH of their environment than others, and information on the stability of a metal as a function of pH and potential is available in the literature.3
SCOPE
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)).  
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 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.  
1.4 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 D8459-23(Test Method)
Standard Test Methods for Detecting Water Soluble Sulfates in Construction Soils

SIGNIFICANCE AND USE
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).  
5.2 When sulfate containing cohesive soils are treated with calcium-based stabilizers for foundation improvements, sulfates and free alumina in natural soils react with calcium and free hydroxide to form crystalline minerals, such as ettringite and thaumasite.4 Thaumasite forms when ettringite undergoes changes in the presence of carbonates at low temperatures.5 The sulfate minerals expand considerably when they are hydrated.
Note 2: For more information on the effect of treating soils containing water soluble sulfates, refer to the following publication: Little, D.N., Stabilization of Pavement Subgrades and Base Course with Lime, Kendal/Hunt Publishing Co., Dubuque, IA, 1995.
Note 3: 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 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.
Note 1: These test methods are partially based on the research conducted by Texas A & M University.  
1.2 The field method, Method A, is used as a screening test for the presence of sulfates and their concentration. The laboratory method, Method B, provides better resolution than the field method.  
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.  
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 appropri...

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