ASTM D5765-16

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

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.  
5.3 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 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.

General Information

• Status: Published
• Publication Date: 31-Dec-2015
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: D19 - Water
• Drafting Committee: D19.07 - Sediments, Geomorphology, and Open-Channel Flow

Relations

• Replaces: ASTM D5765-05(2010) - Standard Practice for Solvent Extraction of Total Petroleum Hydrocarbons from Soils and Sediments Using Closed Vessel Microwave Heating
• Effective Date: 01-Jan-2016
• Refers: ASTM D3694-96(2024) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
• Effective Date: 01-Apr-2024
• Refers: ASTM D3974-09(2023) - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 15-Dec-2023
• Refers: ASTM D1129-13(2020)e2 - Standard Terminology Relating to Water
• Effective Date: 01-May-2020
• Refers: ASTM D3974-09(2015) - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 01-Jan-2015
• Refers: ASTM D5368-13 - Standard Test Methods for Gravimetric Determination of Total Solvent Extractable Content (TSEC) of Solid Waste Samples (Withdrawn 2014)
• Effective Date: 01-Apr-2013
• Refers: ASTM D3856-11 - Standard Guide for Management Systems in Laboratories Engaged in Analysis of Water
• Effective Date: 15-Nov-2011
• Refers: ASTM D3694-96(2011) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
• Effective Date: 01-May-2011
• Refers: ASTM D3976-92(2010) - Standard Practice for Preparation of Sediment Samples for Chemical Analysis
• Effective Date: 15-Jun-2010
• Refers: ASTM D1129-10 - Standard Terminology Relating to Water
• Effective Date: 01-Mar-2010
• Refers: ASTM D3974-09 - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 01-May-2009
• Refers: ASTM D3974-81(2008) - Standard Practices for Extraction of Trace Elements from Sediments
• Effective Date: 01-Oct-2008
• Refers: ASTM D1129-06ae1 - Standard Terminology Relating to Water
• Effective Date: 01-Sep-2006
• Refers: ASTM D1129-06a - Standard Terminology Relating to Water
• Effective Date: 01-Sep-2006
• Refers: ASTM D3856-95(2006) - Standard Guide for Good Laboratory Practices in Laboratories Engaged in Sampling and Analysis of Water
• Effective Date: 15-Feb-2006

Overview

ASTM D5765-16 is a standard practice developed by ASTM International that details the solvent extraction of total petroleum hydrocarbons (TPH) from soils and sediments using closed vessel microwave heating. Designed for solid environmental samples that can pass through a 10-mesh screen, this practice supports the efficient extraction and subsequent analysis of petroleum hydrocarbons. The extracted samples can then be analyzed using gravimetric or gas chromatographic techniques. The use of closed vessel microwave systems offers significant operational advantages, such as reduced extraction time and lower solvent consumption, while improving laboratory safety and data reliability.

Key Topics

• Total Petroleum Hydrocarbons (TPH) Extraction: This practice allows for the extraction of both nonvolatile and semivolatile petroleum hydrocarbons from soil and sediment matrices.
• Closed Vessel Microwave Heating: The process utilizes sealed, microwave-transparent extraction vessels, which enable rapid and consistent heating beyond the atmospheric boiling point of common solvents like acetone/hexane.
• Reduced Solvent Usage: By operating in closed systems, the practice minimizes solvent losses due to evaporation or boiling, making it more cost-effective and environmentally friendly.
• Applicability and Limitations: The practice is specifically intended for solid samples that can pass a 2 mm screen and only uses solvents recommended for microwave extraction systems.
• Precautionary Measures: User safety is emphasized through adherence to equipment-specific safety guidelines and regulatory compliance. The practice also highlights the need for proper reagent purity and vessel cleanliness to ensure accurate results.

Applications

• Environmental Site Assessment: The method is widely used for evaluating contaminated sites by quantifying the presence and mobility of petroleum hydrocarbons in soils and sediments.
• Water Quality Analysis: Extracted hydrocarbons offer critical data for assessing potential risks to surrounding water resources due to leaching or site changes.
• Regulatory Compliance: Laboratories conducting tests to meet environmental regulations can utilize this standard to produce consistent, defensible data for total petroleum hydrocarbon content.
• Laboratory Efficiency: The rapid heating made possible by microwave extraction reduces sample turnaround times, reduces solvent use, and increases overall operational safety.
• Sample Preparation for Advanced Analysis: The solvent extract can be further cleaned and prepared for detailed gas chromatographic analysis of specific petroleum hydrocarbon fractions.

Related Standards

• ASTM D1129: Terminology relating to water, referenced for standardized definitions.
• ASTM D3694: Practices for preparation of sample containers and for preservation of organic constituents.
• ASTM D3856: Guide for management systems in laboratories engaged in water analysis.
• ASTM D3974: Practices for extraction of trace elements from sediments.
• ASTM D3976: Practice for the preparation of sediment samples for chemical analysis.
• ASTM D5368: Test methods for gravimetric determination of total solvent extractable content (TSEC) of solid waste samples.

By following ASTM D5765-16, laboratories and field professionals can ensure precise, efficient, and standardized extraction of petroleum hydrocarbons, supporting accurate environmental assessments, regulatory reporting, and improved sample throughput in environmental laboratories. This practice offers practical value to those involved in soil and sediment contamination investigations, site remediation, and compliance monitoring.

Standards Content (Sample)

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.
Designation: D5765 − 16
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 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 Management Systems in Laboratories
petroleum hydrocarbon (TPH) from soils and sediments, using
Engaged in 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 ofTotal
Solvent Extractable Content (TSEC) of Solid Waste
1.3 The solvent extract obtained by this practice may be
analyzed for total or specific nonvolatile and semivolatile Samples (Withdrawn 2014)
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
47, Part 18
1.4 This practice is limited to solvents that are recom-
mended for use in microwave solvent extraction systems.
3. Terminology
1.5 The values stated in SI units are to be regarded as
3.1 Definitions:
standard.
3.1.1 For definitions of terms used in this standard, refer to
1.5.1 Exception—The inch-pound values given for units of
Terminology D1129.
pressure are to be regarded as standard; SI unit conversions are
shown in parentheses.
4. Summary of Practice
1.6 This standard does not purport to address all of the
4.1 The chemical portion of this practice involves solvent
safety concerns, if any, associated with its use. It is the
extraction to dissociate petroleum hydrocarbons from the
responsibility of the user of this standard to establish appro-
matrix.
priate safety and health practices and determine the applica-
4.2 The sample is extracted with acetone/hexane in a sealed
bility of regulatory limitations prior to use. Specific hazard
statements are given in Section 9. microwave transparent vessel using microwave heating to an
internal temperature of 150°C.
2. Referenced Documents
4.3 This practice provides a sample suitable for analysis by
2.1 ASTM Standards: gas chromatography or gravimetric measurements.
D1129 Terminology Relating to Water
5. Significance and Use
5.1 Solvent extraction of soils and sediments can provide
This practice is under the jurisdiction of ASTM Committee D19 on Water and
information on the availability of petroleum hydrocarbons to
is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology,
leaching, water quality changes, or other site conditions.
and Open-Channel Flow.
Current edition approved Jan. 1, 2016. Published January 2016. Originally
approved in 1995. Last previous edition approved in 2010 as D5765 – 05 (2010).
DOI: 10.1520/D5765-15. The last approved version of this historical standard is referenced on
For referenced ASTM standards, visit the ASTM website, www.astm.org, or www.astm.org.
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
Standards volume information, refer to the standard’s Document Summary page on 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
the ASTM website. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5765 − 16
5.2 Rapid heating, in combination with temperatures in all reagents shall conform to the specifications of the commit-
excess of the atmospheric boiling point of acetone/hexane, tee onAnalytical Reagents of theAmerican Chemical Society,
reduces sample preparation or extraction times. where such specifications are available.
5.3 Reduced amounts of solvents are required and solvent 8.2 Acetone, HPLC grade.
loss due to boiling and evaporation are eliminated by use of
8.3 Hexane, HPLC grade.
closed extraction vessels.
8.4 Sodium Sulfate—Reagent grade, granular, anhydrous,
6. Interferences
prepared by heating at 400°C for a minimum of 4 h.
6.1 No interferences to the extraction of soils and sediments
8.5 Ashless Filter Paper.
using microwave heating have been observed.
9. Hazards
6.2 Precautions should be exercised to avoid those interfer-
ences normally associated with the final determination of total
9.1 Themicrowavesystemshallbeoperatedandmaintained
petroleum hydrocarbons using gas chromatography or gravi-
in accordance with the manufacturer’s recommended safety
metric techniques.
precautions.
7. Apparatus 9.2 The extraction vessels shall be used and maintained in
accordance with the manufacturer’s recommended safety pre-
7.1 Microwave Heating System—A laboratory microwave
cautions.
heating system capable of delivering a minimum of 900 W of
microwave energy. The system should be capable of 1 %
9.3 Use only microwave systems and vessels approved for
power adjustments and 1 s time adjustment. The microwave solvent use.
cavity should be constructed so as to prevent any possible
metal to metal arcing from occurring within the cavity. The 10. Sampling
oven cavity should be equipped with an exhaust ventilation
10.1 Collect a soil o
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5765 − 05 (Reapproved 2010) D5765 − 16
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 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
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) SI units are to be regarded as the standard. The SI units given in
parentheses are for information only.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 89.
2. Referenced Documents
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D3974 Practices for Extraction of Trace Elements from Sediments
D3976 Practice for Preparation of Sediment Samples for Chemical Analysis
D5368 Test Methods for Gravimetric Determination of Total Solvent Extractable Content (TSEC) of Solid Waste Samples
(Withdrawn 2014)
2.2 Federal Standard:
Code of Federal Regulations,Regulations Title 21, Part 1030,1030; and Title 47, Part 18
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
This practice is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.07 on Sediments, Geomorphology, and
Open-Channel Flow.
Current edition approved June 15, 2010Jan. 1, 2016. Published December 2010January 2016. Originally approved in 1995. Last previous edition approved in 20052010
as D5765 – 05.D5765 – 05 (2010). DOI: 10.1520/D5765-05R10.10.1520/D5765-15.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5765 − 16
4. Summary of Practice
4.1 The chemical portion of this practice involves solvent extraction to dissociate petroleum hydrocarbons from the matrix.
4.2 The sample is extracted with acetone/hexane in a sealed microwave transparent vessel using microwave heating to an
internal temperature of 150 °C.150°C.
4.3 This practice provides a sample suitable for analysis by gas chromatography or gravimetric measurements.
5. 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.
5.3 Reduced amounts of solvents are required and solvent loss due to boiling and evaporation are eliminated by use of closed
extraction vessels.
6. Interferences
6.1 No interferences to the extraction of soils and sediments using microwave heating have been observed.
6.2 Precautions should be exercised to avoid those interferences normally associated with the final determination of total
petroleum hydrocarbons using gas chromatography or gravimetric techniques.
7. Apparatus
7.1 Microwave Heating System—A laboratory microwave heating system capable of delivering a minimum of 900 W of
microwave energy. The system should be capable of 1 % power adjustments and 1 s time adjustment. The microwave cavity should
be constructed so as to prevent any possible metal to metal arcing from occurring within the cavity. The oven cavity should be
equipped with an exhaust ventilation sufficient to provide ten chamber exchanges per minute. The ventilation exhaust should
contain a solvent sensor capable of detecting solvent concentrations below their lower explosive limits and shutting the microwave
source off. The cavity shall have a 360° oscillating turntable to ensure even sample heating, and be capable of monitoring and
control of solvent temperature using either an in-situ control vessel or by external vessel monitoring. Safety interlocks, to shut off
magnetron power output shall be contained in the cavity door opening mechanism. The system shall comply with Department of
Health and Human Services Standards under the Code of Fed
...