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.

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ASTM D5765-16 - 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)

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
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 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
3
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
4
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
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
1
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).
3
DOI: 10.1520/D5765-15. The last approved version of this historical standard is referenced on
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or www.astm.org.
4
contact ASTM Customer Service at service@astm.org. 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
1

---------------------- Page: 1 ----------------------
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,
5
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 Sulf
...

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
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
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
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
3
(Withdrawn 2014)
2.2 Federal Standard:
4
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.
1
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.
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 the ASTM website.
3
The last approved version of this historical standard is referenced on www.astm.org.
4
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
1

---------------------- Page: 1 ----------------------
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 so
...

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