ASTM D6010-12

Standard Practice for Closed Vessel Microwave Solvent Extraction of Organic Compounds from Solid Matrices (Withdrawn 2016)

SIGNIFICANCE AND USE
5.1 Extraction of organic pollutants from wastes can provide information on the susceptibility of compounds to leeching, water quality changes, or other site conditions.  
5.2 Rapid heating, in combination with temperatures in excess of the atmospheric boiling point of organic solvents, reduces sample extraction times.  
5.3 Small amounts of solvents (30 mL) are used resulting in reduced sample preparation cost and time.
SCOPE
1.1 This practice describes the closed vessel microwave extraction of soils, sediments, sludges, and wastes for subsequent determination of solvent extractable semivolatile and nonvolatile organic compounds by such techniques as gas chromatography and gas chromatography-mass spectrometry.  
1.1.1 Compounds listed in Tables 1–5 can be extracted from the preceding materials.  
1.2 This test method is applicable to samples that will pass through a 10-mesh (approximately 2-mm opening) screen.  
1.3 The detection limit and linear concentration range for each compound is dependent on the gas chromatograph or gas chromatograph-mass spectrometer technique employed and may be found in the manual accompanying the instrument used.  
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 and health practices and determine the applicability of regulatory limitations prior to use.
WITHDRAWN RATIONALE
This practice described the closed vessel microwave extraction of soils, sediments, sludges, and wastes for subsequent determination of solvent extractable semivolatile and nonvolatile organic compounds by such techniques as gas chromatography and gas chromatography-mass spectrometry.
Formerly under the jurisdiction of Committee D34 on Waste Management, this practice was withdrawn in November 2016. This standard is being withdrawn without replacement due to its limited use by industry.

General Information

• Status: Withdrawn
• Publication Date: 31-Oct-2012
• Withdrawal Date: 10-Nov-2016
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: D34 - Waste Management
• Drafting Committee: D34.01.06 - Analytical Methods

Relations

• 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-Nov-2012

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: D6010 − 12
StandardPractice for
Closed Vessel Microwave Solvent Extraction of Organic
1
Compounds from Solid Matrices
This standard is issued under the fixed designation D6010; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D5681Terminology for Waste and Waste Management
1.1 This practice describes the closed vessel microwave 2.2 Other Standards:
extraction of soils, sediments, sludges, and wastes for subse- United States Environmental Protection Agency (USEPA),
quent determination of solvent extractable semivolatile and
Test Methods for Evaluating Solid Waste Volume
3
nonvolatile organic compounds by such techniques as gas 1A:Laboratory Manual Physical/Chemical Methods
chromatography and gas chromatography-mass spectrometry. Title21,CodeofFederalRegulations(CFR),Part1030,and
3
1.1.1 CompoundslistedinTables1–5canbeextractedfrom Title 47, Part 18
the preceding materials.
3. Terminology
1.2 This test method is applicable to samples that will pass
through a 10-mesh (approximately 2-mm opening) screen.
3.1 Definitions—For definitions of terms used in this
practice, see Terminology D5681.
1.3 The detection limit and linear concentration range for
each compound is dependent on the gas chromatograph or gas
4. Summary of Practice
chromatograph-mass spectrometer technique employed and
may be found in the manual accompanying the instrument
4.1 This procedure ensures intimate contact of the sample
used.
matrix with 115°C extraction solvent.
1.4 The values stated in SI units are to be regarded as
4.2 A1 to 5-g portion of a solid sample is extracted in a
standard. No other units of measurement are included in this
sealed microwave transparent extraction vessel with 30 mL of
standard.
acetone-hexane (1+1).
1.5 This standard does not purport to address all of the
4.3 Up to 12 samples may be extracted simultaneously.
safety concerns, if any, associated with its use. It is the
4.4 After extraction the vessels are cooled to room
responsibility of the user of this standard to establish appro-
temperature, opened, and the solvent and sample are separated
priate safety and health practices and determine the applica-
by decanting, filtration, or centrifuging.
bility of regulatory limitations prior to use.
4.5 This practice provides a sample suitable for analysis by
2. Referenced Documents
gas chromatography or gas chromatography-mass spectrom-
2
2.1 ASTM Standards: etry.
D1193Specification for Reagent Water
D3976Practice for Preparation of Sediment Samples for 5. Significance and Use
Chemical Analysis
5.1 Extraction of organic pollutants from wastes can pro-
D5368TestMethodsforGravimetricDeterminationofTotal
vide information on the susceptibility of compounds to
Solvent Extractable Content (TSEC) of Solid Waste
leeching, water quality changes, or other site conditions.
Samples
5.2 Rapid heating, in combination with temperatures in
excess of the atmospheric boiling point of organic solvents,
1
This practice is under the jurisdiction of ASTM Committee D34 on Waste
reduces sample extraction times.
Management and is the direct responsibility of Subcommittee D34.01.06 on
Analytical Methods.
5.3 Smallamountsofsolvents(30mL)areusedresultingin
Current edition approved Nov. 1, 2012. Published December 2012. Originally
reduced sample preparation cost and time.
approved in 1996. Last previous edition approved in 2006 as D6010–96 (2006).
DOI: 10.1520/D6010-12.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Available from the Superintendent of Documents, U.S. Government Printing
the ASTM website. Office, Washington, DC 20402.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D6010 − 12
TABLE 1 Continued
6. Interferences
Spike Level, Average
Analyte RSD, %
A
6.1 Methodinterferencesmaybecausedbycontaminantsin
mg/kg Recovery, %
solvents, labware, and other hardware used in sample process-
Fluoranthene 5.0 110 8.7
ing that lead to discrete artifacts or elevated baselines in gas
Fluorene 5.0 101 10
chromatograms. The analyst must demonstrate, through the Hexachlorobenzene 5.0 108 8.9
Hexachlorobutadiene 5.0 89.5 11
analysisofreagentblanks,thatthesystemandthematerialsare
Hexachlorocyclopentadiene 5.0 60.9 14
free from interferents.
Hexachloroethane 5.0 83.7 13
Indeno(1,2,3-cd)pyrene 5.0 99.2 6.2
6.2 The use of high-purit
...