ASTM D6010-96

Standard Practice for Closed Vessel Microwave Solvent Extraction of Organic Compounds from Solid Matrices

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 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. See Section 8 for specific hazard statements.

General Information

• Status: Historical
• Publication Date: 31-Dec-2000
• Technical Committee: D34 - Waste Management
• Drafting Committee: D34.01.06 - Analytical Methods

Relations

• Replaced By: ASTM D6010-96(2001) - Standard Practice for Closed Vessel Microwave Solvent Extraction of Organic Compounds from Solid Matrices
• Effective Date: 01-Jan-2001
• 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

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 6010 – 96
Standard Practice for
Closed Vessel Microwave Solvent Extraction of Organic
Compounds from Solid Matrices
This standard is issued under the fixed designation D 6010; 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 Title 21, Code of Federal Regulations (CFR), Part 1030, and
Title 47, Part 18
1.1 This practice describes the closed vessel microwave
extraction of soils, sediments, sludges, and wastes for subse-
3. Summary of Practice
quent determination of solvent extractable semivolatile and
3.1 This procedure ensures intimate contact of the sample
nonvolatile organic compounds by such techniques as gas
matrix with 115°C extraction solvent.
chromatography and gas chromatography-mass spectrometry.
3.2 A 1 to 5-g portion of a solid sample is extracted in a
1.1.1 Compounds listed in Tables 1–5 can be extracted from
sealed microwave transparent extraction vessel with 30 mL of
the preceding materials.
acetone-hexane (1 + 1).
1.2 This test method is applicable to samples that will pass
3.3 Up to 12 samples may be extracted simultaneously.
through a 10-mesh (approximately 2-mm opening) screen.
3.4 After extraction the vessels are cooled to room tempera-
1.3 The detection limit and linear concentration range for
ture, opened, and the solvent and sample are separated by
each compound is dependent on the gas chromatograph or gas
decanting, filtration, or centrifuging.
chromatograph-mass spectrometer technique employed and
3.5 This practice provides a sample suitable for analysis by
may be found in the manual accompanying the instrument
gas chromatography or gas chromatography-mass spectrom-
used.
etry.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Significance and Use
responsibility of the user of this standard to establish appro-
4.1 Extraction of organic pollutants from wastes can pro-
priate safety and health practices and determine the applica-
vide information on the susceptibility of compounds to leech-
bility of regulatory limitations prior to use. See Section 8 for
ing, water quality changes, or other site conditions.
specific hazard statements.
4.2 Rapid heating, in combination with temperatures in
2. Referenced Documents excess of the atmospheric boiling point of organic solvents,
reduces sample extraction times.
2.1 ASTM Standards:
4.3 Small amounts of solvents (30 mL) are used resulting in
D 1193 Specification for Reagent Water
reduced sample preparation cost and time.
D 3976 Practice for Preparation of Sediment Samples for
Chemical Analysis
5. Interferences
D 5368 Test Method for the Gravimetric Determination of
5.1 Method interferences may be caused by contaminants in
Total Solvent Extractable Content (TSEC) of Solid Waste
solvents, labware, and other hardware used in sample process-
Samples
ing that lead to discrete artifacts or elevated baselines in gas
2.2 Other Standards:
chromatograms. The analyst must demonstrate, through the
United States Environmental Protection Agency (USEPA),
analysis of reagent blanks, that the system and the materials are
Test Methods for Evaluating Solid Waste Volume 1A: L-
free from interferents.
aboratory Manual Physical/Chemical Methods
5.2 The use of high-purity solvents helps to minimize
interference problems.
This practice is under the jurisdiction of ASTM Committee D-34 on Waste
5.3 Matrix interferences are caused by contaminants that are
Management and is the direct responsibility of Subcommittee D34.02 on Physical
coextracted from the sample. The extent of matrix interfer-
and Chemical Characterization.
Current edition approved Oct. 10, 1996. Published December 1996. ences may vary considerably from sample to sample.
Annual Book of ASTM Standards, Vol 11.01.
5.4 After cleaning, vessel liners and covers should be stored
Annual Book of ASTM Standards, Vol 11.02.
in a clean environment to prevent accumulation of contami-
Annual Book of ASTM Standards, Vol 11.04.
nants.
Available from the Superintendent of Documents, U.S. Government Printing
Office, Washington, DC 20402.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 6010
TABLE 1 Semivolatile Analyte Recovery from Freshly Spiked
Topsoil
Spike Level, Average
Analyte RSD, %
A
mg/kg Recovery, %
Spike Level, Average
Analyte RSD, %
A
4-Nitrophenol 5.0 104 6.0
mg/kg Recovery, %
N-nitroso-di-n-butylamine 5.0 97.5 9.3
N-nitroso-di-n-propylamine 5.0 87.5 20
Acenaphthene 5.0 97.6 9.8
N-nitrosopiperidine 5.0 90.8 7.6
Acenaphthylene 5.0 100 10
Pentachlorobenzene 5.0 101 9.1
Acetophenone 5.0 92.2 12
Pentachloronitrobenzene 5.0 109 9.7
4-Aminobiphenyl 5.0 77.3 9.5
Pentachlorophenol 5.0 86.2 8.1
Aniline 5.0 68.1 7.5
Phenacetin 5.0 97.0 12
Anthracene 5.0 108 9.2
Phenanthrene 5.0 109 8.5
Benzidine 5.0 0
Phenol 5.0 97.3 9.2
Benzoic acid 5.0 42.3 13
2-Picoline 5.0 7.7 30
Benzo(a)anthracene 5.0 113 9.4
Pronamid 5.0 120 11
Benzo(b)fluoranthene 5.0
Pyrene 5.0 113 8.4
Benzo(k)fluoranthene 5.0 116 9.3
1,2,4,5-Tetrachlorobenzene 5.0 91.2 8.6
Benzo(g,h,i)perylene 5.0 111 4.7
2,3,4,6-Tetrachlorophenol 5.0 104 7.3
Benzo(a)pyrene 5.0 110 8.6
1,2,4-Trichlorobenzene 5.0 89.3 11
Benzyl alcohol 5.0 96.1 9.0
2,4,5-Trichlorophenol 5.0 95.1 12
Bis(2-chloroethoxy)methane 5.0 92.4 9.8
2,3,6-Trichlorophenol 5.0 96.4 6.7
Bis(2-chloroethyl)ether 5.0 96.0 11
2-Fluorobipenyl 2.5 92.9 8.0
Bis(2-chloroisopropyl)ether 5.0 95.2 12
2-Fluorophenol 5.0 95.4 7.7
Bis(2-ethylhexyl)phthalate 5.0 116 9.3
Nitrobenzene-d 2.5 92.2 9.8
4-Bromophenylphenyl ether 5.0 108 9.0
Phenol-d 5.0 98.9 9.7
Butyl benzyl phthalate 5.0 116 9.8 5
Terphenyl-d 2.5 112 10
4-Chloroaniline 5.0 97.0 9.2
2,4,6-Tribromophenol 5.0 92.3 7.7
1-Chloronaphthalene 5.0 104 12
2-Chloronaphthalene 5.0 91.8 7.3 A
The topsoil was dry when spiked. The number of determinations was three.
4-Chloro-3-methylphenol 5.0 107 12
Determinations were made by gas chromatography-mass spectrometry. All recov-
2-Chlorophenol 5.0 94.5 7.8
eries were corrected for analyte losses incurred during blowdown evaporation of
4-Chlorophenyl phenyl ether 5.0 106 9.7
solvent to determine, specifically, recoveries by microwave extraction.
Chrysene 5.0 111 8.8
B
Determined as azobenzene.
Dibenzo(a,j)acridine 5.0 10.6 34
Dibenzo(a,h)anthracene 5.0 110 5.9
6. Apparatus
Dibenzofuran 5.0 98.8 9.9
Di-n-butyl phthalate 5.0 113 9.4
6.1 Microwave Heating System—A laboratory microwave
1,2-Dichlorobenzene 5.0 89.9 12
heating system capable of delivering a minimum of 900 W of
1,3-Dichlorobenzene 5.0 87.6 13
1,4-Dichlorobenzene 5.0 87.3 13 microwave energy. The system should be capable of 1 %
3,3-Dichlorobenzidine 5.0 96.8 12
power adjustments and 1-s time adjustments. The microwave
2,4-Dichlorophenol 5.0 97.5 8.0
2,6-Dichlorophenol 5.0 93.1 12
Diethyl phthalate 5.0 111 8.0
TABLE 2 Semivolatile Analyte Recovery from ERA Soil
Dimethylaminoazobenzene 5.0 116 11
A
(Lot 324)
7,12-Dimethylbenz(a)anthracene 5.0 128 7.0
aa-Dimethylphenethylamine 5.0 7.0 4.1
Certified Average
2,4-Dimenthylphenol 5.0 107 9.4
Analyte Concentration Recovery, RSD, %
B C,D
Dimethyl phthalate 5.0 106 8.4
mg/kg %
4,6-Dinitro-2-methylphenol 5.0 57.6 9.3
Anthracene 1.01 68.6 4.7
2,4-Dinitrophenol 5.0 17.2 39
Benzo(a)anthracene 2.03 103 6.7
2,4-Dinitrotoluene 5.0 98.2 6.2
Bis(2-ethylhexyl)phthalate 7.12 150 11.2
2,6-Dinitrotoluene 5.0 98.5 9.9
B Butyl benzyl phthalate 10.6 128 10.8
1,2-Diphenylhydrazine 5.0 108 11
2-Chlorophenol 5.08 76.2 15.7
Di-n-octyl phthalate 5.0 117 12
Chrysene 2.35 114 8.5
Ethyl methanesulfonate 5.0 77.9 10
Dibenzofuran 6.79 88.8 1.9
Fluoranthene 5.0 110 8.7
2,4-Dinitrotoluene 5.0 83.0 4.2
Fluorene 5.0 101 10
Fluorene 6.06 72.1 1.0
Hexachlorobenzene 5.0 108 8.9
Naphthalene 1.64 64.3 15.7
Hexachlorobutadiene 5.0 89.5 11
Pentachlorophenol 12.2 85.0 6.8
Hexachlorocyclopentadiene 5.0 60.9 14
Phenanthrene 1.57 110 6.8
Hexachloroethane 5.0 83.7 13
Pyrene 8.03 110 12.8
Indeno(1,2,3-cd)pyrene 5.0 99.2 6.2
2,4,5-Trichlorophenol 7.99 96.9 1.3
Isophorone 5.0 88.7 8.5
2,4,6-Trichlorophenol 4.56 71.1 4.7
3-Methylcholanthrene 5.0 117 8.6
2-Fluorobiphenyl 6.0 102 8.8
Methyl methanesulfonate 5.0 48.5 28
2-Fluorophenol 20.0 99.5 14.1
2-Methylnaphthalene 5.0 104 9.3
Nitrobenzene-d 5.0 87.4 15.8
2-Methylphenol 5.0 95.1 8.5
Phenol-d 20.0 96.0 13.1
4-Methylphenol 5.0 92.4 11
Terphenyl-d 5.0 142 8.4
Naphthalene 5.0 95.0 12
2,4,6-Tribromophenol 20.0 94.8 3.9
1-Naphthylamine 5.0 57.8 8.7
A
2-Naphthylamine 5.0 73.5 9.0
This soil was obtained from Environmental Resources Associates (ERA) in
2-Nitroaniline 5.0 100 7.7
Arvada, CO, and has been certified for the compounds listed in this table.
B
3-Nitroaniline 5.0 96.8 8.5
Reported by ERA.
C
4-Nitroaniline 5.0 99.0 8.5
The number of determinations was four. The recoveries are based on the ERA
Nitrobenzene 5.0 88.4 19
certified values.
D
2-Nitrophenol 5.0 85.3 10
Recoveries corrected for analyte losses incurred during blowdown evapora-
tion of solvent to determine, specifically, recoveries by microwave extraction.
D 6010
TABLE 3 Chlorinated Pesticide Recovery from Freshly Spiked TABLE 4 Organophosphorus Pesticide and Industrial Chemical
A
Topsoil Compound Recovery from Freshly Spiked Topsoil
Spike Level, Average Spike Level Average Recovery,
Pesticide RSD, % Pesticide RSD, %
A A
μg/kg Recovery, % mg/kg %
Alachlor 200 87.6 2.3 Aspon 1.0 91.8 3.4
Aldrin 20 87.0 2.1 Azinphos-methyl 2.0 103 0.9
a-BHC 20 94.4 4.1 Azinphos-ethyl 1.0 122 1.4
b-BHC 20 90.4 3.6 Bolstar 1.0 103 1.8
g-BHC 20 89.6 1.3 Chlorofenvinphos 2.0 1.02 3.8
d-BHC 20 96.9 2.8 Chlorpyrifos 1.0 90.9 3.8
Captafol 200 122 4.7 Chlorpyrifos methyl 1.0 95.5 3.6
Captan 200 105 1.7 Coumaphos 2.0 100 0.7
Chlorobenzilate 100 82.6 5.6 Crotoxyphos 2.0 109 0.8
a-Chlordane 20 80.0 3.9 Demeton-O 1.0 98.7 7.1
g-Chlordane 20 86.2 2.9 Demeton-S 1.0 95.2 7.3
Chloroneb 100 69.6 2.4 Dichlorofenthion 1.0 73.5 9.6
Chloropropylate 100 86.0 5.6 Dichlorvos 1.0 63.4 14
Chlorothalonil 60 83.4 0.9 Dicrotophos 1.0 79.5 2.5
DBCP 100 55.1 19.8 Dimethoate 1.0 85.8 8.8
DCPA 60 93.3 1.5 Dioxathon 2.0 99.0 1.7
4,48-DDD 20 76.9 4.5 Disulfoton 1.0 97.5 3.5
4,48-DDE 20 84.7 3.1 EPN 1.0 102 1.3
4,48-DDT 20 116 5.6 Ethion 1.0 102 2.4
Diallate 200 98.6 4.1 Ethopro
...