1、Designation: D 6010 96 (Reapproved 2006)Standard Practice forClosed Vessel Microwave Solvent Extraction of OrganicCompounds from Solid Matrices1This standard is issued under the fixed designation D 6010; the number immediately following the designation indicates the year oforiginal adoption or, in t
2、he case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice describes the closed vessel microwaveextraction of soils, sediments, s
3、ludges, and wastes for subse-quent determination of solvent extractable semivolatile andnonvolatile organic compounds by such techniques as gaschromatography and gas chromatography-mass spectrometry.1.1.1 Compounds listed in Tables 15 can be extracted fromthe preceding materials.1.2 This test method
4、 is applicable to samples that will passthrough a 10-mesh (approximately 2-mm opening) screen.1.3 The detection limit and linear concentration range foreach compound is dependent on the gas chromatograph or gaschromatograph-mass spectrometer technique employed andmay be found in the manual accompany
5、ing the instrumentused.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior
6、 to use. See Section 8 forspecific hazard statements.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 3976 Practice for Preparation of Sediment Samples forChemical AnalysisD 5368 Test Methods for Gravimetric Determination ofTotal Solvent Extractable Content (TSEC) o
7、f Solid WasteSamples2.2 Other Standards:United States Environmental Protection Agency (USEPA),Test Methods for Evaluating Solid Waste Volume 1A: L-aboratory Manual Physical/Chemical Methods3Title 21, Code of Federal Regulations (CFR), Part 1030, andTitle 47, Part 1833. Summary of Practice3.1 This pr
8、ocedure ensures intimate contact of the samplematrix with 115C extraction solvent.3.2 A 1 to 5-g portion of a solid sample is extracted in asealed microwave transparent extraction vessel with 30 mL ofacetone-hexane (1 + 1).3.3 Up to 12 samples may be extracted simultaneously.3.4 After extraction the
9、 vessels are cooled to room tempera-ture, opened, and the solvent and sample are separated bydecanting, filtration, or centrifuging.3.5 This practice provides a sample suitable for analysis bygas chromatography or gas chromatography-mass spectrom-etry.4. Significance and Use4.1 Extraction of organic
10、 pollutants from wastes can pro-vide information on the susceptibility of compounds to leech-ing, water quality changes, or other site conditions.4.2 Rapid heating, in combination with temperatures inexcess of the atmospheric boiling point of organic solvents,reduces sample extraction times.4.3 Smal
11、l amounts of solvents (30 mL) are used resulting inreduced sample preparation cost and time.5. Interferences5.1 Method interferences may be caused by contaminants insolvents, labware, and other hardware used in sample process-ing that lead to discrete artifacts or elevated baselines in gaschromatogr
12、ams. The analyst must demonstrate, through theanalysis of reagent blanks, that the system and the materials arefree from interferents.5.2 The use of high-purity solvents helps to minimizeinterference problems.1This practice is under the jurisdiction of ASTM Committee D34 on WasteManagement and is th
13、e direct responsibility of Subcommittee D34.01.06 onAnalytical Methods.Current edition approved Feb. 1, 2006. Published March 2006. Originallyapproved in 1996. Last previous edition approved in 2001 as D 6010 - 96(2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact
14、ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from the Superintendent of Documents, U.S. Government PrintingOffice, Washington, DC 20402.1Copyright ASTM International, 100 Barr
15、 Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.3 Matrix interferences are caused by contaminants that arecoextracted from the sample. The extent of matrix interfer-ences may vary considerably from sample to sample.5.4 After cleaning, vessel liners and covers should be
16、storedin a clean environment to prevent accumulation of contami-nants.TABLE 1 Semivolatile Analyte Recovery from Freshly SpikedTopsoilAnalyteSpike Level,mg/kgAverageRecovery, %ARSD, %Acenaphthene 5.0 97.6 9.8Acenaphthylene 5.0 100 10Acetophenone 5.0 92.2 124-Aminobiphenyl 5.0 77.3 9.5Aniline 5.0 68.
17、1 7.5Anthracene 5.0 108 9.2Benzidine 5.0 0Benzoic acid 5.0 42.3 13Benzo(a)anthracene 5.0 113 9.4Benzo(b)fluoranthene 5.0Benzo(k)fluoranthene 5.0 116 9.3Benzo(g,h,i)perylene 5.0 111 4.7Benzo(a)pyrene 5.0 110 8.6Benzyl alcohol 5.0 96.1 9.0Bis(2-chloroethoxy)methane 5.0 92.4 9.8Bis(2-chloroethyl)ether
18、5.0 96.0 11Bis(2-chloroisopropyl)ether 5.0 95.2 12Bis(2-ethylhexyl)phthalate 5.0 116 9.34-Bromophenylphenyl ether 5.0 108 9.0Butyl benzyl phthalate 5.0 116 9.84-Chloroaniline 5.0 97.0 9.21-Chloronaphthalene 5.0 104 122-Chloronaphthalene 5.0 91.8 7.34-Chloro-3-methylphenol 5.0 107 122-Chlorophenol 5.
19、0 94.5 7.84-Chlorophenyl phenyl ether 5.0 106 9.7Chrysene 5.0 111 8.8Dibenzo(a,j)acridine 5.0 10.6 34Dibenzo(a,h)anthracene 5.0 110 5.9Dibenzofuran 5.0 98.8 9.9Di-n-butyl phthalate 5.0 113 9.41,2-Dichlorobenzene 5.0 89.9 121,3-Dichlorobenzene 5.0 87.6 131,4-Dichlorobenzene 5.0 87.3 133,3-Dichloroben
20、zidine 5.0 96.8 122,4-Dichlorophenol 5.0 97.5 8.02,6-Dichlorophenol 5.0 93.1 12Diethyl phthalate 5.0 111 8.0Dimethylaminoazobenzene 5.0 116 117,12-Dimethylbenz(a)anthracene 5.0 128 7.0aa-Dimethylphenethylamine 5.0 7.0 4.12,4-Dimenthylphenol 5.0 107 9.4Dimethyl phthalate 5.0 106 8.44,6-Dinitro-2-meth
21、ylphenol 5.0 57.6 9.32,4-Dinitrophenol 5.0 17.2 392,4-Dinitrotoluene 5.0 98.2 6.22,6-Dinitrotoluene 5.0 98.5 9.91,2-DiphenylhydrazineB5.0 108 11Di-n-octyl phthalate 5.0 117 12Ethyl methanesulfonate 5.0 77.9 10Fluoranthene 5.0 110 8.7Fluorene 5.0 101 10Hexachlorobenzene 5.0 108 8.9Hexachlorobutadiene
22、 5.0 89.5 11Hexachlorocyclopentadiene 5.0 60.9 14Hexachloroethane 5.0 83.7 13Indeno(1,2,3-cd)pyrene 5.0 99.2 6.2Isophorone 5.0 88.7 8.53-Methylcholanthrene 5.0 117 8.6Methyl methanesulfonate 5.0 48.5 282-Methylnaphthalene 5.0 104 9.32-Methylphenol 5.0 95.1 8.5AnalyteSpike Level,mg/kgAverageRecovery,
23、 %ARSD, %4-Methylphenol 5.0 92.4 11Naphthalene 5.0 95.0 121-Naphthylamine 5.0 57.8 8.72-Naphthylamine 5.0 73.5 9.02-Nitroaniline 5.0 100 7.73-Nitroaniline 5.0 96.8 8.54-Nitroaniline 5.0 99.0 8.5Nitrobenzene 5.0 88.4 192-Nitrophenol 5.0 85.3 104-Nitrophenol 5.0 104 6.0N-nitroso-di-n-butylamine 5.0 97
24、.5 9.3N-nitroso-di-n-propylamine 5.0 87.5 20N-nitrosopiperidine 5.0 90.8 7.6Pentachlorobenzene 5.0 101 9.1Pentachloronitrobenzene 5.0 109 9.7Pentachlorophenol 5.0 86.2 8.1Phenacetin 5.0 97.0 12Phenanthrene 5.0 109 8.5Phenol 5.0 97.3 9.22-Picoline 5.0 7.7 30Pronamid 5.0 120 11Pyrene 5.0 113 8.41,2,4,
25、5-Tetrachlorobenzene 5.0 91.2 8.62,3,4,6-Tetrachlorophenol 5.0 104 7.31,2,4-Trichlorobenzene 5.0 89.3 112,4,5-Trichlorophenol 5.0 95.1 122,3,6-Trichlorophenol 5.0 96.4 6.72-Fluorobipenyl 2.5 92.9 8.02-Fluorophenol 5.0 95.4 7.7Nitrobenzene-d52.5 92.2 9.8Phenol-d55.0 98.9 9.7Terphenyl-d142.5 112 102,4
26、,6-Tribromophenol 5.0 92.3 7.7AThe topsoil was dry when spiked. The number of determinations was three.Determinations were made by gas chromatography-mass spectrometry. All recov-eries were corrected for analyte losses incurred during blowdown evaporation ofsolvent to determine, specifically, recove
27、ries by microwave extraction.BDetermined as azobenzene.6. Apparatus6.1 Microwave Heating SystemA laboratory microwaveheating system capable of delivering a minimum of 900 W ofmicrowave energy. The system should be capable of 1 %power adjustments and 1-s time adjustments. The microwaveunit must be ca
28、pable of measuring and controlling solventtemperature within an extraction vessel. The microwave cavityshould be constructed so as to prevent any possible metal tometal arcing from occurring within the cavity. The oven cavityshould be equipped with an exhaust ventilation sufficient toprovide ten cha
29、mber exchanges/min. The ventilation exhaustshould contain an air flow sensor and a solvent sensor capableof detecting no air flow and solvent concentrations below theirlower explosive limits and shutting the microwave source off.The cavity shall have a 360 oscillating turntable to ensureeven sample
30、heating and be capable of removing containedvessel-vented solvents. Safety interlocks to shut off magnetronpower output shall be contained in the cavity door openingmechanism. The system shall comply with the Department ofHealth and Human Services Standards under the CFR, Part1030.10, Subpart (c)(1)
31、, (c)(2), and (c)(3), for microwaveleakage. The system should have Federal CommunicationCommission (FCC) type approval for operations under FCCRule Part 18. If the system is used outside of the United Statesit should comply with health and human service standards forthe country in which it is used.D
32、 6010 96 (2006)26.2 Extraction VesselsA closed lined extraction vessel ofapproximately 100-mL capacity. The vessel consists of afluoropolymer inner liner and cover to contain and isolate asolvent solution from a higher strength polymer outer pressurevessel body. The vessel assembly shall be transpar
33、ent tomicrowave energy and capable of withstanding an internalpressure of 200 psi (13.8 3 106dynes/cm2) and a temperatureof 200C. The vessel assembly shall contain a safety pressurerelief device that will prevent possible vessel rupture and beconnected to a sealed venting system capable of removingv
34、ented solvent vapors from the microwave cavity.6.3 Temperature-Pressure Control VesselA closed linedextraction vessel with temperature and pressure monitoringports capable of withstanding an internal pressure of 200 psi(13.8 3 106dynes/cm2) and a temperature of 200C. The vesselassembly shall contain
35、 a safety pressure relief device that willprevent possible vessel rupture and that is connected to a sealedventing system capable of removing vented solvent vaporsfrom the microwave cavity.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all extractions. Unless otherwise indi
36、cated, it isintended that all reagents shall conform to the specifications ofthe committee on Analytical Reagents of the American Chemi-cal Society, where such specifications are available.47.2 Acetone, pesticide quality or equivalent.7.3 Hexane, pesticide quality or equivalent.4Reagent Chemicals, A
37、merican Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formul
38、ary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 2 Semivolatile Analyte Recovery from ERA Soil(Lot 324)AAnalyteCertifiedConcentrationmg/kgBAverageRecovery,%C,DRSD, %Anthracene 1.01 68.6 4.7Benzo(a)anthracene 2.03 103 6.7Bis(2-ethylhexyl)phthalate 7.12 150 11.2Butyl benzyl phthalat
39、e 10.6 128 10.82-Chlorophenol 5.08 76.2 15.7Chrysene 2.35 114 8.5Dibenzofuran 6.79 88.8 1.92,4-Dinitrotoluene 5.0 83.0 4.2Fluorene 6.06 72.1 1.0Naphthalene 1.64 64.3 15.7Pentachlorophenol 12.2 85.0 6.8Phenanthrene 1.57 110 6.8Pyrene 8.03 110 12.82,4,5-Trichlorophenol 7.99 96.9 1.32,4,6-Trichlorophen
40、ol 4.56 71.1 4.72-Fluorobiphenyl 6.0 102 8.82-Fluorophenol 20.0 99.5 14.1Nitrobenzene-d55.0 87.4 15.8Phenol-d520.0 96.0 13.1Terphenyl-d145.0 142 8.42,4,6-Tribromophenol 20.0 94.8 3.9AThis soil was obtained from Environmental Resources Associates (ERA) inArvada, CO, and has been certified for the com
41、pounds listed in this table.BReported by ERA.CThe number of determinations was four. The recoveries are based on the ERAcertified values.DRecoveries corrected for analyte losses incurred during blowdown evapora-tion of solvent to determine, specifically, recoveries by microwave extraction.TABLE 3 Ch
42、lorinated Pesticide Recovery from Freshly SpikedTopsoilAPesticideSpike Level,g/kgAverageRecovery, %ARSD, %Alachlor 200 87.6 2.3Aldrin 20 87.0 2.1a-BHC 20 94.4 4.1b-BHC 20 90.4 3.6g-BHC 20 89.6 1.3d-BHC 20 96.9 2.8Captafol 200 122 4.7Captan 200 105 1.7Chlorobenzilate 100 82.6 5.6a-Chlordane 20 80.0 3
43、.9g-Chlordane 20 86.2 2.9Chloroneb 100 69.6 2.4Chloropropylate 100 86.0 5.6Chlorothalonil 60 83.4 0.9DBCP 100 55.1 19.8DCPA 60 93.3 1.54,48-DDD 20 76.9 4.54,48-DDE 20 84.7 3.14,48-DDT 20 116 5.6Diallate 200 98.6 4.1Dichlone 200 77.7 2.6Dichloran 60 110 9.3Dieldrin 20 85.9 3.8Endosulfan I 20 86.8 3.1
44、Endosulfan Ii 20 71.9 6.3Endosulfan sulfate 20 81.6 6.5Endrin 20 97.4 1.9Endrin aldehyde 20 78.3 3.5Endrin ketone 20 90.6 3.0Etridiazole 100 92.6 14Heptachlor 20 110 1.4Heptachlor epoxide 20 95.3 2.7Hexachlorobenzene 200 80.8 1.6Hexachlorocyclopentadiene 100 107 12Isodrin 20 103 1.3Methoxychlor 60 9
45、0.9 2.7Mirex 20 93.5 3.4Nitrofen 100 90.2 3.6PCNB 100 94.5 1.8Perthane 200 86.8 4.0Propachlor 100 91.5 8.4Trans-Nonachlor 20 81.7 5.4Cis-Permethrin 60 81.2 4.8Trans-Permethrin 60 103 32Trifluralin 40 101 2.4AThe number of determinations was three. The recoveries were corrected foranalyte losses incu
46、rred during blowdown evaporation of solvent to determine,specifically, recoveries by microwave extraction.D 6010 96 (2006)37.4 Purity of Water Unless otherwise indicated, refer-ences to water shall be understood to mean reagent waterconforming to Type III of Specification D 1193.8. Hazards8.1 The mi
47、crowave system shall be operated and maintainedin accordance with the manufacturers recommended safetyprecautions.8.2 The extraction vessels shall be used and maintained inaccordance with the manufacturers recommended safety pre-cautions.8.3 Use only microwave systems and vessels approved forsolvent
48、 use.9. Sampling9.1 Collect a soil, sediment, sludge, or waste sample usingan appropriate sampling technique.9.2 Prepare the soil, sediment, sludge, or waste sample inaccordance with Practice D 3976, Test Method D 5368, andEPA Test Methods for Evaluating Solid Waste, Vol 1A.9.3 Determination of Wate
49、r ContentIn certain cases,sample results are to be reported on a dry-weight basis. Whensuch data are desired, a sample portion for water contentdetermination should be weighed out at the same time as theportion used for organic analytical determination. Water con-tent then is determined on that portion of the sample inaccordance with Practice D 3976.10. Vessel Cleaning10.1 Follow the manufacturers recommended cleaning pro-cedure or clean the vessel liners and covers as follows:10.1.1 Clean each liner and cover as soon as possible afteruse by rinsing with acetone-hexane
