1、Designation: D 5830 95 (Reapproved 2006)Standard Test Method forSolvents Analysis in Hazardous Waste Using GasChromatography1This standard is issued under the fixed designation D 5830; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision
2、, 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 test method is used to determine qualitatively andquantitatively the presence of the following com
3、pounds inwaste samples using gas chromatography. This test method isdesigned for use as a screening method with a typical reportinglevel of 0.1 %.Dichodifluoromethane TetrahydrofuranTrichlorofluoromethane Acetone1,1,2-Trichloro-1,2,2-trifluoroethaneMethyl Ethyl KetoneMIBKMethanol CyclohexanoneEthano
4、l Ethyl AcetateIsopropanol Propyl Acetaten-Propanol Butyl AcetateIsobutanol Benzenen-Butanol Toluenetert-Butanol EthylbenzeneMethylene Chloride XylenesChloroform StyreneCarbon Tetrachloride Chlorobenzene1,1-Dichloroethane Dichlorobenzenes1,2-Dichloroethane Nitrobenzene1,2-Dichloropropane Fluorobenze
5、ne1,1-Dichloroethylene n-Propyl Benzene1,2-Dichloroethene Isopropyl Benzene1,1,1-Trichloroethane Isobutyl BenzeneTetrachloroethylene n-Butyl BenzeneTrichloroethylene 2-EthoxyethanolTetrachloroethane 2-ButoxyethanolCyclopentane 2-Ethoxyethanol AcetatePentane 2-MethoxyethanolHexane BromoformHeptane Ca
6、rbitolCyclohexane Ethyl EtherIsooctane 1,4-DioxaneNitropropane Diacetone AlcoholEthanolamine AcetonitrileNitromethane PyridineEthylene Chloride ToluidineBenzyl Chloride Ethylene GlycolPropylene Glycol1.1.1 This compound list is a compilation of hazardoussolvents and other constituents that are routi
7、nely seen inhazardous waste samples.1.2 The scope of this test method may be expanded toinclude other volatile and semivolatile organic constituents.1.2.1 Hydrocarbon mixtures such as kerosene and mineralspirits.1.2.2 High-boiling organics, defined here as compoundswhich boil above n-Hexadecane.1.2.
8、3 Other organics that the analyst is able to identify,either through retention time data or gas chromatography/massspectrometric (GC/MS) analysis.1.3 Gas chromatographic methods are recommended for useonly by, or under close supervision of, an experienced analyst.1.4 This standard does not purport t
9、o 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 to use.2. Referenced Documents2.1 ASTM Standards:2D 1193 S
10、pecification for Reagent Water2.2 EPA Document:Gas Chromatography/Mass Spectrometry Method 8260,Test Methods for Evaluating Solid Waste Physical/Chemical Methods, SW-846, Third Edition, Final Update1, July 199233. Summary of Test Method3.1 Waste samples are analyzed by direct injection, or bycarbon
11、disulfide, M-Pyrol, or other suitable solvent extractionand injection of the extract into a gas chromatograph. Detec-tion is achieved using a detector which is specific for theneeded application, for example, flame ionization detector(FID), electron capture detector (ECD), thermal conductivity1This
12、test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.06 onAnalytical Methods.Current edition approved Feb. 1, 2006. Published March 2006. Originallyapproved in 1995. Last previous edition approved in 2001 as D 5830 95(
13、2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact 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. G
14、overnment PrintingOffice, Washington, DC 20402.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.detector (TCD), photoionization detector (PID), or mass selec-tive detector (MSD). This test method may be expanded toutilize other detect
15、or types not previously mentioned.4. Significance and Use4.1 This test method is useful in identifying the majorsolvent constituents in hazardous waste samples. This testmethod is designed to support field or site assessments,recycling operations, plant operations, or pollution controlprograms.5. In
16、terferences5.1 Interferences may be encountered from any number oforganic compounds that respond in the detector. Also, closelyeluting components may complicate identification based solelyon retention time. When these types of interferences areencountered, the analyst must rely on other sources of i
17、nfor-mation for positive identification, such as:5.1.1 Gas chromatography/mass spectrometric (GC/MS)confirmation, see EPA Method 8260, direct injection tech-nique;5.1.2 Use of confirmation column, or confirmatory detector;5.1.3 Use of varying temperature programs or standardcomparison, or both;5.1.4
18、 Sample history, for example, any information avail-able from the waste generator; and,5.1.5 Physical characteristics, for example, flammability,specific gravity, or miscibility with water.5.2 Interferences may also be encountered from syringecarryover. Immediately following each injection, the syri
19、ngeshould be thoroughly rinsed with carbon disulfide, or M-Pyrol.Other solvents such as methanol may be used as rinse solventsif sample types necessitate their use, but be aware thatcarryover and possible interferences may occur if the rinsesolvent is not completely cleaned from the syringe beforere
20、use. Before each injection the syringe must be thoroughlyrinsed with the sample to be injected, where the first twopumps are flushed into a separate waste receptacle.5.3 When carbon disulfide (CS2) is used to extract solids orsludges that contain significant amounts of water, low recoveryof the wate
21、r miscible solvents may result.FIG. 1 Daily QC Standard FID/DB-1701D 5830 95 (2006)25.4 Some grades of CS2may contain trace amounts ofbenzene.5.5 M-Pyrol seems to degrade slowly with time. The low-level degradation products interfere with some late elutingcompounds on some columns (approximately fiv
22、e smallpeaks).5.6 Interference from the CS2solvent peak may occur ifusing a TCD.5.7 When using a TCD, be aware that water, as well asoxygenated compounds, for example, MEK, MIBK, maysuppress detector response.5.8 If an electrolytic conductivity detector (ECD) must beused, be aware that CS2, M-Pyrol,
23、 and high concentrations ofhalogenated compounds may overload and possibly damagethe detector. It is recommended that the ECD be used onlywhen very low detection levels of halogenated compounds areexpected and direct injection of the sample is possible.6. Apparatus6.1 Gas Chromatograph SystemEquippe
24、d with capillaryor packed column injection ports, or both, detector, and datasystem.6.2 Recommended Chromatographic Columns:6.2.1 Capillary; Microbore or Megabore.6.2.1.1 DB-1701, 30M 3 0.25-mm inside diameter,0.25-m film thickness.6.2.1.2 DB-624, 30M 3 0.3-mm inside diameter, 1.8-mfilm thickness.6.
25、2.2 Packed: Stainless Steel or Glass.6.2.2.1 1 % SP-1000, 60/80 Carbopak B, 8-ft by18-in.inside diameter.6.2.2.2 10 % SP-2100, 100/120 Chromosorb WHP, 2M 3 2mm ID.NOTE 1These columns are recommended and have shown to givegood results. Operating conditions for each is listed in Section 10.Equivalent
26、or alternative columns, or both, may be used depending onapplication.6.3 Glass Screw-Cap Vials or EquivalentTo collectsamples and store standards. Polytetrafluoroethylene or otherinert material should be used for the cap liner.6.4 Microsyringes, 1.0, 10, and 100 L.6.5 Analytical Balance, accurate to
27、 0.0001 g.6.6 Pipettes, glass, disposable, or volumetric micropipettoror equivalent.6.7 Microdisk Filters, 0.45, 1.0, or 5.0 m, optional.6.8 Centrifuge, optional.6.9 Vortex-Type Mixer.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise i
28、ndicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.4Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit i
29、ts use without lessening the accuracy ofthe determination.7.2 Purity of Water Unless otherwise indicated, refer-ences to water shall be understood to mean reagent water asdefined by Type II of Specification D 1193.7.3 Nitrogen or Helium (High Purity)For carrier andmakeup gases. Air and hydrogen (hig
30、h purity) for fuel gases.Gases may be obtained from a gas generator if available,through purification of a lower grade, or from a high-puritytank supply.7.4 Carbon Disulfide, CS2Chromatography grade.7.5 M-Pyrol, CoHoNOAvailable through several chemi-cal suppliers and sources as 1-methyl-2-pyrrolidon
31、e.7.6 Individual Standards for Each Component of Interest99 % purity available from many vendors.8. Standard Preparation8.1 Stock Standard SolutionsStock standards are preparedfrom pure standard materials. It is recommended that thestandards be prepared so that each component is 5 to 10 % byweight.
32、The stock standards must be prepared by directlyweighing each component. For extremely volatile components,such as ether and freons, it is recommended that a new stockstandard be prepared daily or as needed. If a dilution solvent isneeded when preparing the stock standards, use the samesolvent used
33、for sample extraction or dilution in Section 7.NOTE 2Due to the incompatibility of some standard compounds, thatis, some compounds are not miscible with each other, and also because ofthe number of compounds typically looked for in a single chromato-graphic run, it is advisable to prepare 3 or 4 sta
34、ndard solutions eachcomposed of 10 to 15 compounds. A set of standard chromatograms anda retention timetable should be available for reference.8.2 Secondary Working StandardsThese are preparedfrom stock standard solutions using the appropriate solvent.Secondary standards should encompass the linear
35、range of theGC system.NOTE 3Linear response and range must be established with alldetectors and chromatography systems used for quantitation. All calibra-tion and sample analysis must be done within the established linear range.8.3 Calibration Check StandardA calibration check stan-dard should be pr
36、epared. The standard mixture should providea good overall check of the GC/detector system. The com-pounds should cover the major compound types, for example,alcohols, aromatics, aliphatics, ketones, and halogenates. Atypical calibration check standard flame ionization detector(FID) chromatogram is s
37、hown in Fig. 1.9. Sample Collection, Preservation, and Handling9.1 Sample collection should be in accordance with appro-priate sampling protocols.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlist
38、ed by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.D 5830 95 (2006)39.2 Samples should be collected in glass containers,
39、thathave tightly sealing caps. If very volatile organics are ofparticular interest, the headspace in the container should bekept to a minimum.9.3 Sample Transfer ImplementsImplements are requiredto transfer portions of waste samples from the sample contain-ers to the laboratory containers. Liquid sa
40、mples may betransferred using disposable pipets. Solids and semisolids maybe transferred using a conventional laboratory spatula.9.4 Samples shall be handled maintaining safe laboratorypractices. Any samples with special hazards must be appropri-ately labeled.9.5 Unused sample material, laboratory d
41、ilutions, and wastefrom the samples may be regulated. Consult your specialist orthe regulations, or both, for guidance in the proper handlingand disposal of laboratory wastes.10. Procedure10.1 Sample Preparation:10.1.1 Analyze liquid matrices with relatively low viscosityusing direct injection into
42、the GC, either as received or afterdilution with CS2, M-Pyrol, or other suitable solvent.10.1.2 Analyze solid or semisolid samples as follows:10.1.2.1 For carbon disulfide or M-Pyrol preparation, weigh3 g of the waste sample in a 15-mL glass vial. Add3gofcarbon disulfide or M-Pyrol to the vial and t
43、he mixture isvortexed vigorously. After allowing the solids to settle, injectthe CS2or M-Pyrol extract into the GC.10.1.2.2 Use alternate sample sizes and extraction solventweights if necessary. Actual sample size and solvent weightmust be recorded in the appropriate sample preparation logbook. It i
44、s essential for accurate waste sample analysis thatsample size be sufficient to ensure a representative sample. Ifalternate sample size or extraction solvent volumes, or both,are used, this must be reflected in the calculations under thedilution factor in Section 11.10.1.3 Multiple phases or layers
45、are typically present inhazardous waste samples. Depending on treatment or processrequirements, it may be necessary to analyze each phase orlayer individually.10.2 Recommended GC Operating Conditions:10.2.1 For Capillary DB-1701 with FIDColumn flow rate 11.5 mL/minMake-up gas flow rate 3060 mL/minSp
46、lit flow 60 cm3/minInjector temperature 250CDetector temperature 250CAirflow (FID) Approximately 300 mL/minHydrogen flow (FID) Approximately 30 mL/minInitial oven temperature 35CInitial time 6 minLevel 1 rate 6C/minLevel 1 final value 180CLevel 2 rate 10C/minLevel 2 final value 230CRun time 40 minTh
47、reshold 4 unitsPeak width 0.04 minNOTE 4Typical chromatograms are shown in Figs. 2-5.10.2.2 For Capillary DB-624 with FIDColumn flow rate 3.5 mL/minMake-up gas flow 29 mL/minAirflow (FID) Approximately 300 mL/minHydrogen flow (FID) Approximately 30 mL/minInjector temperature 275CDetector temperature
48、 275CInitial oven temperature 35CInitial time 5 minLevel 1 rate 5C/minLevel 1 final value 150CLevel 1 hold time 4 minLevel 2 rate 20C/minLevel 2 final value 225CRun time 45 min10.2.3 For Packed SP-1000 with FIDColumn flow rate 40 mL/minAir pressure (FID) 300 kPaHydrogen pressure (FID) 130 kPaInjecto
49、r temperature 250CDetector temperature 250CInitial oven temperature 90CInitial time 6 minLevel 1 rate 3C/minLevel 1 final value 120CLevel 2 rate 5C/minLevel 2 final value 180CLevel 3 rate 10C/minLevel 3 final value 230CRun time 46 min10.2.4 For packed SP-2100 with FIDCarrier gas flow 30 mL/minInjector temperatuare 250CDetector temperature 300CAirflow (FID) Approximately 300 mL/minHydrogen flow (FID) Approximately 30 mL/minInitial oven temperature 45CInitial hold time 3 minLevel 1 rate 15C/minLevel 1 final value 90CLevel 2 rate 10C
