1、Designation: D5830 95 (Reapproved 2006)D5830 14Standard Test Method forSolvents Analysis in Hazardous Waste Using GasChromatography1This standard is issued under the fixed designation D5830; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re
2、vision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method is used to determine qualitatively and quantitatively the presence of the followi
3、ng compounds in wastesamples using gas chromatography. This test method is designed for use as a screening method with a typical reporting level of0.1 %.Dichodifluoromethane TetrahydrofuranTrichlorofluoromethane Acetone1,1,2-Trichloro-1,2,2-trifluoroethaneMethyl Ethyl KetoneMIBKMethanol Cyclohexanon
4、eEthanol 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 Fluo
5、robenzene1,1-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 BromoformHep
6、tane CarbitolCyclohexane Ethyl EtherIsooctane 1,4-DioxaneNitropropane Diacetone AlcoholEthanolamine AcetonitrileNitromethane PyridineEthylene Chloride ToluidineBenzyl Chloride Ethylene GlycolPropylene Glycol1.1.1 This compound list is a compilation of hazardous solvents and other constituents that a
7、re routinely seen in hazardous wastesamples.1.2 The scope of this test method may be expanded to include other volatile and semivolatile organic constituents.1.2.1 Hydrocarbon mixtures such as kerosene and mineral spirits.1.2.2 High-boiling organics, defined here as compounds which boil above n-Hexa
8、decane.1.2.3 Other organics that the analyst is able to identify, either through retention time data or gas chromatography/massspectrometric (GC/MS) analysis.1 This test method is under the jurisdiction of ASTM Committee D34 on Waste Management and is the direct responsibility of Subcommittee D34.01
9、.06 on AnalyticalMethods.Current edition approved Feb. 1, 2006May 1, 2014. Published March 2006June 2014. Originally approved in 1995. Last previous edition approved in 20012006 asD5830 95(2001).(2006). DOI: 10.1520/D5830-95R06.10.1520/D5830-14.This document is not an ASTM standard and is intended o
10、nly to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit 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 ver
11、sionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States11.3 Gas chromatographic methods are recommended for use only by, or under close supervision of, an expe
12、rienced analyst.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2
13、. Referenced Documents2.1 ASTM Standards:2D1193 Specification 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 Update 1, July 199233. Summary of Test Method3.1 Waste samp
14、les are analyzed by direct injection, or by carbon disulfide, M-Pyrol, or other suitable solvent extraction andinjection of the extract into a gas chromatograph. Detection is achieved using a detector which is specific for the neededapplication, for example, flame ionization detector (FID), electron
15、 capture detector (ECD), thermal conductivity detector (TCD),photoionization detector (PID), or mass selective detector (MSD). This test method may be expanded to utilize other detector typesnot previously mentioned.4. Significance and Use4.1 This test method is useful in identifying the major solve
16、nt constituents in hazardous waste samples. This test method isdesigned to support field or site assessments, recycling operations, plant operations, or pollution control programs.5. Interferences5.1 Interferences may be encountered from any number of organic compounds that respond in the detector.A
17、lso, closely elutingcomponents may complicate identification based solely on retention time. When these types of interferences are encountered, theanalyst must rely on other sources of information for positive identification, such as:5.1.1 Gas chromatography/mass spectrometric (GC/MS) confirmation,
18、see EPA Method 8260, direct injection technique;5.1.2 Use of confirmation column, or confirmatory detector;5.1.2.1 This method identifies one column (DB1701) and one detector (FID) and utilizes three solvent standards and one QCdaily check. Use of confirmatory columns or detectors, or both, will als
19、o require the use of the three solvent standards (see Note2, 8.1) and QC daily check, one for each confirmatory column or detector, or both.5.1.3 Use of varying temperature programs or standard comparison, or both;5.1.3.1 Use of varying analytical programs will also require the use of three solvent
20、standards and QC daily check for eachvariation.5.1.4 Sample history, for example, any information available 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 syringe carr
21、yover. Immediately following each injection, the syringe should bethoroughly rinsed with carbon disulfide, or M-Pyrol. Other solvents such as methanol may be used as rinse solvents if sample typesnecessitate their use, but be aware that carryover and possible interferences may occur if the rinse sol
22、vent is not completely cleanedfrom the syringe before reuse. Before each injection the syringe must be thoroughly rinsed with the sample to be injected, wherethe first two pumps are flushed into a separate waste receptacle.5.3 When carbon disulfide (CS2) is used to extract solids or sludges that con
23、tain significant amounts of water, low recovery ofthe water miscible solvents may result.5.4 Some grades of CS2 may contain trace amounts of benzene.5.5 M-Pyrol seems to degrade slowly with time. The low-level degradation products interfere with some late eluting compoundson some columns (approximat
24、ely five small peaks).5.6 Interference from the CS2 solvent peak may occur if using a TCD.5.7 When using a TCD, be aware that water, as well as oxygenated compounds, for example, MEK, MIBK, may suppressdetector response.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactA
25、STM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402.D5830 1425.8 If an electrolytic condu
26、ctivity detector (ELCD) or electron capture detector (ECD) must be used, be aware that CS2,M-Pyrol, -Pyrol (required for an ELCD), and high concentrations of halogenated compounds may overload and possibly damagethe detector.both detectors. It is recommended that the ECDthese detectors be used only
27、when very low detection levels ofhalogenated compounds are expected and direct injection of the sample is possible.6. Apparatus6.1 Gas Chromatograph SystemEquipped with capillary or packed column injection ports, or both, detector, and data system.6.2 Recommended Chromatographic Columns:6.2.1 Capill
28、ary; Microbore or Megabore.6.2.1.1 DB-1701, 30M 0.25-mm inside diameter, 0.25-m film thickness.6.2.1.2 DB-624, 30M 0.3-mm inside diameter, 1.8-m film thickness.6.2.2 Packed: Stainless Steel or Glass.6.2.2.1 1 % SP-1000, 60/80 Carbopak B, 8-ft by 18-in. inside diameter.6.2.2.2 10 % SP-2100, 100/120 C
29、hromosorb WHP, 2M 2 mm ID.NOTE 1These columns are recommended and have shown to give good results. Operating conditions for each is listed in Section 10. Equivalent oralternative columns, or both, may be used depending on application.6.3 Glass Screw-Cap Vials or EquivalentTo collect samples and stor
30、e standards. Polytetrafluoroethylene or other inertmaterial should be used for the cap liner.6.4 Microsyringes, 1.0, 10, and 100 L.FIG. 1 Daily QC Standard FID/DB-1701D5830 1436.5 Analytical Balance, accurate to 0.0001 g.6.6 Pipettes, glass, disposable, or volumetric micropipettor or equivalent.6.7
31、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 be used in all tests. Unless otherwise indicated, it is intended that allreagents conform to the specifications of the Committe
32、e on Analytical Reagents of the American Chemical Society where suchspecifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accuracy of the determination.7.2 Purity of Water Unles
33、s otherwise indicated, references to water shall be understood to mean reagent water as defined byType II of Specification D1193.7.3 Nitrogen or Helium (High Purity)For carrier and makeup gases.Air and hydrogen (high purity) for fuel gases. Gases maybe obtained from a gas generator if available, thr
34、ough purification of a lower grade, or from a high-purity tank supply.7.4 Carbon Disulfide, CS2 Chromatography grade.7.5 M-Pyrol, Co5Ho9NOAvailable through several chemical suppliers and sources as 1-methyl-2-pyrrolidone.7.6 Individual Standards for Each Component of Interest99 % purity available fr
35、om many vendors.8. Standard Preparation8.1 Stock Standard SolutionsStock standards are prepared from pure standard materials. It is recommended that the standardsbe prepared so that each component is 5 to 10 % by weight. The stock standards must be prepared by directly weighing eachcomponent. For ex
36、tremely volatile components, such as ether and freons, it is recommended that a new stock standard be prepareddaily or as needed. If a dilution solvent is needed when preparing the stock standards, use the same solvent used for sampleextraction or dilution in Section 7.NOTE 2Due to the incompatibili
37、ty of some standard compounds, that is, some compounds are not miscible with each other, and also because of thenumber of compounds typically looked for in a single chromatographic run, it is advisable to prepare 3 or 4 standard solutions each composed of 10 to15 compounds. A set of standard chromat
38、ograms and a retention timetable should be available for reference.8.2 Secondary Working StandardsThese are prepared from stock standard solutions using the appropriate solvent. Secondarystandards should encompass the linear range of the GC system.NOTE 3Linear response and range must be established
39、with all detectors and chromatography systems used for quantitation. All calibration andsample analysis must be done within the established linear range.8.3 Calibration Check StandardAcalibration check standard should be prepared. The standard mixture should provide a goodoverall check of the GC/det
40、ector system. The compounds should cover the major compound types, for example, alcohols,aromatics, aliphatics, ketones, and halogenates.Atypical calibration check standard flame ionization detector (FID) chromatogramis shown in Fig. 1.9. Sample Collection, Preservation, and Handling9.1 Sample colle
41、ction should be in accordance with appropriate sampling protocols.9.2 Samples should be collected in glass containers, that have tightly sealing caps. If very volatile organics are of particularinterest, the headspace in the container should be kept to a minimum.9.3 Sample Transfer ImplementsImpleme
42、nts are required to transfer portions of waste samples from the sample containers tothe laboratory containers. Liquid samples may be transferred using disposable pipets. Solids and semisolids may be transferredusing a conventional laboratory spatula.9.4 Samples shall be handled maintaining safe labo
43、ratory practices. Any samples with special hazards must be appropriatelylabeled.9.5 Unused sample material, laboratory dilutions, and waste from the samples may be regulated. Consult your specialist or theregulations, or both, for guidance in the proper handling and disposal of laboratory wastes.4 R
44、eagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacope
45、ia and NationalFormulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.D5830 14410. Procedure10.1 Sample Preparation:10.1.1 Analyze liquid matrices with relatively low viscosity using direct injection into the GC, either as received or after dilutionwith CS2, M-Pyrol, or other suitable
46、 solvent.10.1.2 Analyze solid or semisolid samples as follows:10.1.2.1 For carbon disulfide or M-Pyrol preparation, weigh 3 g of the waste sample in a 15-mL glass vial. Add 3 g of carbondisulfide or M-Pyrol to the vial and the mixture is vortexed vigorously.After allowing the solids to settle, injec
47、t the CS2 or M-Pyrolextract into the GC.10.1.2.2 Use alternate sample sizes and extraction solvent weights if necessary. Actual sample size and solvent weight must berecorded in the appropriate sample preparation log book. It is essential for accurate waste sample analysis that sample size besuffici
48、ent to ensure a representative sample. If alternate sample size or extraction solvent volumes, or both, are used, this must bereflected in the calculations under the dilution factor in Section 11.10.1.3 Multiple phases or layers are typically present in hazardous waste samples. Depending on treatmen
49、t or processrequirements, it may be necessary to analyze each phase or layer 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/minSplit 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 minThreshold 4 unitsPe
