1、Designation: D4547 15Standard Guide forSampling Waste and Soils for Volatile Organic Compounds1This standard is issued under the fixed designation D4547; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A
2、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 guide describes recommended procedures for thecollection, handling, and preparation of solid waste, soil, andsediment samples for
3、subsequent determination of volatileorganic compounds (VOCs). This class of compounds includeslow molecular weight aromatics, hydrocarbons, halogenatedhydrocarbons, ketones, acetates, nitriles, acrylates, ethers, andsulfides with boiling points below 200 Celsius (C) that areinsoluble or slightly sol
4、uble in water.1.2 Methods of sample collection, handling, storage, andpreparation for analysis are described.1.3 This guide does not cover the details of sampling design,laboratory preparation of containers, and the analysis of thesamples.1.4 It is recommended that this guide be used in conjunctionw
5、ith Guide D4687.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 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 t
6、o establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1586 Test Method for Penetration Test (SPT) and Split-Barrel Sampling of SoilsD3550 Practice f
7、or Thick Wall, Ring-Lined, Split Barrel,Drive Sampling of SoilsD4687 Guide for General Planning of Waste SamplingD4700 Guide for Soil Sampling from the Vadose ZoneD5058 Practices for Compatibility of Screening Analysis ofWasteD5681 Terminology for Waste and Waste ManagementD5792 Practice for Generat
8、ion of Environmental Data Re-lated to Waste Management Activities: Development ofData Quality ObjectivesD6051 Guide for Composite Sampling and Field Subsam-pling for Environmental Waste Management ActivitiesD6282 Guide for Direct Push Soil Sampling for Environ-mental Site CharacterizationsD6418 Prac
9、tice for Using the Disposable En Core Samplerfor Sampling and Storing Soil for Volatile Organic Analy-sisD6640 Practice for Collection and Handling of Soils Ob-tained in Core Barrel Samplers for Environmental Inves-tigations2.2 Federal Standard:Title 49 Transportation, Code of Federal Regulations (C
10、FR),Part 172, List of Hazardous Substances and ReportableQuantities33. Terminology3.1 sample, na portion of material taken from a largerquantity for the purpose of estimating properties or composi-tion of the larger quantity. (D5681)3.2 subsample, na portion of a sample taken for thepurpose of estim
11、ating properties or composition of the wholesample. (D6051)3.2.1 DiscussionA subsample, by definition, is also asample.4. Summary of Guide4.1 This guide addresses the use of tools for sample collec-tion and transfer, conditions for sample storage, samplepreservation, and two common means of sample p
12、reparationfor analysis. Special attention is given to each step from samplecollection to analysis to limit the loss of VOCs by volatilizationand biodegradation. The sample collected and analyzed should1This guide is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct re
13、sponsibility of Subcommittee D34.01.02 onSampling Techniques.Current edition approved Sept. 1, 2015. Published October 2015. Originallyapproved in 1991. Last previous edition approved in 2009 as D4547 - 09. DOI:10.1520/D4547-15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, or
14、contact 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 Superintendent of Documents, U.S. Government PrintingOffice, Washington, DC 20402.Copyright ASTM International, 100 B
15、arr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1be representative of the matrix material sampled. The twomethods cited for the preparation of samples for VOC analysisare methanol extraction and vapor partitioning (that is, purge-and-trap, headspace, and vacuum distilla
16、tion). The method ofsample preparation for VOC analysis should be consistent withthe data quality objectives (see Practice D5792).5. Significance and Use5.1 This guide describes sample collection and handlingprocedures designed to minimize losses of VOCs. The princi-pal mechanisms for the loss of VO
17、Cs from materials duringcollection, handling and storage are volatilization and biodeg-radation. Susceptibility of various VOCs to these two lossmechanisms is both compound and matrix specific. In general,compounds with higher vapor pressures are more susceptible tovolatilization than compounds with
18、 lower vapor pressures.Also, aerobically degradable compounds are generally moresusceptible to biodegradation than anaerobically degradablecompounds. In some cases, the formation of other compoundsnot originally present in the material can occur. Loss or gain ofVOCs leads to analytical results that
19、are unrepresentative offield conditions.5.2 Ancillary information concerning sample collection,handling and storage for VOC analysis is provided in Appen-dix X1, Appendix X2, and Appendix X3. These appendixesand cited references are recommended reading for thoseunfamiliar with the many challenges pr
20、esented during thecollection, handling and storage of samples for VOC analysis.6. Selection of Sample Preparation Method for VOCAnalysis6.1 Introduction:6.1.1 Sample collection, handling, and preservation meth-ods should be compatible with the method used to prepare thesample for VOC analysis, and m
21、eet the projects data qualityobjectives (see Practice D5792). Preparation of a sample forinstrumental analysis can be initiated either in the field orlaboratory. In either case, prior to analysis, the sample shouldbe placed into a tared volatile organic analysis (VOA) vial orbottle meeting the speci
22、fications given in 7.3. When workingwith an uncharacterized solid waste, it is advisable to performcompatibility tests (see Test Methods D5058) between thesample material and the solution (see 6.2 and 6.3) into whichit will be transferred in preparation for analysis. For instance,when collecting hig
23、hly contaminated soils or waste of un-known composition, it is strongly recommended that prelimi-nary testing be performed to adequately characterize the wastematerials so that when the user applies the procedures cited inthis guide, there will be no chemical reaction which mayjeopardize the users s
24、afety.6.1.2 Figs. 1 and 2 are flow diagrams showing someFIG. 1 Sample Handling Options for Cohesive MaterialsD4547 152different options for combining sample collection, handlingand preparation methods for instrumental analysis.6.2 Methanol Extraction:6.2.1 This method involves the extraction of VOCs
25、 from asample with methanol and the subsequent transfer of an aliquotof the extract to water for either purge-and-trap, headspaceanalysis, or vacuum distillation.6.2.2 Advantages of methanol extraction are (1) largesamples or composite samples, or both, can be collected toenhance representatives (se
26、e Guide D6051), (2) biodegradationis inhibited, (3) an efficient extraction of VOCs from the matrixmaterials can be achieved with methanol due to its strongaffinity for these compounds and favorable wetting properties,(4) a subsample can be analyzed several times, and (5) sampleextracts can be archi
27、ved, if verified that VOC losses have notoccurred (see 10.1.1).6.2.3 The primary disadvantages of methanol extraction are(1) samples may have to be shipped as a flammable liquiddepending on the amount of methanol present (for example,U.S. DOT reg. 49CFR172.101), (2) hazards to personnel dueto methan
28、ols toxicity and flammability, (3) detection limits areelevated due to analyte dilution, (4) possible interference of themethanol peak with VOCs of interest, (5) potential adverseimpact of methanol on the performance of certain gaschromatograph/detector systems, and (6) samples extractedwith methano
29、l must be disposed of as a regulated waste.6.2.4 Logistical challenges of performing these tasks in thefield can be overcome by extracting samples with methanolonce they have been received in a laboratory, provided that thesamples are transported in an airtight container (see 7.3.2, 9.1and 9.2). Fur
30、thermore, if VOC levels are unknown, a replicatesample can be obtained and screened to determine if methanolextraction is appropriate for the expected contaminant concen-trations.6.3 Vapor Partitioning:6.3.1 Vapor partitioning involves the direct analysis of asample by either purge-and-trap, headspa
31、ce, or vacuum distil-lation. In each case, the sample is placed into a tared volatileanalysis (VOA) vial or flask (for vacuum distillation) contain-ing water or a preservative solution (for example, acidifiedwater) from which the vapor is removed for analysis withoutthe container being opened.6.3.2
32、The principal advantages of this method are (1)itcanoffer lower detection limits than methanol extraction becauseno dilution is involved, (2) there are no organic solventinterferences, and (3) there is no use of regulated organicsolvents, which may require special shipment, disposal, andfield handli
33、ng practices.6.3.3 The disadvantages associated with vapor partitioningare (1) the VOA vial (VOA vials are different sizes forautomated purge-and-trap and headspace instrumentation) oradapter used in conjunction with a VOAvial, or both, often areinstrument specific, (2) sample size is limited (10 g)
34、 byautomated systems, (3) a matrix-appropriate method of pres-ervation may be necessary (see Appendix X2), (4) vaporpartitioning is less efficient at recovering VOCs from somematerials than methanol extraction, and (5) when using purge-and-trap or vacuum distillation, only a single analysis of thesa
35、me sample can be made; similarly only a single analysis mayFIG. 2 Sample Handling Options for Non-Cohesive and Cementitious MaterialsD4547 153be possible with headspace analysis unless concentrationsallow for the use of a small injection volume.6.3.4 Limitations imposed by vapor phase partitioningme
36、thods with regard to number of analyses that can beperformed on a single sample can be addressed by takingreplicate samples.6.3.5 When employing vapor phase partitioning methods,the logistical challenges of performing sample preparation inthe field (see 7.3.3) can be avoided by performing the prepa-
37、ration step in the laboratory, so long as the sample is trans-ported to the laboratory in an airtight container (see 7.2.1). IfVOC levels are unknown, a replicate sample can be obtainedand screened to determine if it is appropriate to use a vaporpartitioning method of sample preparation.7. Sampling
38、Tools and Containers7.1 All sample handling devices and vessels used to collectand store samples for analysis should be constructed ofnonreactive materials that will not sorb, leach or diffuseconstituents of interest. Examples of materials that meet thesecriteria are glass, stainless steel, steel, a
39、nd brass. Materials,such as polytetrafluoroethylene (PTFE) and many rigid plasticsalso can be used; however, it should be recognized that theymay have some limited adsorptive properties or allow slowdiffusive passage of some VOCs. Materials which show limitedreactivity can be used when they have a v
40、ery short period ofcontact with the sample or when they are necessary for makingairtight (hermetic) seals. Collection tools and storage contain-ers made of materials other than those cited in this sectionshould only be used after they have demonstrated equivalency(see 7.2.1). All collection tools an
41、d storage containers shouldbe cleaned in a manner consistent with their intended use.7.2 ToolsThere are often several steps to sampling, par-ticularly if it involves obtaining bulk material from thesubsurface. Most of the equipment used to obtain samples fromthe subsurface was originally developed f
42、or the geotechnicalindustry; however, several devices have been developed spe-cifically for environmental sampling by direct push methods(Guide D6282). The subsurface bulk sampling systems aredesigned to obtain intact cylindrical cores of material, ranginganywhere from 2.5 to 10.2 cm in diameter and
43、 30.5 cm or morein length. Two geotechnical tools that have been used forsubsurface sample collection are the split-spoon sampler (TestMethod D1586), which opens to expose the entire length of thematerial obtained for subsampling, and core barrel liners(ring-lined barrel sampling, see Practice D3550
44、) that aretypically subsampled through open ends. Core barrel linersshould not be used for storage of samples intended for VOCanalysis because they do not have airtight seals, see AppendixX1. Single tube and dual tube sampling devices have beendeveloped for environmental applications (Guide D6282) a
45、ndare usually operated by direct push methods. Sample linersused in the bulk sampling systems come in a variety of lengthsand materials (stainless steel, brass, PTFE, rigid plastics, etc.).Additional information on the design and application ofdifferent types of subsurface collection systems that ar
46、e avail-able can be found in Guide D4700 and Guide D6282. Subsur-face materials retrieved for VOC characterization should beobtained (sampling tubes filled and brought to the surface) asquickly as possible and remain intact and undisturbed untilthey are subsampled (see Practice D6640). Subsampling a
47、 bulksample should occur as quickly as possible after it is brought tothe surface. It is important for subsampling to occur quicklybecause for bulk sample retrieval systems where the material isexposed directly to the atmosphere for a period of time duringsubsampling, there is an opportunity for VOC
48、 loss to occur.Suggested liner configurations and examples of samplingtechniques for bulk soil samples collected by single tube directpush methods that provide limited exposure of the soil beingsampled to the atmosphere, are described in Appendix X3 (see8.1 through 8.3 for additional sampling guidan
49、ce).7.2.1 In addition to the coring devices which retrieve bulkquantities of material, there are smaller hand-operated coringtools for obtaining samples of the appropriate size (forexample, coring devices capable of collecting 3- and 15-cm3volumes, for collection of approximately 5- and 25-g samples,respectively) for analysis (see Fig. 3). If one of these smallercoring devices is used to store the sample (see 9.1.1), the mainbody shall be constructed of materials that are nonreactive andhave airtight seals that show limited sorption and penetration ofVOCs. Hand-operated cor
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