1、Designation: D 4547 09Standard Guide forSampling Waste and Soils for Volatile Organic Compounds1This standard is issued under the fixed designation D 4547; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision.
2、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 guide describes recommended procedures for thecollection, handling, and preparation of solid waste, soil, andsediment samples fo
3、r 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 s
4、oluble 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 conjunctio
5、nwith Guide D 4687.1.5 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 standar
6、d 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 Specification for Reagent WaterD 1586 Test Method for Penetration Test (SPT) and Split-Barrel Sampling of SoilsD 3550 Prac
7、tice for Thick Wall, Ring-Lined, Split Barrel,Drive Sampling of SoilsD 4687 Guide for General Planning of Waste SamplingD 4700 Guide for Soil Sampling from the Vadose ZoneD 5058 Test Methods for Compatibility of ScreeningAnalysis of WasteD 5792 Practice for Generation of Environmental DataRelated to
8、 Waste Management Activities: Development ofData Quality ObjectivesD 6051 Guide for Composite Sampling and Field Subsam-pling for Environmental Waste Management ActivitiesD 6282 Guide for Direct Push Soil Sampling for Environ-mental Site CharacterizationsD 6418 Practice for Using the Disposable En C
9、ore Samplerfor Sampling and Storing Soil for Volatile Organic Analy-sisD 6640 Practice for Collection and Handling of Soils Ob-tained in Core Barrel Samplers for Environmental Inves-tigationsE 856 Definitions of Terms and Abbreviations Relating toPhysical and Chemical Characteristics of Refuse Deriv
10、edFuel2.2 Federal Standard:Title 49 Transportation, Code of Federal Regulations(CFR), Part 172, List of Hazardous Substances andReportable Quantities33. Terminology3.1 sample, na portion of material taken from a largerquantity for the purpose of estimating properties or composi-tion of the larger qu
11、antity. (E 856)3.2 subsample, na portion of a sample taken for thepurpose of estimating properties or composition of the wholesample. (D 6051)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,
12、conditions for sample storage, sample pres-ervation, and two common means of sample preparation foranalysis. 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 shouldbe representat
13、ive 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 and headspace). The method of sample preparation for1This guide is under the jurisdiction of ASTM Committee D34 on WasteMana
14、gement and is the direct responsibility of Subcommittee D34.01.02 onSampling Techniques.Current edition approved July 1, 2009. Published August 2009. Originallyapproved in 1991. Last previous edition approved in 2006 as D 4547 - 06.2For referenced ASTM standards, visit the ASTM website, www.astm.org
15、, 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 Superintendent of Documents, U.S. Government PrintingOffice, Washington, DC 20402.1Copyright ASTM International,
16、100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.VOC analysis should be consistent with the data qualityobjectives (see Practice D 5792).5. Significance and Use5.1 This guide describes sample collection and handlingprocedures designed to minimize losses of VOCs. Th
17、e princi-pal mechanisms for the loss of VOCs 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 suscep
18、tible tovolatilization than compounds with 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 gai
19、n ofVOCs leads to analytical results that are unrepresentative offield conditions.5.2 Ancillary information concerning sample collection,handling and storage for VOC analysis is provided in Appen-dices Appendix X1, Appendix X2, and Appendix X3. Theseappendixes and cited references are recommended re
20、ading forthose unfamiliar with the many challenges presented 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 met
21、hod used to prepare thesample for VOC analysis, and meet the projects data qualityobjectives (see Practice D 5792). 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
22、organic analysis (VOA) vial orbottle meeting the specifications given in 7.3. When workingwith an uncharacterized solid waste, it is advisable to performcompatibility tests (see Test Methods D 5058) between thesample material and the solution (see 6.2 and 6.3) into whichit will be transferred in pre
23、paration for analysis. For instance,when collecting highly 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
24、be no chemical reaction which mayjeopardize the users safety.6.1.2 Figs. 1 and 2 are flow diagrams showing somedifferent 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 from a
25、sample with methanol and the subsequent transfer of an aliquotof the extract to water for either purge-and-trap or headspaceanalysis.FIG. 1 Sample Handling Options for Cohesive MaterialsD45470926.2.2 Advantages of methanol extraction are (1) largesamples or composite samples, or both, can be collect
26、ed toenhance representatives (see Guide D 6051), (2) biodegrada-tion is inhibited, (3) an efficient extraction of VOCs from thematrix materials can be achieved with methanol due to itsstrong affinity for these compounds and favorable wettingproperties, (4) a subsample can be analyzed several times,
27、and(5) sample extracts can be archived, if verified that VOC losseshave not occurred (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
28、) hazards to personnel dueto methanols 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, an
29、d (6) samples extractedwith methanol 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 con
30、tainer (see 7.3.2, 9.1and 9.2). Furthermore, 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 asampl
31、e by either purge-and-trap or headspace. In both cases,the sample is placed into a tared volatile analysis (VOA) vialcontaining water or a preservative solution (for example,acidified water) from which the vapor is removed for analysiswithout the container being opened.6.3.2 The principal advantages
32、 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 handling practices.6.3.3 The d
33、isadvantages 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) byautomated systems, (3
34、) 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, only a single analysis of the same sample can bemade; similarly only a single
35、analysis may be possible withheadspace analysis unless concentrations allow for the use of asmall injection volume.FIG. 2 Sample Handling Options for Non-Cohesive and Cementitious MaterialsD45470936.3.4 Limitations imposed by vapor phase partitioningmethods with regard to number of analyses that can
36、 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-ration step in the laboratory, so long as the sa
37、mple 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 Tools and Containers7.1 All sample handling devi
38、ces 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, and brass. Materials,such as polytetrafluorethyle
39、ne (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 very short period ofcontact with the sample or whe
40、n 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 and storage containers shouldbe cleaned in a manner
41、 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 for the geotechnicalindustry; however, several dev
42、ices have been developed spe-cifically for environmental sampling by direct push methods(Guide D 6282). The subsurface bulk sampling systems aredesigned to obtain intact cylindrical cores of material, ranginganywhere from 2.5 to 10.2 cm in diameter and 30.5 cm or morein length. Two geotechnical tool
43、s that have been used forsubsurface sample collection are the split-spoon sampler (TestMethod D 1586), which opens to expose the entire length ofthe material obtained for subsampling, and core barrel liners(ring-lined barrel sampling, see Practice D 3550) that aretypically subsampled through open en
44、ds. 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 D 6282) andare usually operated by direct push methods
45、. 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 are avail-able can be found in Guide D 4700 and
46、 Guide D 6282.Subsurface materials retrieved for VOC characterizationshould be obtained (sampling tubes filled and brought to thesurface) as quickly as possible and remain intact and undis-turbed until they are subsampled (see Practice D 6640). Sub-sampling a bulk sample should occur as quickly as p
47、ossibleafter it is brought to the surface. It is important for subsamplingto occur quickly because for bulk sample retrieval systemswhere the material is exposed directly to the atmosphere for aperiod of time during subsampling, there is an opportunity forVOC loss to occur. Suggested liner configura
48、tions and ex-amples of sampling techniques for bulk soil samples collectedby single tube direct push methods that provide limitedexposure of the soil being sampled to the atmosphere, aredescribed in Appendix X3 (see 8.1 through 8.3 for additionalsampling guidance).7.2.1 In addition to the coring dev
49、ices which retrieve bulkquantities of material, there are smaller hand-operated coringtools for obtaining samples of the appropriate size (for ex-ample, 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 should be constructed of materials that are nonreactiveand have airtight seals that show limited sorption and penetra-tion of VOCs. Hand-operated coring devices that are used tostore s
