1、Designation: D 4547 06Standard 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 (e) 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 f
3、or 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
4、soluble 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 conjuncti
5、onwith Guide D 4687.1.5 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 to
6、 use. See 7.2 and 8.1.1for specific warnings.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 3350 Specification for Polyethylene Plastics Pipe andFittings MaterialsD 4687 Guide for General Planning of Waste SamplingD 4700 Guide for Soil Sampling from the Vadose Zon
7、eD 5058 Test Methods for Compatibility of ScreeningAnalysis of WasteD 5792 Practice for Generation of Environmental DataRelated to Waste Management Activities: Development ofData Quality ObjectivesD 6051 Guide for Composite Sampling and Field Subsam-pling for Environmental Waste Management Activitie
8、sD 6418 Practice for Using the Disposable En Core 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 toPhysica
9、l and Chemical Characteristics of Refuse DerivedFuel2.2 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 estimati
10、ng properties or composi-tion of the larger quantity. (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
11、of tools for sample collec-tion and transfer, 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 samp
12、le collected and analyzed shouldbe 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 and headspace). The method of sample preparation forVOC analysis should be con
13、sistent with the data qualityobjectives (see Practice D 5792).1This guide is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.02 onMonitoring.Current edition approved Feb. 1, 2006. Published March 2006. Originallyapproved in 1991
14、. Last previous edition approved in 2003 as D 4547 - 03.2For 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.3Avai
15、lable from Superintendent of Documents, U.S. Government PrintingOffice, Washington, DC 20402.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 This guide describes sample collection and handlingprocedures des
16、igned to minimize losses of VOCs. The 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 hi
17、gher vapor pressures are more susceptible 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
18、 the material can occur. Loss or gain 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 inAppendixX1 and Appendix X2. These appendixes and cited referencesare recomm
19、ended reading for those unfamiliar with the manychallenges presented during the collection, handling and stor-age 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 wi
20、th the method 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
21、 volatile 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 transfer
22、red in preparation 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, t
23、here will 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:FIG. 1 Sample Handling Options for Cohesive Ma
24、terialsD45470626.2.1 This method involves the extraction of VOCs from asample with methanol and the subsequent transfer of an aliquotof the extract to water for either purge-and-trap or headspaceanalysis.6.2.2 Advantages of methanol extraction are (1) largesamples or composite samples, or both, can
25、be collected 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 sever
26、al times, 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. 49CFR17
27、2.101), (2) 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 s
28、ystems, and (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 ai
29、rtight container (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
30、 of asample 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
31、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 handling practices.6
32、.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) byautomated s
33、ystems, (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, only a single analysis of the same sample can beFIG. 2 Sample Handli
34、ng Options for Non-Cohesive and Cementitious MaterialsD4547063made; similarly only a single analysis may be possible withheadspace analysis unless concentrations allow for the use of asmall injection volume.6.3.4 Limitations imposed by vapor phase partitioningmethods with regard to number of analyse
35、s 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-ration step in the laboratory, so long
36、 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 Tools and Containers7.1 All sample han
37、dling 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, and brass. Materials,such as polytetraf
38、luorethylene (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 sam
39、ple 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 and storage containers shouldbe cleaned i
40、n a manner consistent with their intended use.7.2 ToolsThere are often several steps to sampling, par-ticularly if it involves obtaining bulk materials from subsurfaceregions. Most of the equipment used to obtain samples fromthe subsurface was originally developed for the geotechnicalindustry. These
41、 subsurface bulk sample retrieval systems aredesigned to obtain intact cylindrical cores of material, ranginganywhere from 1 to 4 in. in diameter, and 1 to several ft inlength. Two commonly used collection devices for subsurfacesample collection are the split-spoon corer that opens to exposethe enti
42、re length of the material obtained for subsampling andcore barrel liners (that is, ring-lined barrel sampling, seePractice D 3550) that typically are subsampled through theopen ends. Core barrel liners fit snugly within a corer and comein a variety of lengths and materials (stainless steel, brass,PT
43、FE, rigid plastics, etc.). Several liners, or a single long liner,can be placed within the core barrel, depending on thesampling plan (See Warning at the end of this paragraph).Additional information on the application and design ofdifferent types of subsurface collection systems available canbe fou
44、nd in Guide D 4700. Subsurface materials retrieved forVOC characterization should be obtained (sampling tubesfilled and brought to the surface) as quickly as possible andremain intact and undisturbed until they are subsampled (seePractice D 6640). Subsampling of a bulk sample should occurwithin a co
45、uple minutes of its being brought to the surface (see8.1 through 8.3 for additional sampling guidance).(WarningCore barrel liners are not recommended for stor-age of samples intended for VOC analysis because they do nothave airtight seals (see Appendix X1).)7.2.1 In addition to the coring devices wh
46、ich 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
47、 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 samples should be evaluated
48、 using the procedure given inAppendix X3 to ensure that the device meets these criteria.When the coring device is only used to rapidly transfer thesample to a VOA vial, corer material requirements are lessstringent.7.3 ContainersVOAvials and bottles used for storage andpreparation of samples for ana
49、lysis should be made of glassand have airtight seals. To achieve an airtight seal, thesecontainers should have a thick septum cushion between thesealing material (PTFE) and cap (rigid plastic screw cap oraluminum crimp top). PTFE-lined caps that do not haveflexible septum backing often fail to achieve a liquid or airtightseal. Furthermore, the thickness of the PTFE used for a linedseptum should be at least 10 mil (0.254 mm).7.3.1 Preparation of VOA Vial or BottleRecord the taredweight of the VOA vial or bottle and cap prior to the samplingevent. Moreover, depending on the
