1、Designation: D 7339 07Standard Test Method forDetermination of Volatile Organic Compounds Emitted fromCarpet using a Specific Sorbent Tube and ThermalDesorption / Gas Chromatography1This standard is issued under the fixed designation D 7339; the number immediately following the designation indicates
2、 the year oforiginal adoption or, in the case of revision, 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 describes an analytical proce
3、dure foridentifying and quantifying the masses of individual volatileorganic compounds (individual VOCs or IVOCs) that areemitted into a flow of air from carpet specimens and collectedon sorbent sampling tubes during emissions testing.1.2 This test method will be used in conjunction with astandard p
4、ractice for sampling and preparing carpet specimensfor emissions testing. If a specific chamber practice is notavailable for the carpet specimens, this standard test methodshould be used in conjunction with approved standard practicesfor emissions testing and sample preparation.1.3 When used in conj
5、unction with standard practices forcarpet specimen preparation and collection of vapor-phaseemissions , this test method will provide a standardized meansof determining the levels of IVOC in the exhaust stream of theemissions test chamber/cell. If this test method is used with areliable practice for
6、 emissions testing, these IVOC levels canbe used to determine the emission rate from a unit quantity(usually surface area) of the sample material under test.1.4 VOCs in the exhaust stream of an emissions test deviceare collected on thermal desorption tubes packed with aspecific combination of sorben
7、ts using active (pumped) sam-pling. (See Practice D 6196 for a more general description ofvapor collection using pumped sampling onto sorbent tubes).The samples are analyzed by thermal desorption (TD) with gaschromatography and mass spectrometry detection (GC/MS)and/or flame ionization detection (FI
8、D) depending upon therequirements of the specific materials emissions testing/certification protocol.1.5 This test method can be used for the measurement ofmost GC-compatible organic vapors ranging from the approxi-mate volatility from n-hexane to n-hexadecane (that is, com-pounds with vapor pressur
9、es ranging from 16 kPa to 4 3 10-4kPa at 25C). Properties other than a compounds vaporpressure such as affinity for the sorbent may need to be takeninto account. Compounds with vapor pressures outside thisrange may or may not be quantifiable by this method. How-ever, qualitative data concerning the
10、identity of a compound(s),outside the stated volatility range for quantitation, may still beuseful to the user. The method can be applied to analytes overa wide concentration rangetypically 1 g/m3to 1 mg/m3concentration of vapor in the exhaust air from the emission cellor chamber.1.6 This test metho
11、d is not capable of quantifying allcompounds which are emitted from carpets. See the appropri-ate test practices/methods for determining other compoundsthat are not amenable to analysis by gas chromatography (thatis, Test Method D 5197 for the determination of aldehydes).1.7 This standard does not p
12、urport 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 use.2. Referenced Documents2.1 ASTM Standards:2
13、D 1356 Terminology Relating to Sampling and Analysis ofAtmospheresD 3686 Practice for Sampling Atmospheres to Collect Or-ganic Compound Vapors (Activated Charcoal Tube Ad-sorption Method)D5116 Guide for Small-Scale Environmental Chamber De-terminations of Organic Emissions From Indoor Materials/Prod
14、uctsD 5197 Test Method for Determination of Formaldehydeand Other Carbonyl Compounds in Air (Active SamplerMethodology)D 5337 Practice for Flow Rate Calibration of PersonalSampling PumpsD 6196 Practice for Selection of Sorbents, Sampling, andThermal Desorption Analysis Procedures for Volatile Or-gan
15、ic Compounds in AirD 6670 Practice for Full-Scale Chamber Determination of1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.Current edition approved April 1, 2007. Published May 2007.2For referenced A
16、STM 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Consho
17、hocken, PA 19428-2959, United States.Volatile Organic Emissions from Indoor Materials/ProductsD 7143 Practice for Emission Cells for the Determination ofVolatile Organic Emissions from Indoor Materials/ProductsE 355 Practice for Gas Chromatography Terms and Rela-tionships2.2 ISO Standards:3EN ISO 16
18、000-6 Determination of volatile organic com-pounds in indoor and test chamber air by active samplingon Tenax TA sorbent, thermal desorption and gas chroma-tography using MS/FIDEN ISO 16000-9 Indoor AirPart 9: Determination of theemission of volatile organic compounds from buildingproducts and furnis
19、hingsEmission test chamber methodEN ISO 16000-10 Indoor AirPart 10: Determination ofthe emission of volatile organic compounds from buildingproducts and furnishingsEmission test cell methodEN ISO 16000-11 Indoor AirPart 11: Determination ofthe emission of volatile organic compounds from buildingprod
20、ucts and furnishingsSampling, storage of samplesand preparation of test specimens2.3 US EPA Methods:4TO-15 Determination of Volatile Organic Compounds(VOCs) in Air Collected in Specially-Prepared Canistersand Analyzed by Gas Chromatography/Mass Spectrom-etry (GC/MS)TO-17 Determination of Volatile Or
21、ganic Compounds inAmbient Air Using Active Sampling onto Sorbent Tubes3. Terminology3.1 DefinitionsRefer to Terminology D 1356 and PracticeE 355 for definitions of terms used in this test method.4. Summary of Test Method4.1 A sample of the VOCs emitted from a carpet specimenis collected following th
22、e preparation and collection guidelinesprovided in the appropriate chamber/emission cell practices/guides. See, for example Guide D5116 (small chamber),Practice D 6670 (full-scale chamber), Practice D 7143 (emis-sion cells), EN ISO 16000-9 (small chambers),EN ISO 16000-10 (emission cells), ENV 13419
23、-1 (smallchambers), ENV 13419-2 (emission cells), andEN ISO 16000-11 16000-11 (sample preparation).4.2 Organic vapors in the exhaust stream of an emission testchamber or cell are pumped onto standard thermal desorptiontubes (see Practice D 6196) containing either 200 mg of apolyphenylene oxide resin
24、-based (PPOR-B) sorbent with ashort bed (1-2 mm) of quartz wool, a glass frit, or stainless steelscreen at each end of the 200 mg of PPOR-B sorbent. Thepump flow rate and sampling time must be controlled (seePractice D 6196). The sorbent tubes are then thermally des-orbed, in a reverse flow of carri
25、er gas, using appropriatetwo-stage desorption apparatus, (See Practice D 6196) suchthat volatile organic compounds are transferred (injected)efficiently into the capillary GC column for analysis.4.3 GC-compatible organic compounds which are retainedby the PPOR-B sorbent or quartz/PPOR-B sorbent tube
26、 duringvapor collection and which elute between n-C6and n-C16on a100 %, polydimethylsiloxane (PDMS) fused silica capillarycolumn are identified and quantified by gas chromatography/mass spectrometry (see Section 11). Selective ion monitoring,ion extraction or spectral de-convolution shall be used to
27、quantify specific volatile organic compounds. Individual com-ponents of interest are quantified using authentic standards ofthat particular compound. Other compounds are quantifiedusing toluene as the surrogate standard reference material (see11.7.2).NOTE 1The procedure is similar to that outlined i
28、n EN ISO 16000-6.5. Significance and Use5.1 Manufacturers of carpet need to monitor emissions ofVOCs to assess the environmental impact of their productsindoors. These results are also used to demonstrate compliancewith VOC emission limits for individual VOCs.5.2 These data are also used to understa
29、nd which VOCs areemitted from a product or material and to measure themagnitude of those emissions.5.3 Emission data may be used to compare different lots ofcarpet of the same materials of construction, or carpetscomposed of different materials of construction, in order todevelop products with lower
30、 emissions and lower potentialenvironmental impact.5.4 This test method should be used in conjunction withpractices/guidelines for emissions testing such as GuideD5116, Practice D 7143, EN ISO 16000-9 andEN ISO 16000-10. These detail how to select and preparesamples and how and when to carry out emi
31、ssions tests suchthat the concentration and profile of vapors in the exhaust air ofthe emission chamber/cell are representative of the productunder test. This standard method covers the sampling andanalysis of volatile organic compounds in the exhaust gas fromthe chamber/cell using thermal desorptio
32、ncompatible sor-bent tubes and will provide the necessary analytical consis-tency to ensure that reproducible data is obtained for theanalysis of identical vapor samples by different laboratories.6. Interferences6.1 Organic compounds that have the same or nearly thesame retention times as the analyt
33、e of interest can interfereduring gas chromatographic analysis. High resolution capillarycolumns are required to minimize these issues. Artifacts can begenerated during sampling and analysis. Interferences can beminimized by proper selection of gas chromatographic col-umns and conditions, and by str
34、ingent conditioning of both thesorbent tubes and the analytical system before use. Artifactsmay be formed during storage of blank sorbent tubes. This isminimized by correctly sealing and storing blank and sampledtubes (see 7.3 and 10.1). The effectiveness of these methods for3Available from American
35、 National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.4Found in “Compendium of Methods for the Determination of Toxic OrganicCompounds in Ambient Air,” 2nd Ed., 1999, US. Environmental ProtectionAgency/625/R-96/010b. Available from United States Envir
36、onmental ProtectionAssociation (EPA),Ariel Rios Bldg., 1200 PennsylvaniaAve., NW, Washington, DC20460, http:/www.epa.gov.D7339072controlling the potential interferences can be demonstrated byproper quality assurance procedures including the use of blanksand spiked sampling tubes.NOTE 2Note that inhe
37、rent artifact levels will vary from sorbent tosorbent but are generally at sub-nanogram levels for quartz wool, PPOR-Band for carbon-black type sorbent (see Practice D 6196).6.2 Compounds of interest that co-elute chromatographi-cally, are not distinguishable when using an FID. Identificationand qua
38、ntification shall be done using a mass spectrometer inthe selected ion monitoring (SIM) mode, or in SCAN mode incombination with post-run processing using spectral deconvo-lution, or ion extraction, or both.6.3 Even if mass spectroscopy is employed, it may not bepossible to uniquely identify individ
39、ual compounds whensimilar compounds co-elute exactly (co-maximize) under theanalytical conditions selected.6.4 The method is suitable for sampling and analyzingvapor samples ranging up to 95 % relative humidity for allhydrophobic sorbents such as quartz wool, PPOR-B andgraphitized carbon blacks. Whe
40、n less hydrophobic, strongsorbents such as carbonized molecular sieves are used in asecondary (back-up) tube, (see Note 3 and Note 8) care must betaken to reduce the mass of water retained from humid samples(see Practice D 6196).7. Apparatus7.1 Sorbent Tubes for Pumped SamplingSample tubes(see Pract
41、ice D 6196) packed with 200 mg of PPOR-B sorbentor with a combination of 1 or 2 mm of loosely packed quartzwool, glass frit, or stainless steel screens bracketing 200 mg ofPPOR-B sorbent should be used for collection of the volatileorganic vapors in the exhaust gas from the emission chamber/cell. An
42、alyses of glass or stainless steel spiked tubes indicatesthat similar results are obtained using either glass wool, orstainless steel frits, as long as the sorbent is in the heated zoneof the thermal desorber (see 12.2).NOTE 3Note that use of a secondary back-up tube can serve as auseful check on th
43、e breakthrough volume of the primary PPOR-B orquartz/PPOR-B tubes. Breakthrough should be determined using twosorbent tubes containing the same sorbent and placed in series. Tubeperformance should be addressed by individual laboratory QC programs,see EPA Method TO-17 for guidance.7.2 Sorbent Tube En
44、d Caps for Long-term Storage Blankand sampled tubes should be sealed with metal screw-capfittings with combined (one-piece) PTFE ferrules for storageand transportation. If alternate fittings are used, the laboratoryshould determine that they meet storage and transportationstability requirements.NOTE
45、 4As a quick test that long term storage caps have been fittedcorrectly, check the length of the capped tube to make sure the seals areseated as far down the tube as possible and check that the caps cannot bepulled off the tubes by hand using reasonable force.7.3 SyringesA precision 10L liquid syrin
46、ge readable to0.1 L.7.4 Soap Bubble MeterA soap bubble flow meter oranother suitable calibrated device is required for calibratingpump, desorption, and split flows. Follow the manufacturersrecommended procedure and or the participating laboratoryQC program. See Practice D 3686 for further guidance.7
47、.5 Thermal Desorption ApparatusA two-stage apparatusis required for thermally desorbing VOCs retained on thesorbent tubes and transferring/injecting them into a gas chro-matograph (GC) in a flow of inert carrier gas. A typicalapparatus contains a mechanism for holding the tubes to bedesorbed while t
48、hey are heated and purged simultaneously withinert carrier gas. The sample flow path through the thermaldesorber must be constructed entirely of inert materials (that is,quartz, fused silica, silica-coated steel, PTFE, etc.), includingall valve components which may come into contact withsample vapor
49、s. The desorption temperature and time should beadjustable, as should the carrier gas flow rate. Air must bepurged from the sample tube and analytical system before heatis applied to prevent sorbent and analyte oxidation. None of thepurged air should be allowed to reach the GC column ordetector. The apparatus should incorporate a stringent leak testof every sample (see Note 5) to check flow path integritybefore sample desorption/analysis. The secondary focusing(cold) trap should contain appropriate sorbents and be ofsufficient internal diameter to prevent i
