1、Designation: D5466 01 (Reapproved 2007)D5466 15Standard Test Method forDetermination of Volatile Organic ChemicalsCompounds inAtmospheres (Canister Sampling Methodology)1This standard is issued under the fixed designation D5466; the number immediately following the designation indicates the year ofo
2、riginal adoption or, in the case of revision, 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 standard describes a procedure for sampling
3、 and analysis of selected volatile organic compounds (VOCs)in ambient, indoor, orand workplace atmospheres. The test method is based on the collection of whole air samples in stainless steelcanisters with specially treated (passivated) interior surfaces. For sample analysis, a portion of the sample
4、is subsequently removedfrom the canister and the collected VOCs are selectively concentrated by adsorption or condensation onto a trap, subsequentlyreleased by thermal desorption, separated by gas chromatography, and measured by a mass spectrometric detector or otherdetector(s). This test method des
5、cribes procedures for sampling into canisters to final pressures both above and below atmosphericpressure (respectively referred to as pressurized and subatmospheric pressure sampling).21.2 This test method is applicable to specific VOCs that have been tested and determined to be stable when stored
6、in canisters.Numerous compounds, many of which are chlorinated VOCs, have been successfully tested for storage stability in pressurizedcanisters (1-4).3 Although not as extensive, documentation Documentation is also available demonstrating stability of VOCs insubatmospheric pressure canisters. While
7、 initial studies were concentrated on non-polar VOCs, information on storage stability hasbeen extended to Information on storage stability is available for many polar compounds as well (5-7).1.3 The procedure for collecting the sample involves the use of inlet lines and lines, air filters, flow rat
8、e regulators for obtainingtime-integrated samples, and in the case of pressurized samples, an air pump. Canister Typical long-term fixed location canistersamplers have been designed to automatically start and stop the sample collection process using electronically actuated valves andtimers (8-10). T
9、emporary or short-term canister samplers may require the user to manually start and stop sample collection. Aweatherproof shelter is may be required if the sampler is to be usedused outdoors. For the purposes of this test method, refer toPractice D1357 outside. for practices and planning ambient sam
10、pling events.1.4 The organic compounds that have been successfully measured at single-digit parts-per-billion by volume (ppbv) levels withthis test method are listed in Table 1. ThisThe test method is applicable to VOC concentrations ranging from the detection limitto approximately 300 ppbv. Above t
11、his concentration, samples require dilution smaller sample aliquots of sample gas may beanalyzed or samples can be diluted with dry ultra-high-purity nitrogen or air.1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.6 This
12、 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. Safety practices should
13、be part of the users SOP manual.2. Referenced Documents2.1 ASTM Standards:4D1356 Terminology Relating to Sampling and Analysis of AtmospheresD1357 Practice for Planning the Sampling of the Ambient AtmosphereE260 Practice for Packed Column Gas ChromatographyE355 Practice for Gas Chromatography Terms
14、and Relationships1 This test method is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.Current edition approved April 1, 2007Dec. 1, 2015. Published June 2007June 2016. Originally approved in 1993. Last previous editio
15、n approved in 20012007 asD5466 01.D5466 01 (2007). DOI: 10.1520/D5466-01R07.10.1520/D5466-15.2 This test method is based on EPACompendium Method TO-14, “The Determination of Volatile Organic Compounds (VOCs) inAmbientAir Using SUMMAPassivatedCanister Sampling and Gas Chromatographic Analysis,” May 1
16、988.3 The boldface numbers in parentheses refer to the list of references at the end of the standard.4 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Do
17、cument Summary page on the ASTM website.This document is not an ASTM standard and is intended only 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
18、 recommends that users consult prior editions as appropriate. In all cases only the current versionof 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 States1TABLE 2
19、Ion/Abundance and Expected Retention Time for Selected VOCs Analyzed by GC-MS-SIMCompoundIon/Abundance(amu/%base peak)ExpectedRetentionTime (min)Freon 12 (Dichlorodifluoromethane) 85/100 5.0187/31Methyl chloride (Chloromethane) 50/100 5.6952/34Freon 114 (1,2-Dichloro-1,1,2,2-tetrafluoroethane) 85/10
20、0 6.55135/5687/33Vinyl chloride (Chloroethene) 62/100 6.7127/12564/32Methyl bromide (Bromomethane) 94/100 7.8396/85Ethyl chloride (Chloroethane) 64/100 8.4329/14027/140Freon 11 (Trichlorofluoromethane) 101/100 9.97103/67Vinylidene chloride (1,1-Dichloroethylene) 61/100 10.9396/5563/31Dichloromethane
21、 (Methylene chloride) 49/100 11.2184/6586/45Freon 113 (1,1,2-Trichloro-1,2,2-trifluoroethane) 151/100 11.60101/140103/901,1-Dichloroethane 63/100 12.5027/6465/33cis-1,2-Dichloroethylene 61/100 13.4096/6098/44Chloroform (Trichloromethane) 83/100 13.7585/6547/351,2-Dichloroethane (Ethylene dichloride)
22、 62/100 14.3927/7064/31Methyl chloroform (1,1,1-Trichloroethane) 97/100 14.6299/6461/61Benzene 78/100 15.0477/2550/35Carbon tetrachloride (Tetrachloromethane) 117/100 15.18119/971,2-Dichloropropane (Propylene dichloride) 63/100 15.8341/9062/70Trichloroethylene (Trichloroethene) 130/100 16.10132/9295
23、/87cis-1,3-Dichloropropene 75/100 16.9639/7077/30trans-1,3-Dichloropropene 75/100 17.4939/7077/301,1,2-Trichloroethane (Vinyl trichloride) 97/100 17.6183/9061/82Toluene (Methyl benzene) 91/100 17.8692/571,2-Dibromoethane (Ethylene dibromide) 107/100 18.48109/9627/115Tetrachloroethylene (Perchloroeth
24、ylene) 166/100 19.01164/74131/60Chlorobenzene 112/100 19.7377/62114/32D5466 152TABLE 2 ContinuedCompoundIon/Abundance(amu/%base peak)ExpectedRetentionTime (min)Ethylbenzene 91/100 20.20106/28m,p-Xylene (1,3/1,4-dimethylbenzene) 91/100 20.41106/40Styrene (Vinyl benzene) 104/100 20.8178/60103/491,1,2,
25、2-Tetrachloroethane 83/100 20.9285/64o-Xylene (1,2-Dimethylbenzene) 91/100 20.92106/404-Ethyltoluene 105/100 22.53120/291,3,5-Trimethylbenzene (Mesitylene) 105/100 22.65120/421,2,4-Trimethylbenzene 105/100 23.18120/42m-Dichlorobenzene (1,3-Dichlorobenzene) 146/100 23.31148/65111/40Benzyl chloride (-
26、Chlorotoluene) 91/100 23.32126/26p-Dichlorobenzene (1,4-Dichlorobenzene) 146/100 23.41148/65111/40o-Dichlorobenzene (1,2-Dichlorobenzene) 146/100 23.88148/65111/401,2,4-Trichlorobenzene 180/100 26.71182/98184/30Hexachlorobutadiene (1,1,2,3,4,4-Hexachloro- 225/100 27.681,3-butadiene) 227/66223/60TABL
27、E 1 Typical Volatile Organic Compounds Determined by the Canister MethodCompound (Synonym) Formula MolecularWeight Boiling Point(C) Melting Point (C) CASNumberFreon 12 (Dichlorodifluoromethane) Cl2CF2 120.91 29.8 158.0Methyl chloride (Chloromethane) CH3Cl 50.49 24.2 97.1 74-87-3Freon 114 (1,2-Dichlo
28、ro-1,1,2,2-tetrafluoroethane) ClCF2CClF2 170.93 4.1 94.0Vinyl chloride (Chloroethylene) CH2=CHCl 62.50 13.4 1538.0 75-01-4Methyl bromide (Bromomethane) CH3Br 94.94 3.6 93.6 74-83-9Ethyl chloride (Chloroethane) CH3CH2Cl 64.52 12.3 136.4 75-00-3Freon 11 (Trichlorofluoromethane) CCl3F 137.38 23.7 111.0
29、Vinylidene chloride (1,1-Dichloroethene) C2H2Cl2 96.95 31.7 122.5 75-35-4Dichloromethane (Methylene chloride) CH2Cl2 84.94 39.8 95.1 75-09-2Freon 113 (1,1,2-Trichloro-1,2,2-trifluoroethane) CF2ClCCl2F 187.38 47.7 36.41,1-Dichloroethane CH3CHCl2 98.96 57.3 97.0 74-34-3cis-1,2-Dichloroethylene CHCl=CH
30、Cl 96.94 60.3 80.5Chloroform (Trichloromethane) CHCl3 119.38 61.7 63.5 67-66-31,2-Dichloroethane (Ethylene dichloride) ClCH2CH2Cl 98.96 83.5 35.3 107-06-2Methyl chloroform (1,1,1,-Trichloroethane) CH3CCl3 133.41 74.1 30.4 71-55-6Benzene C6H6 78.12 80.1 5.5 71-43-2Carbon tetrachloride (Tetrachloromet
31、hane) CCl4 153.82 76.5 23.0 56-23-51,2-Dichloropropane (Propylene dichloride) CH3CHClCH2Cl 112.99 96.4 100.4 78-87-5Trichloroethylene (Trichloroethene) ClCH=CCl2 131.29 87 73.0 79-01-6cis-1,3-Dichloropropene (cis-1,3-dichloropropylene) CH3CC=CHCl 110.97 76trans-1,3-Dichloropropene (trans-1,3-Dichlor
32、opropylene)ClCH2CH=CHCl 110.97 112.01,1,2-Trichloroethane (Vinyl trichloride) CH2ClCHCl2 133.41 113.8 36.5 79-00-5Toluene (Methyl benzene) C6H5CH3 92.15 110.6 95.0 108-88-31,2-Dibromoethane (Ethylene dibromide) BrCH2CH2Br 187.88 131.3 9.8 106-93-4Tetrachloroethylene (Perchloroethylene) Cl2C=CCl2 165
33、.83 121.1 19.0 127-18-4Chlorobenzene C6H5Cl 112.56 132.0 45.6 108-90-7Ethylbenzene C6H5C2H5 106.17 136.2 95.0 100-41-4m-Xylene (1,3-Dimethylbenzene) 1,3-(CH3)2C6H4 106.17 139.1 47.9p-Xylene (1,4-Dimethylxylene) 1,4-(CH3)2C6H4 106.17 138.3 13.3Styrene (Vinyl benzene) C6H5CH=CH2 104.16 145.2 30.6 100-
34、42-51,1,2,2-Tetrachloroethane CHCl2CHCl2 167.85 146.2 36.0 79-34-5o-Xylene (1,2-Dimethylbenzene) 1,2-(CH3)2C6H4 106.17 144.4 25.21,3,5-Trimethylbenzene (Mesitylene) 1,3,5-(CH3)3C6H6 120.20 164.7 44.7 108-67-8D5466 153Compound (Synonym) Formula MolecularWeight Boiling Point(C) Melting Point (C) CASNu
35、mber1,2,4-Trimethylbenzene 1,2,4-(CH3)3C6H6 120.20 169.3 43.8 95-63-6m-Dichlorobenzene (1,3-Dichlorobenzene) 1,3-Cl2C6H4 147.01 173.0 24.7 541-73-1Benzyl chloride (-Chlorotoluene) C6H5CH2Cl 126.59 179.3 39.0 100-44-7o-Dichlorobenzene (1,2-Dichlorobenzene) 1,2-Cl2C6H4 147.01 180.5 17.0 95-50-1p-Dichl
36、orobenzene (1,4-Dichlorobenzene) 1,4-Cl2C6H4 147.01 174.0 53.1 106-46-71,1,2,3,4,4Hexachloro1,3-butadiene Cl6C4 260.76 215 -21.0 7-68-3TABLE 1 Typical Volatile Organic Compounds Determined by the Canister MethodCompound (Synonym) Formula MolecularWeight Boiling Point(C)VaperPressurekPa at 25CListed
37、in theU.S. EPA TO-14A/TO-15CASNumberAcetylenePropyleneFreon 12 (Dichlorodifluoromethane) Cl2CF2 120.91 29.8 X/XMethyl chloride (Chloromethane) CH3Cl 50.49 24.2 X/X 74-87-3Freon 114 (1,2-Dichloro-1,1,2,2-tetrafluoroethane)ClCF2CClF2 170.93 4.1 X/XVinyl chloride (Chloroethylene) CH2=CHCl 62.50 13.4 X/
38、X 75-01-41,3-Butadiene /XMethyl bromide (Bromomethane) CH3Br 94.94 3.6 X/X 74-83-9Ethyl chloride (Chloroethane) CH3CH2Cl 64.52 12.3 X/X 75-00-3Acetonitrile /XFreon 11 (Trichlorofluoromethane) CCl3F 137.38 23.7 X/XAcrylonitrileVinylidene chloride (1,1-Dichloroethene) C2H2Cl2 96.95 31.7 X/X 75-35-4Dic
39、hloromethane (Methylene chloride) CH2Cl2 84.94 39.8 X/X 75-09-2Freon 113 (1,1,2-Trichloro-1,2,2-trifluoroethane)CF2ClCCl2F 187.38 47.7 X/XTrans-1,2-Dichloroethylene /X1,1-Dichloroethane CH3CHCl2 98.96 57.3 X/X 74-34-3Methyl tert-Butyl Ether /X2-Butanone Methyl Ethyl Ketone /XChloroprene /Xcis-1,2-Di
40、chloroethylene CHCl=CHCl 96.94 60.3 X/XBromochloromethane /XChloroform (Trichloromethane) CHCl3 119.38 61.7 X/X 67-66-3Ethyl tert-Butyl Ether X/X1,2-Dichloroethane (Ethylene dichloride) ClCH2CH2Cl 98.96 83.5 X/X 107-06-2Methyl chloroform (1,1,1,-Trichloroethane) CH3CCl3 133.41 74.1 X/X 71-55-6Benzen
41、e C6H6 78.12 80.1 X/X 71-43-2Carbon tetrachloride (Tetrachloromethane) CCl4 153.82 76.5 X/X 56-23-5Tert-Amyl Methyl Ether /X1,2-Dichloropropane (Propylene dichloride) CH3CHClCH2Cl 112.99 96.4 X/X 78-87-5Ethyl Acrylate /XTrichloroethylene (Trichloroethene) ClCH=CCl2 131.29 87 X/X 79-01-6Methyl Methac
42、rylate X/Xcis-1,3-Dichloropropene (cis-1,3-dichloropropylene)CH3CC=CHCl 110.97 76 X/XMethyl Methacrylate /Xtrans-1,3-Dichloropropene (trans-1,3-Dichloropropylene)ClCH2CH=CHCl 110.97 112.0 X/X1,1,2-Trichloroethane (Vinyl trichloride) CH2ClCHCl2 133.41 113.8 X/X 79-00-5Toluene (Methyl benzene) C6H5CH3
43、 92.15 110.6 X/X 108-88-3Dibromochloromethane /X1,2-Dibromoethane (Ethylene dibromide) BrCH2CH2Br 187.88 131.3 X/X 106-93-4n-Octane X/XTetrachloroethylene (Perchloroethylene) Cl2C=CCl2 165.83 121.1 X/X 127-18-4Chlorobenzene C6H5Cl 112.56 132.0 X/X 108-90-7Ethylbenzene C6H5C2H5 106.17 136.2 X/X 100-4
44、1-4m-Xylene (1,3-Dimethylbenzene) 1,3-(CH3)2C6H4 106.17 139.1 X/Xp-Xylene (1,4-Dimethylxylene) 1,4-(CH3)2C6H4 106.17 138.3 X/XStyrene (Vinyl benzene) C6H5CH=CH2 104.16 145.2 X/X 100-42-51,1,2,2-Tetrachloroethane CHCl2CHCl2 167.85 146.2 X/X 79-34-5o-Xylene (1,2-Dimethylbenzene) 1,2-(CH3)2C6H4 106.17
45、144.4 X/X4-Ethyltoluene C9H12 120.19 162 3 mm Hg X 6229681,3,5-Trimethylbenzene (Mesitylene) 1,3,5-(CH3)3C6H6 120.20 164.7 X/X 108-67-81,2,4-Trimethylbenzene 1,2,4-(CH3)3C6H6 120.20 169.3 X/X 95-63-6m-Dichlorobenzene (1,3-Dichlorobenzene) 1,3-Cl2C6H4 147.01 173.0 X/X 541-73-1Chloromethylbenzene /XBe
46、nzyl chloride (-Chlorotoluene) C6H5CH2Cl 126.59 179.3 X 100-44-7o-Dichlorobenzene (1,2-Dichlorobenzene) 1,2-Cl2C6H4 147.01 180.5 X/X 95-50-1p-Dichlorobenzene (1,4-Dichlorobenzene) 1,4-Cl2C6H4 147.01 174.0 X/X 106-46-71,1,2,3,4,4Hexachloro1,3-butadiene Cl6C4 260.76 215 X 7-68-31,2,4 - Trichlorbenzene
47、 /XD5466 1542.2 OtherEPA Documents:5U.S. Environmental Protection Agency, Compendium of Methods for the Determination to Toxic Organic Compounds inAmbient Air, Method TO-14A, EPA 600/R-96/010b Compendium of Methods for the Determination to Toxic OrganicCompounds in Ambient Air, Method TO-14AEPA 625/
48、R-96/010b Compendium of Methods for the Determination to Toxic Organic Compounds in Ambient Air, SecondEdition, Compendium Method TO-153. Terminology3.1 DefinitionsFor definitions of terms used in this test method, standard, refer to Terminology D1356. Other pertinentabbreviations and symbols are de
49、fined within this practice at point of use.3.2 Definitions of Terms Specific to This Standard:3.2.1 absolute canister pressurepressure, nPg + Pa, where Pg = gage = gauge pressure in the canister. (kPa, psi) canister;(kPa) and Pa = barometric pressure.3.2.2 absolute pressurepressure, npressure measured with reference to absolute zero pressure (as opposed to atmosphericpressure), usually expressed as kPa, mm Hg, or psia.kPa.3.2.3 certificationthe process of demonstrating with humid zero air and humid calibration gases
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