ASTM E1388-2012 Standard Practice for Sampling of Headspace Vapors from Fire Debris Samples 《从火烧瓦砾样品中进行液上蒸气取样的标准操作规程》.pdf

1、Designation: E1388 12Standard Practice forSampling of Headspace Vapors from Fire Debris Samples1This standard is issued under the fixed designation E1388; 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 practice describes the procedure for removingsmall quantities of ignitable liquid vapor from samples of firedebris by sampling th

3、e headspace of the debris container.1.2 Separation and concentration procedures are listed in thereferenced documents. (See Practices E1386, E1412, E1413,and E2154.)1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of th

4、e 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:2E1386 Practice for Separation of Ignitable Liquid Residuesfrom Fire Debris Samples by Solvent ExtractionE14

5、12 Practice for Separation of Ignitable Liquid Residuesfrom Fire Debris Samples by Passive Headspace Concen-tration With Activated CharcoalE1413 Practice for Separation and Concentration of Ignit-able Liquid Residues from Fire Debris Samples by Dy-namic Headspace ConcentrationE1459 Guide for Physica

6、l Evidence Labeling and RelatedDocumentationE1492 Practice for Receiving, Documenting, Storing, andRetrieving Evidence in a Forensic Science LaboratoryE1618 Test Method for Ignitable Liquid Residues in Ex-tracts from Fire Debris Samples by Gas Chromatography-Mass SpectrometryE2154 Practice for Separ

7、ation and Concentration of Ignit-able Liquid Residues from Fire Debris Samples by PassiveHeadspace Concentration with Solid Phase Microextrac-tion (SPME)3. Summary of Practice3.1 The sample, preferably in its original container, isheated in order to volatilize any ignitable liquid residuespresent in

8、 the debris. After heating, the headspace is sampledand analyzed by gas chromatography-mass spectrometry.4. Significance and Use4.1 This procedure is particularly useful for screening firedebris samples to determine relative ignitable liquid concen-trations and possible ignitable liquid class prior

9、to extractionwith other techniques.4.2 This practice is useful when volatile oxygenated prod-ucts such as alcohols or lacquer thinners are suspected.4.3 This practice is the least sensitive of the sample prepa-ration techniques and may not detect quantities of less than 10L of an ignitable liquid.4.

10、4 Because this separation takes place in a closed con-tainer, the sample remains in approximately the same conditionin which it was submitted. Repeat and interlaboratory analysesare therefore possible.4.5 Due to variables in the debris sample condition prior toheadspace sampling, complete reproducib

11、ility of chromato-grams may be difficult to obtain.4.5.1 To obtain greater reproducibility, use one of theseparation procedures which results in a solution of theignitable liquid residue (see Practices E1386, E1412, andE1413).4.5.2 To obtain greater sensitivity for petroleum distillatesand oxygenate

12、d products, use solid phase microextraction. (SeePractice E2154.)4.6 High concentrations of highly volatile compounds mayswamp the headspace, inhibiting the recovery of less volatilecomponents.5. Apparatus5.1 Heating SystemAn oven, heating mantle or hot platedesigned to fit the evidence container.5.

13、2 Temperature Measuring DeviceA thermometer orthermocouple capable of measuring temperatures in the rangefrom 40 to 150C.5.3 A gas-tight syringe capable of reproducibility introduc-ing sample sizes in the range from 0.5 to 5 mL.5.4 Disposable 20 cc syringes.1This practice in under the jurisdiction o

14、f ASTM Committee E30 on ForensicSciences and is the direct responsibility of Subcommittee E30.01 on CriminalisticsCurrent edition approved Feb. 1, 2012. Published March 2012. Originallyapproved in 1990. Last previous edition approved in 2005 as E1388 05. DOI:10.1520/E1388-12.2For referenced ASTM sta

15、ndards, 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 Conshohocken,

16、 PA 19428-2959, United States.5.5 Disposable 1620 gauge syringe needles.5.6 A drill, punch, or other device to puncture holes insample containers.5.7 Headspace sample vials.6. Sample Preparation6.1 Observe the appropriate procedures for handling anddocumentation of all submitted samples as described

17、 in GuideE1459 and Practice E1492.6.1.1 Open and examine the fire debris sample in order todetermine that it is consistent with its description.6.1.1.1 Resolve any discrepancies between the submittingagencys description of the evidence and the analysts obser-vation prior to the completion of the rep

18、ort.6.2 Punch or drill a small hole in the container lid and coverthe hole with tape.6.2.1 Alternatively, a rubber sleeve stopper may be placedin the hole.6.3 If the sample is going to be heated, place the containerin the heating system until the container reaches the desiredtemperature (not to exce

19、ed 90C).6.4 The syringe may be heated prior to sampling7. Sampling Procedure7.1 Direct Headspace Sampling:7.1.1 Remove the container from the heating apparatus thenpush the syringe through the tape or rubber sleeve stopper intothe hole in the container lid. Slowly pump the syringe severaltimes, with

20、draw from the lid, and inject 0.5 to 2.0 mL ofsample into the gas chromatograph. Analyze as described inTest Method E1618.7.1.2 After the headspace sample has been removed, resealthe hole.7.2 Indirect Headspace Sampling Using Headspace SampleVials:7.2.1 Some automated sample injection systems utiliz

21、eheadspace sample vials for delivery of the sample headspaceinto the gas chromatograph.7.2.2 Assemble and seal (crimp or screw) lid onto head-space sample vial. Using a 20 cc syringe and needle, puncturethe headspace vial septum and evacuate the contents of thevial. Repeat this procedure 3 to 4 time

22、s.7.2.3 Remove the container from the heating apparatus thenpush the 20 cc syringe through the tape or rubber sleevestopper into the hole in the container lid. Slowly pump thesyringe several times, withdraw 20 cc of vapor and inject intoheadspace sample vial. Repeat this process 2 to 4 times.7.2.3.1

23、 If the headspace sample vial was properly sealed andevacuated, the vacuum created should pull the initial injectioninto the vial. The latter injections into the vial will requireforcibly injecting the 20 cc sample.7.2.3.2 The sequence method on the gas chromatographshould be setup to inject 0.5 to

24、2.0 mL of the sample into thegas chromatograph. Analyze as described in Test MethodE1618.7.2.4 After the headspace samples have been removed,reseal the hole in the container.8. Keywords8.1 fire debris samples; headspaceASTM International takes no position respecting the validity of any patent rights

25、 asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any ti

26、me by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will

27、receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM

28、International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).E1388 122