ASTM E2154-01
(Practice)Standard Practice for Separation and Concentration of Ignitable Liquid Residues from Fire Debris Samples by Passive Headspace Concentration with Solid Phase Microextraction (SPME)
Standard Practice for Separation and Concentration of Ignitable Liquid Residues from Fire Debris Samples by Passive Headspace Concentration with Solid Phase Microextraction (SPME)
SIGNIFICANCE AND USE
This practice is suited ideally for screening samples for the presence, relative concentration, and potential class of ignitable liquid residues in fire debris.
This is a very sensitive separation procedure, capable of isolating small quantities of ignitable liquid residues from a sample, that is, a 0.1 μL spike of gasoline on a cellulose wipe inside of a 1-gal can is detectable.
Actual recovery will vary, depending on several factors, including adsorption temperature, container size, competition from the sample matrix, ignitable liquid class and relative ignitable liquid concentration.
Because this separation takes place in a closed container, the sample remains in approximately the same condition in which it was submitted. Repeat and interlaboratory analyses, therefore, may be possible. Since the extraction is nonexhaustive, the technique permits reanalysis of samples.
This practice is intended for use in conjunction with other extraction techniques described in Practices E 1385, E 1386, E 1388, E 1412, and E 1413.
The extract is consumed in the analysis. If a more permanent extract is desired, one of the separation practices described in Practices E 1385, E 1386, E 1412, or E 1413 should be used.
SCOPE
1.1 This practice describes the procedure for removing small quantities of ignitable liquid residues from samples of fire debris. An adsorbent material is used to extract the residue from the static headspace above the sample. Then, analytes are thermally desorbed in the injection port of the gas chromatograph (GC).
1.2 This practice is best suited for screening fire debris samples to assess relative ignitable liquid concentration and for extracting ignitable liquid from aqueous samples.
1.3 This practice is suitable for extracting ignitable liquid residues when a high level of sensitivity is required due to a very low concentration of ignitable liquid residues in the sample.
1.3.1 Unlike other methods of separation and concentration, this method recovers a minimal amount of the ignitable residues present in the evidence, leaving residues that are suitable for subsequent resampling.
1.4 Alternate separation and concentration procedures are listed in Section 2.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation:E2154–01
Standard Practice for
Separation and Concentration of Ignitable Liquid Residues
from Fire Debris Samples by Passive Headspace
Concentration with Solid Phase Microextraction (SPME)
This standard is issued under the fixed designation E 2154; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope E 1387 Test Method for Flammable or Combustible Liquid
Residues in Extracts from Samples of Fire Debris by Gas
1.1 This practice describes the procedure for removing
Chromatography
small quantities of ignitable liquid residues from samples of
E 1388 Practice for Sampling Headspace Vapors from Fire
fire debris.An adsorbent material is used to extract the residue
Debris Samples
from the static headspace above the sample. Then, analytes are
E 1412 Practice for Separation and Concentration of Flam-
thermally desorbed in the injection port of the gas chromato-
mable or Combustible Liquid Residues from Fire Debris
graph (GC).
Samples by Passive Headspace Concentration with Acti-
1.2 This practice is best suited for screening fire debris
vated Charcoal
samplestoassessrelativeignitableliquidconcentrationandfor
E 1413 Practice for Separation and Concentration of Flam-
extracting ignitable liquid from aqueous samples.
mable or Combustible Liquid Residues from Fire Debris
1.3 This practice is suitable for extracting ignitable liquid
Samples by Dynamic Headspace Concentration
residues when a high level of sensitivity is required due to a
E 1459 Guide for Physical Evidence Labeling and Related
very low concentration of ignitable liquid residues in the
Documentation
sample.
E 1492 Practice for Receiving, Documenting, Storing, and
1.3.1 Unlike other methods of separation and concentration,
Retrieving Evidence in a Forensic Science Laboratory
this method recovers a minimal amount of the ignitable
E 1618 Guide for Ignitable Liquid Residues in Extracts
residues present in the evidence, leaving residues that are
from Fire Debris Samples by Gas Chromatography-Mass
suitable for subsequent resampling.
Spectrometry
1.4 Alternate separation and concentration procedures are
listed in Section 2.
3. Summary of Practice
1.5 This standard does not purport to address all of the
3.1 A fiber coated with a polydimethylsiloxane stationary
safety concerns, if any, associated with its use. It is the
phase is exposed to the headspace of the fire debris sample
responsibility of the user of this standard to establish appro-
container to extract ignitable liquid residues. The fiber, which
priate safety and health practices and determine the applica-
is housed in a needle similar to a syringe needle, is introduced
bility of regulatory limitations prior to use.
directly in the injection port of a gas chromatograph to
2. Referenced Documents thermally desorb the analytes.
2.1 ASTM Standards:
4. Significance and Use
E 1385 Practice for Separation and Concentration of Flam-
4.1 This practice is suited ideally for screening samples for
mable or Combustible Liquid Residues from Fire Debris
2 the presence, relative concentration, and potential class of
Samples by Steam Distillation
ignitable liquid residues in fire debris.
E 1386 Practice for Separation and Concentration of Flam-
4.2 This is a very sensitive separation procedure, capable of
mable or Combustible Liquid Residues from Fire Debris
isolating small quantities of ignitable liquid residues from a
Samples by Solvent Extraction
sample, that is, a 0.1 µL spike of gasoline on a cellulose wipe
inside of a 1-gal can is detectable.
4.3 Actual recovery will vary, depending on several factors,
This practice is under the jurisdiction of ASTM Committee E30 on Forensic
including adsorption temperature, container size, competition
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics.
from the sample matrix, ignitable liquid class and relative
Current edition approved Sept 10, 2001. Published December 2001.
Annual Book of ASTM Standards, Vol 14.02. ignitable liquid concentration.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E2154
4.4 Because this separation takes place in a closed con- 6.4.2 Temperatures above 80°C may result in a significant
tainer,thesampleremains in approximately the samecondition discrimination against high volatility compounds when the 100
inwhichitwassubmitted.Repeatandinterlaboratoryanalyses, µm PDMS fiber is used.
therefore, may be possible. Since the extraction is nonexhaus- 6.5 Remove the container from the heating apparatus.
tive, the technique permits reanalysis of samples.
6.6 Immediately puncture the rubber sleeve septum or
4.5 This practice is intended for use in conjunction with plastic evidence bag with the needle of the SPME apparatus.
other extraction techniques described in Practices E 1385,
6.7 ExposetheSPMEfibertotheheadspaceofthecontainer
E 1386, E 1388, E 1412, and E 1413. for the desired sampling duration.
4.6 The extract is consumed in the analysis. If a more
6.7.1 The optimum exposure time for maximum sensitivity
permanent extract is desired, one of the separation practices will depend on the temperature and the concentration and
described in Practices E 1385, E 1386, E 1412, or E 1413
composition of the volatile compound present in the sample
should be used. headspace.
6.7.2 Exposure times for routine screening of samples
5. Apparatus
typically are in the range of 5-15 min.
5.1 HeatingSystem,suchas,anovenorheatingmantletofit
6.7.3 Residue extracts that provide off-scale or poorly
the evidence container (or a hot plate)
...
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