ASTM E1413-00(2005)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:E1413–00 (Reapproved 2005)
Standard Practice for
Separation and Concentration of Ignitable Liquid Residues
from Fire Debris Samples by Dynamic Headspace
Concentration
This standard is issued under the fixed designation E 1413; 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 time, the headspace in the sample is drawn or pushed through
a tube containing activated charcoal which adsorbs the vapor-
1.1 This practice describes the procedure for separation of
ized compounds.
small quantities of ignitable liquid residues from fire debris
samples using the absorption/elution method of headspace
4. Significance and Use
concentration.
4.1 This practice is useful for preparing extracts from fire
1.2 Both positive and negative pressure systems are de-
debris for later analysis by gas chromatography, GC/MS, or
scribed.
GC/IR.
1.3 While this practice is suitable for successfully extracting
4.2 This is a very sensitive separation procedure, capable of
ignitable liquid residues over the entire range of concentration,
isolating quantities smaller than ⁄10 µL of ignitable liquid
theheadspaceconcentrationmethodsarebestusedwhenahigh
residue from a sample.
level of sensitivity is required due to a very low concentration
4.2.1 Actual recovery will vary, depending on several fac-
of ignitable liquid residues in the sample.
tors, including adsorption temperature, container size, and
1.4 Alternate separation and concentration procedures are
competition from the sample matrix.
listed in Section 2.
4.3 “This is a potentially destructive technique.” Portions of
1.5 This standard does not purport to address all of the
the sample subjected to this procedure may not be suitable for
safety concerns, if any, associated with its use. It is the
re-sampling. Therefore, a portion of the sample extract should
responsibility of the user of this standard to establish appro-
be saved for potential future analysis. Consider using passive
priate safety and health practices and determine the applica-
headspace concentration as described in Practice E 1412.
bility of regulatory limitations prior to use.
5. Apparatus
2. Referenced Documents
5.1 Positive Pressure Apparatus:
2.1 ASTM Standards:
5.1.1 Sample Pressurization Device—A system capable of
D 1193 Specification for Reagent Water
delivering pressurized dry nitrogen (or other inert gas) at up to
E 752 PracticeforSafetyandHealthRequirementsRelating
40 psi (276 kPa) to an orifice to be inserted into the bottom of
to Occupational Exposure to Carbon Disulfide
the sample container.
E 1387 Test Method for Flammable or Combustible Liquid
5.1.1.1 A needle valve capable of fine control of the flow
Residues in Extracts from Samples of Fire Debris by Gas
rate of the dry nitrogen, at up to 1500 cc/min.
Chromatography
5.1.1.2 A flow meter capable of measuring the flow of dry
E 1412 Practice for Separation and Concentration of Flam-
nitrogen through the end of the charcoal adsorption tube at the
mable and Combustible Liquid Residues from Fire Debris
rate of 0 to 1500 cc/min.
Samples by Passive Headspace Concentration
5.1.1.3 Container Closure—A device suitable for sealing
3. Summary of Practice the container and directing the effluent nitrogen and vapors to
the charcoal tube.
3.1 The sample, preferably in its original container, is
5.2 Negative Pressure Apparatus:
heated, forcing volatile compounds to vaporize. At the same
5.2.1 Inlet and outlet system—A tube containing 1 cm of
charcoal is fitted into the lid of the original container with a
This practice is under the jurisdiction of ASTM Committee E30 on Forensic
sleeve stopper. This serves as a filter for incoming room air. A
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics.
vacuum is pulled on an adsorption tube also fitted into the lid
Current edition approved May 1, 2005. Published September 2005. Originally
of the original container with a sleeve stopper.
approved in 1991. Last previous edition approved in 2000 as E 1413 – 00.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E1413–00 (2005)
5.2.2 Avacuum system capable of pulling between 200 and 7.1.1.1 Resolve any discrepancies between the submitting
1500 cc/min on the sample collection tube. agent’s description of the evidence and the analyst’s observa-
5.2.3 A flow meter capable of measuring the flow of air tion with the submitting agent prior to the completion of the
through the end of the charcoal tube at the rate of 200 to 1500 report.
cc/min.
7.2 Place the sample in an appropriate, clean sampling
5.3 Adsorption Tubes—Suitable absorption tubes may be container, which is designed to be flushed by positive or
made by inserting a small (approximately 1 cm) plug of glass
negative pressure.
wool or cotton in the bottom of a Pasteur pipette (approxi- 7.2.1 Ideally, the system will be designed so that the
mately 5 mm diameter), then adding approximately 5 cm of
majority of samples can be extracted directly from the con-
activated charcoal, and finally, holding the charcoal in place tainer in which they are delivered to the laboratory.
with an additional 1 cm of glass wool or cotton.
5.3.1 Alternatively, charcoal tubes are available from com-
8. Adsorption Procedure
mercial sources.
8.1 Positive Pressure:
5.3.2 The use of a different adsorbing media such as Tenax
8.1.1 Place the sample container in the heating system and
is possible, but this results in complications in the desorbing
connect to the nitrogen source which will introduce nitrogen
phase because certain solvents cause the dissolution of the
into the bottom of the container, and to the exhaust line
Tenax. Tenax is best employed when desorption is to be
connected to the charcoal adsorbing tube.
performed using a thermal operation.
8.1.1.1 Direct connection of the charcoal tube to the sample
5.4 Heating System—A heating mantel designed to fit the
container is possible, unless an oven is used. Placement of the
evidence container or an oven or a hot plate.
charcoal tube outside the oven requires the use of an interven-
5.4.1 An oven may be set up with any number of stations to
ing line which must be carefully cleaned between uses to
allow for multiple sample preparation.
remove any adsorbed or condensed residues.
5.5 Temperature Measuring Device—A thermometer or
8.1.2 Pressurization—Deliver nitrogen to the sample
thermocoupl
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