ASTM E1413-00

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Designation:E1413–00
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 Residues in Extracts from Samples of Fire Debris by Gas
Chromatography
1.1 This practice describes the procedure for separation of
E 1388 Practice for Sampling of Headspace Vapors from
small quantities of ignitable liquid residues from fire debris
Fire Debris Samples
samples using the absorption/elution method of headspace
E 1412 Practice for Separation and Concentration of Flam-
concentration.
mable and Combustible Liquid Residues from Fire Debris
1.2 Both positive and negative pressure systems are de-
Samples by Passive Headspace Concentration
scribed.
E 1459 Guide for Physical Evidence Labeling and Related
1.3 Whilethispracticeissuitableforsuccessfullyextracting
Documentation
ignitable liquid residues over the entire range of concentration,
E 1492 Practice for Receiving, Documenting, Storing, and
theheadspaceconcentrationmethodsarebestusedwhenahigh
Retrieving Evidence in a Forensic Science Laboratory
level of sensitivity is required due to a very low concentration
E 1618 Guide for Ignitable Liquid Residues in Extracts
of ignitable liquid residues in the sample.
from Fire Debris Samples by Gas Chromatography-Mass
1.4 Alternate separation and concentration procedures are
Spectrometry
listed in Section 2.
1.5 This standard does not purport to address all of the
3. Summary of Practice
safety concerns, if any, associated with its use. It is the
3.1 The sample, preferably in its original container, is
responsibility of the user of this standard to establish appro-
heated, forcing volatile compounds to vaporize. At the same
priate safety and health practices and determine the applica-
time, the headspace in the sample is drawn or pushed through
bility of regulatory limitations prior to use.
a tube containing activated charcoal which adsorbs the vapor-
2. Referenced Documents ized compounds.
2.1 ASTM Standards:
4. Significance and Use
D 1193 Specification for Reagent Water
4.1 This practice is useful for preparing extracts from fire
E 752 PracticeforSafetyandHealthRequirementsRelating
3 debris for later analysis by gas chromatography, GC/MS, or
to Occupational Exposure to Carbon Disulfide
GC/IR.
E 1385 Practice for Separation and Concentration of Ignit-
4.2 This is a very sensitive separation procedure, capable of
able Liquid Residues from Fire Debris Samples by Steam
4 isolating quantities smaller than ⁄10 µL of ignitable liquid
Distillation
residue from a sample.
E 1386 Practice for Separation and Concentration of Flam-
4.2.1 Actual recovery will vary, depending on several fac-
mable or Combustible Liquid Residues from Fire Debris
4 tors, including adsorption temperature, container size, and
Samples by Solvent Extraction
competition from the sample matrix.
E 1387 Test Method for Flammable or Combustible Liquid
4.3 “This is a potentially destructive technique.” Portions of
the sample subjected to this procedure may not be suitable for
1 re-sampling. Therefore, a portion of the sample extract should
This practice is under the jurisdiction of ASTM Committee E-30 on Forensic
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics. be saved for potential future analysis. Consider using passive
Current edition approved Nov. 10, 2000. Published January 2001. Originally
headspace concentration as described in Practice E 1412.
published as E 1413 – 91. Last previous edition E 1413 – 00.
Annual Book of ASTM Standards, Vol 11.01.
5. Apparatus
Discontinued. See 1995 Annual Book of ASTM Standards, Vol 11.03.
Annual Book of ASTM Standards, Vol 14.02. 5.1 Positive Pressure Apparatus:
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E1413
5.1.1 Sample Pressurization Device—A system capable of provided it is first ascertained that the reagent is of sufficiently
delivering pressurized dry nitrogen (or other inert gas) at up to high purity to permit its use without lessening the accuracy of
40 psi (276 kPa) to an orifice to be inserted into the bottom of the determination.
the sample container. 6.1.1 Purity of Water—Unless otherwise indicated, refer-
ences to water shall be understood to mean reagent water as
5.1.1.1 A needle valve capable of fine control of the flow
rate of the dry nitrogen, at up to 1500 cc/min. defined by Type IV of Specification D 1193.
6.2 Activated Charcoal (coconut).
5.1.1.2 A flow meter capable of measuring the flow of dry
6.2.1 Test each new batch of charcoal for residual hydro-
nitrogen through the end of the charcoal adsorption tube at the
carbons by analyzing a concentrated CS extract of a blank
rate of 0 to 1500 cc/min. 2
adsorption tube.
5.1.1.3 Container Closure—A device suitable for sealing
6.3 Glass Wool, or cotton, free of extractable hydrocarbons.
the container and directing the effluent nitrogen and vapors to
6.4 Carbon Disulfide, GC grade.
the charcoal tube.
6.4.1 Read and follow the safety precautions described in
5.2 Negative Pressure Apparatus:
Practice E 752.
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
7. Sample Preparation
sleeve stopper. This serves as a filter for incoming room air. A
7.1 Observe the appropriate procedures for handling and
vacuum is pulled on an adsorption tube also fitted into the lid
documentation of all submitted samples.
of the original container with a sleeve stopper.
7.1.1 Open and examine the fire debris sample in order to
5.2.2 Avacuum system capable of pulling between 200 and
determine that it is consistent with its description.
1500 cc/min on the sample collection tube.
7.1.1.1 Resolve any discrepancies between the submitting
5.2.3 A flow meter capable of measuring the flow of air
agent’s description of the evidence and the analyst’s observa-
through the end of the charcoal tube at the rate of 200 to 1500
tion with the submitting agent prior to the completion of the
cc/min.
report.
5.3 Adsorption Tubes—Suitable absorption tubes may be
7.2 Place the sample in an appropriate, clean sampling
made by inserting a small (approximately 1 cm) plug of glass
container, which is designed to be flushed by positive or
wool or cotton in the bottom of a Pasteur pipette (approxi-
negative pressure.
mately 5 mm diameter), then adding approximately 5 cm of
7.2.1 Ideally, the system will be designed so that the
activated charcoal, and finally, holding the charcoal in place
majority of samples can be extracted directly from the con-
with an additional 1 cm of glass wool or cotton.
...