ASTM E1413-19

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. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E1413 − 13 E1413 − 19
Standard Practice for
Separation of Ignitable Liquid Residues from Fire Debris
Samples by Dynamic Headspace Concentration onto an
Adsorbent Tube
This standard is issued under the fixed designation E1413; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This practice describes the procedure for separation of small quantities of ignitable liquid residues from fire debris samples
using the method of dynamic headspace concentration.dynamic headspace concentration onto an adsorbent tube, with subsequent
solvent elution or thermal desorption.
1.2 Dynamic headspace concentration uses adsorption and subsequent solvent elution or thermal desorption.onto an adsorbent
tube takes place from a closed, rigid sample container (typically a metal can), using a source of dry inert gas or a vacuum system.
1.3 Both positive and negative applied pressure systems for adsorption are described, as well as a thermal desorption
system.dynamic headspace concentration onto an adsorbent tube are illustrated and described.
1.4 While this This practice is suitable for successfully extracting ignitable liquid residues over the entire range of
concentration, the headspace concentration methods are best used when a high level of sensitivity is required due to a very low
concentration preparing extracts from fire debris samples containing a range of volumes (μL to mL) of ignitable liquid residues
in the sample.residues, with sufficient recovery for subsequent qualitative analysis (1).
1.5 Alternate separation and concentration proceduresAlternative headspace concentration methods are listed in Section 2. If
archival of the extract is of importance, then this practice’s thermal desorption procedure, SPME (Practice (see Practices E2154),
and headspace (Practice E1388), E1412sample, E3189separation techniques are not recommended unless a portion of the extract
can be split and retained. In order to have an archivable extract, then this practice’s sample collection on charcoal, solvent
extraction (Practice , and E1386E2154), or passive headspace concentration (Practice ).E1412) is recommended.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 This practice offers a set of instructions for performing one or more specific operations. This standard cannot replace
knowledge, skill,skills, or abilityabilities acquired through appropriate education, training, and experience (Practice E2917) and
should is to be used in conjunction with sound professional judgment.professional judgment by individuals with such
discipline-specific knowledge, skills, and abilities.
1.8 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.9 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
E1386 Practice for Separation of Ignitable Liquid Residues from Fire Debris Samples by Solvent Extraction
E1388 Practice for Static Headspace Sampling of Vapors from Fire Debris Samples
This practice is under the jurisdiction of ASTM Committee E30 on Forensic Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics.
Current edition approved Aug. 15, 2013June 1, 2019. Published September 2013June 2019. Originally approved in 1991. Last previous edition approved in 20072013 as
E1413 – 07.E1413 – 13. DOI: 10.1520/E1413-13.10.1520/E1413-19.
The boldface numbers in parentheses refer to a list of references at the end of this standard.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1413 − 19
E1412 Practice for Separation of Ignitable Liquid Residues from Fire Debris Samples by Passive Headspace Concentration With
Activated Charcoal
E1459 Guide for Physical Evidence Labeling and Related Documentation
E1492 Practice for Receiving, Documenting, Storing, and Retrieving Evidence in a Forensic Science Laboratory
E1618 Test Method for Ignitable Liquid Residues in Extracts from Fire Debris Samples by Gas Chromatography-Mass
Spectrometry
E1732 Terminology Relating to Forensic Science
E2154 Practice for Separation and Concentration of Ignitable Liquid Residues from Fire Debris Samples by Passive Headspace
Concentration with Solid Phase Microextraction (SPME)
E2451 Practice for Preserving Ignitable Liquids and Ignitable Liquid Residue Extracts from Fire Debris Samples
E2917 Practice for Forensic Science Practitioner Training, Continuing Education, and Professional Development Programs
E3189 Practice for Separation of Ignitable Liquid Residues from Fire Debris Samples by Static Headspace Concentration onto
an Adsorbent Tube
3. Terminology
3.1 Definitions—For definitions of terms used in this practice, refer to Terminology E1732.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 dynamic headspace concentration, n—an extraction technique in which a portion of the headspace vapors is exchanged
from the sample container and concentrated onto an adsorbent medium through applied positive or negative pressure.
3.2.2 static headspace concentration, n—an extraction technique in which a portion of the headspace vapors is removed from
the sample container and concentrated onto an adsorbent medium.
4. Summary of Practice
4.1 The sample, preferably in its original container, is heated, forcing volatile compounds to vaporize. The headspace in the
sample is then drawn or pushed through a tube containing an adsorption media (typically activated charcoal or Tenax) which
adsorbs the vaporized compounds. Headspace vapors from the closed sample container are collected and concentrated onto an
adsorbent tube by means of headspace exchange performed through the use of a system based on either positive or negative applied
pressure. The adsorbent tube is subsequently eluted with solvent or desorbed thermally prior to instrumental analysis (typically by
gas chromatography-mass spectrometry (GC-MS)).
4.2 Other solid adsorbents The technique of dynamic headspace concentration onto an adsorbent tube is illustrated in Fig. 1and
collection systems can be used as long as the. The sample container, and the adsorbent tube when necessary, can be heated during
sampling, as outlined in Section 9method has been validated with a wide variety of ignitable liquids with a range of both flash
points and polarity.
5. Significance and Use
5.1 This practice is useful for preparing extracts from fire debris for later subsequent qualitative analysis by gas
chromatography-mass spectrometry (GC-MS),chromatography mass spectrometry, see Test Method E1618.
5.2 This is a very sensitive separation procedure, capable of isolating quantities smaller than The sensitivity of this practice is
such that a sample consisting of a laboratory tissue onto which as little as 0.1 μL of ignitable liquid residue from a samplehas been
deposited, in an otherwise empty sample container, will result in an extract that is sufficient for identification and classification
using Test Method E1618 (1).
Left: Positive applied pressure apparatus. Right: Negative applied pressure apparatus.
FIG. 1 Illustration of Dynamic Headspace Concentration onto an Adsorbent Tube
E1413 − 19
5.2.1 Actual recovery Recovery from fire debris samples will vary, depending on several factors, factors including
adsorptiondebris temperature, container size, and adsorbent temperature, container size, adsorptive material, headspace volume,
sampling time and flow rate, and adsorptive competition from the sample matrix.matrix (2).
5.3 This is a potentially destructive technique. Portions of the sample subjected to this procedure may not be suitable for
re-sampling. Therefore, a portion of the sample extract shouldThe principal concepts of dynamic headspace concentration are
similar to those of static headspace concentration (Practice E3189be saved for potential future analysis. Consider using passive
headspace concentration as described in Practice). The dynamic headspace concentration technique can be more sensitive than the
static headspace concentration technique. However, sample containers E1412.subjected to dynamic headspace concentration could
be unsuitable for re-sampling.
5.3.1 Dynamic headspace concentration alters the original composition of the test sample because a portion of the original
headspace from the sample container is removed and exchanged with dry inert gas or air. A portion of the concentrated headspace
sample should be preserved for potential future analysis, if possible and if required, in accordance with Practice E2451.
5.4 Common solid adsorbent/desorption procedure combinations in use are activated carbon/solvent elution, and Tenax
TA/thermal desorption.
5.5 Solid adsorbent/desorption procedure combinations not specifically described in this standard can be used as long as the
practice has been validated as outlined in Section 11.
6. Apparatus
6.1 Positive Pressure Apparatus: Applied Pressure-Based Sampling System—A system capable of increasing the pressure inside
the sample container by applying dry inert gas at the sample container inlet, thereby pushing the headspace vapors toward and
through the outlet.
6.1.1 Sample Pressurization Device—A system capable of delivering pressurized dry nitrogen (or other inert gas)inert gas at up
to 40 psi (276 kPa) to an orifice to be inserted into the bottom of the sample container.approximately 276 kPa (40 psi) to the inlet.
6.1.1.1 A needle valve capable of fine control of the flow rate of the dry nitrogen, inert gas, at up to 1500 cc/min.approximately
400 mL/min.
5.1.1.2 A flow meter capable of measuring the flow of dry nitrogen through the end of the adsorption tube at the rate of 0 to
1500 cc/min.
5.1.1.3 Container Closure—A device suitable for sealing the container and directing the effluent nitrogen (or other inert gas) and
vapors to the adsorption tube.
6.1.2 A filtering tube, consisting of an adsorbent tube as described in 7.5, attached to the sample container inlet, for the purpose
of filtering incoming dry inert gas.
6.1.3 A flow meter capable of measuring the flow of the dry inert gas through the end of the adsorption tube at the rate of
approximately 40 to 400 mL/min.
6.1.4 Design and use the sampling system in a manner that prevents the loss of volatile compounds from the container and
contamination of the sample from the apparatus itself or the laboratory environment.
6.2 Negative Pressure Apparatus: Applied Pressure-Based Sampling System—
5.2.1 Inlet and Outlet System—A tube containing approximately 1 cm of charcoal is fitted into the lid of the original container
with a suitable penetrable seal. This serves as a filter for incoming room air. A vacuum is pulled on an adsorption tube also fitted
into the lid of the original container with a suitable penetrable seal.A system capable of creating partial vacuum inside the sample
container by connecting a vacuum system to the outlet, thereby pulling the headspace vapors toward and through the outlet.
6.2.1 A vacuum system capable of pulling between 200 and 1500 cc/min on the sample collection tube.approximately 40 and
400 mL/min at the outlet.
6.2.2 A filtering tube, consisting of an adsorbent tube as described in 7.5, attached to the sample container inlet, for the purpose
of filtering incoming air.
6.2.3 A flow meter capable of measuring the flow of air through the end of the charcoal tube filtered air and headspace vapors
through the outlet at the rate of 200 to 1500 cc/min.approximately 40 to 400 mL/min.
6.2.4 Design and use the sampling system in a manner that prevents the loss of volatile compounds from the container and
contamination of the sample from the apparatus itself or the laboratory environment.
6.3 Heating System—An oven large enough to accommodate the sample container, or a heating mantel designed to fit the sample
container, capable of maintaining the required temperature range uniformly throughout.
6.4 Temperature Measuring Device—A thermometer or thermocouple capable of measuring the temperature of the heating
system in the required range of operation, to within approximately 5°C.
6.5 Thermal Desorption Apparatus: System—
Tenax is a trademark of Teijin Carbon America, Inc., Rockwood, TN.
E1413 − 19
5.3.1 Sampling System—An air-tight syringe is connected to the back-end of a Tenax tube. The front end of the Tenax tube is
fitted into the heated container.A system capable of desorbing trapped volatile compounds from an adsorbent tube by means of
elevated temperature, refocusing them on a cold-trap, and subsequently introducing them to a capillary GC column by flash
heating. The desorption apparatus is directly coupled to a GC-MS.
5.3.2 In order to prevent leakage and contamination, the system should be designed to minimize loss of vapors from the
container. For example by means of a septum mounted on top of the lid of the container.
5.3.3 Thermal Desorption Device—A system capable of desorbing the volatiles by means of elevated temperature and trapping
the volatiles in a cold-trap. This apparatus is directly coupled to a GC-MS.
6.6 Adsorption Tubes: Puncturing Device—
5.4.1 Charcoal Tubes—Suitable charcoal filter and sample adsorption tubes may be made by inserting a small (approximately
1 cm) plug of glass wool or cotton in the bottom of a Pasteur pipette (approximately 5 mm diameter), then adding 2.5 to 5 cm
of activated charcoal, and finally, holding the charcoal in place with an additional plug of glass wool or cotton.
5.4.1.1 Alternatively, charcoal tubes are available from commercial sources.A device, such as a nail, that is capable of
puncturing small holes in the lid of the sample container. The size of the holes is such that the adsorbent tubes can be introduced.
5.4.2 Tenax Tubes—Suitable Tenax tubes are commercially available. Note that solvent extraction of these tubes results in
complications in the desorbing phase because certain solvents cause the dissolution of the Tenax. Tenax should be employed when
thermal desorption is to be performed.
5.5 Heating System—A heating mantel designed to fit the evidence container or an oven or a hot plate.
5.5.1 An oven may be set up with any number of stations to allow for multiple sample preparation.
5.6 Temperature Measuring Device—A thermometer or thermocouple capable of measuring temperatures in the range of 40 to
150°C.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent Use reagent grade or better chemicals shall be used in all tests. Unless otherwise indicated,
it is intended that all reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical
Society where such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of
sufficiently high purity through evaluation of appropriate blank(s) to permit its use without lessening the accuracy of the
determination.
7.2 Solid Adsorbent: Filter—
6.2.1 Activated Charcoal (coconut).
6.2.1.1 Charcoal may be activated and cleaned by heating in a 400°C oven for approximately 4 hours and cooling in a
desiccator.
6.2.1.2 Test each new or reconditioned batch of charcoal for residual hydrocarbons by analyzing a concentrated extract of blank
adsorption media according to Test Method E1618.Permeable material such as silanized glass wool, wire mesh or cotton held in
place with a frit.
6.2.2 Tenax:
6.2.2.1 Tenax may be cleaned and conditioned according to the manufacturer’s instructions.
6.2.2.2 Test each new or reconditioned batch of Tenax for residual hydrocarbons by analyzing a concentrated extract of blank
adsorption media according to Test Method E1618.
7.3 Solid Adsorbent—Activated carbon, Tenax TA or equivalent.
7.4 Sampling Tubes—Glass Pasteur pipettes or equivalent glass tubes for solvent elution, and stainless steel or glass tubes for
thermal desorption.
7.5 Glass Wool, Adsorbent Tubes—or cotton, free of extractable hydrocarbons.Sampling tubes packed with a solid adsorbent.
7.5.1 Pre-packed adsorbent tubes are commercially available. Empty sampling tubes that can be packed by the purchaser are
also available.
7.5.1.1 Activated carbon tubes and equivalent for solvent elution can be made by inserting a filter into the bottom of a sampling
tube (approximately 5-mm diameter), then adding 2.5 cm to 5 cm of activated carbon or equivalent, which is held in place with
a second filter.
7.5.1.2 Tenax TA tubes and equivalent for thermal desorption can be made by inserting a filter into one end of a sampling tube,
adding approximately 80 mg of pre-conditioned Tenax TA or equivalent, and then packing tightly with a second filter.
NOTE 1—Tenax TA or equivalent is conditioned by heating, in accordance with instrument manufacturer or supplier instructions.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. PharmaceuticalPharmacopeial Convention, Inc. (USPC), Rockville, MD.
E1413 − 19
7.6 Extraction solvent (for example,Screw cap carbonor disulfide, pentane, ethylcrimp-top glass vials ether).with polytetrafluo-
roethylene (PTFE) lined seals.
6.4.1 Read and follow the safety precautions described in the Safety Data Sheets (SDS) of the extraction solvent that is used.
6.4.2 Test each new lot number of the extraction solvent by analyzing a concentrated portion according to Test Method E1618.
7.7 Tape, rubber sleeve stopper, or equivalent.
7.8 Elution Solvent—Pasteur pipettes and glass vials freeSuitable elution solvents include carbon disulfide, ofn extractable
hydrocarbons.-pentane, dichloromethane and diethyl ether.
8. Sample Preparation
8.1 Observe the appropriate procedures for handling and documentation of all submitted samples (Guide (see Guide E1459 and
Practice E1492).
7.1.1 Examine the fire debris sample in order to determine that it is consistent with its description.
7.1.1.1 Resolve any discrepancies between the submitting agent’s description of the evidence and the analyst’s observation with
the submitting agent prior to the completion of the report.
7.2 This is a potentially destructive technique. Portions of the sample subjected to this procedure may not be suitable for
re-sampling. Therefore, a portion of the sample extract should be saved for potential future analysis. Consider using passive
headspace concentration as described in Practice E1412 which is essentially nondestructive.
8.2 The system should be designed so that the majority of the samples can be extracted from the container in which they are
delivered to the laboratory.Prepare the fire debris sample container for sampling by dynamic headspace concentration.
8.2.1 Alternatively, the sample or a portion of the sample can be placed in an appropriate, clean sampling container which is
designed to be flushed by positive or negative pressure.The sampling system is designed so that the headspace sample can be
extracted from the container in which it was received at the laboratory.
8.2.1.1 Alternatively, the fire debris sample, or a portion of it, can be transferred to a clean, rigid sample container suitable for
dynamic headspace sampling, such as a metal can with a friction-seal lid.
8.2.1.2 Verify the cleanliness of the transfer container prior to sample transfer. Cleanliness is determined by means of analysis
of a dynamic headspace concentration sample obtained from the empty transfer container using the same conditions as will be used
for the questioned sample.
8.2.1.3 Allow the transfer container with sample to equilibrate for at least one hour before sampling
8.2.2 Create two holes in the lid of the rigid sample container using a puncturing device, such that the adsorbent tubes can be
introduced.
8.2.2.1 Seal the holes with tape, rubber sleeve stopper, or equivalent.
NOTE 2—Cans that are designed for fire debris samples, with a hole pre-fitted with a rubber sleeve stopper, are commercially available.
9. Adsorption Procedure
9.1 A laboratory typically has one method of adsorption and elution that is employed. The most common combinations in use
are charcoal adsorption followed by solvent elution, and Tenax adsorption followed by thermal desorption. Both adsorbents can
be collected using uses either a positive applied pressure-based system or a negative pressure system. Other solid adsorbents and
collection systems applied pressure-based system. Either type of system can be used as long as the method has been validated with
a wide variety of ignitablewith the adsorbent tubes described in 7.5liquids with a range of both flash points and polarity.
8.1.1 The volume of air sampled is generally less when thermal desorption is employed as the entire collected sample is
commonly injected into the GC-MS system for analysis.
8.1.2 With thermal desorption there is typically no material that can be archived once GC-MS analysis has been performed. If
archival of a portion of the sample extract is needed, then a different adsorbent and elution combination should be chosen either
following this practice, or following one of the other sample collection methods for fire debris analysis (Practices E1386 or E1412).
Some instrument manufacturers now have the facility to collect the unused sample from the split; if your instrument has such
capability, then there will be material available for archival when thermal desorption is used.
9.2 Positive Pressure: Applied Pressure-Based System:
9.2.1 Place the inlet inert gas filtering adsorption tube and the outlet sample adsorption tube through the holes in the lid of the
sample container by penetrating the tape, rubber sleeve stoppers, or equivalent covering the holes.
9.2.1.1 Use a new inlet inert gas filtering adsorption tube for each sample container.
9.2.2 Place the sample container in the heat
...