ASTM E1412-19

Standard Practice for Separation of Ignitable Liquid Residues from Fire Debris Samples by Passive Headspace Concentration with Activated Charcoal

SIGNIFICANCE AND USE
4.1 This practice is useful for preparing extracts from fire debris for later analysis by gas chromatography mass spectrometry.  
4.2 This is a very sensitive separation procedure, capable of isolating quantities smaller than 1/10 μL of ignitable liquid residue from a sample.
SCOPE
1.1 This practice describes the procedure for separation of small quantities of ignitable liquid residues from samples of fire debris using an adsorbent material to extract the residue from the static headspace above the sample, then eluting the adsorbent with a solvent.  
1.2 While 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 of ignitable liquid residues in the sample.  
1.2.1 Unlike other methods of separation and concentration, this practice is essentially nondestructive.  
1.3 Alternate separation and concentration procedures are listed in the referenced documents (see Practices E1386, E1388, E1413, and E2154).  
1.4 This practice does not replace knowledge, skill, ability, experience, education, or training and should be used in conjunction with professional judgment.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.7 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.

General Information

• Status: Published
• Publication Date: 14-Nov-2019
• ICS: 13.220.99 - Other standards related to protection against fire
• Technical Committee: E30 - Forensic Sciences
• Drafting Committee: E30.01 - Criminalistics

Relations

• Refers: ASTM E1388-24 - Standard Practice for Static Headspace Sampling of Vapors from Fire Debris Samples
• Effective Date: 01-Mar-2024
• Refers: ASTM E2154-15 - Standard Practice for Separation and Concentration of Ignitable Liquid Residues from Fire Debris Samples by Passive Headspace Concentration with Solid Phase Microextraction (SPME)
• Effective Date: 01-Mar-2015
• Refers: ASTM E1618-14 - Standard Test Method for Ignitable Liquid Residues in Extracts from Fire Debris Samples by Gas Chromatography-Mass Spectrometry
• Effective Date: 01-Jul-2014
• Refers: ASTM E1413-13 - Standard Practice for Separation of Ignitable Liquid Residues from Fire Debris Samples by Dynamic Headspace Concentration
• Effective Date: 15-Aug-2013
• Refers: ASTM E1459-13 - Standard Guide for Physical Evidence Labeling and Related Documentation
• Effective Date: 15-Feb-2013
• Refers: ASTM E1388-12 - Standard Practice for Sampling of Headspace Vapors from Fire Debris Samples
• Effective Date: 01-Feb-2012
• Refers: ASTM E1492-11 - Standard Practice for Receiving, Documenting, Storing, and Retrieving Evidence in a Forensic Science Laboratory
• Effective Date: 01-Jun-2011
• Refers: ASTM E1618-11 - Standard Test Method for Ignitable Liquid Residues in Extracts from Fire Debris Samples by Gas Chromatography-Mass Spectrometry
• Effective Date: 01-Jun-2011
• Refers: ASTM E1386-10 - Standard Practice for Separation of Ignitable Liquid Residues from Fire Debris Samples by Solvent Extraction
• Effective Date: 01-Feb-2010
• Refers: ASTM E1618-10 - Standard Test Method for Ignitable Liquid Residues in Extracts from Fire Debris Samples by Gas Chromatography-Mass Spectrometry
• Effective Date: 15-Jan-2010
• Refers: ASTM E1386-09 - Standard Practice for Separation and Concentration of Ignitable Liquid Residues from Fire Debris Samples by Solvent Extraction
• Effective Date: 01-Nov-2009
• Refers: ASTM E2451-08 - Standard Practice for Preserving Ignitable Liquids and Ignitable Liquid Residue Extracts from Fire Debris Samples
• Effective Date: 01-Mar-2008
• Refers: ASTM E2154-01(2008) - Standard Practice for Separation and Concentration of Ignitable Liquid Residues from Fire Debris Samples by Passive Headspace Concentration with Solid Phase Microextraction (SPME)
• Effective Date: 01-Feb-2008
• Refers: ASTM E1413-07 - Standard Practice for Separation and Concentration of Ignitable Liquid Residues from Fire Debris Samples by Dynamic Headspace Concentration
• Effective Date: 15-Apr-2007
• Refers: ASTM E1618-06 - Standard Test Method for Ignitable Liquid Residues in Extracts from Fire Debris Samples by Gas Chromatography-Mass Spectrometry
• Effective Date: 01-Jun-2006

Overview

ASTM E1412-19: Standard Practice for Separation of Ignitable Liquid Residues from Fire Debris Samples by Passive Headspace Concentration with Activated Charcoal provides a sensitive and reliable method for extracting ignitable liquid residues (ILRs) from fire debris. This standard, established by ASTM International and developed by Committee E30 on Forensic Sciences, outlines a passive headspace concentration technique using activated charcoal. The resulting extracts are suitable for detailed analysis, particularly by gas chromatography-mass spectrometry (GC-MS), and support investigations into fire causes and origins.

Key Topics

• Passive Headspace Concentration: The standard describes placing activated charcoal in an evidence container with fire debris, allowing volatile ILRs to adsorb onto the charcoal from the headspace. The charcoal is later eluted with a suitable solvent for analysis.
• High Sensitivity Extraction: Capable of separating ILR quantities smaller than 0.1 μL, making it invaluable when trace levels are involved.
• Non-destructive Methodology: Unlike some other extraction procedures, this approach does not significantly alter or destroy the original sample.
• Quality Assurance Measures: The practice includes procedures for analyzing blanks and ensuring both the adsorbent and solvents are free from contaminants.
• Applicable Scope: Effective across a wide range of ignitable liquid concentrations, though especially beneficial when only low levels are present.

Applications

• Forensic Fire Investigation: ASTM E1412-19 is widely applied in forensic science laboratories for analyzing fire debris and detecting the presence of accelerants or other ignitable liquids, a common requirement in arson investigations.
• Gas Chromatography-Mass Spectrometry Preparation: The procedure prepares clean extracts suitable for subsequent GC-MS analysis, aiding accurate identification of residual ignitable liquids.
• Evidence Preservation: By relying on non-destructive sampling and extract storage techniques, investigators preserve the integrity of evidence, allowing for future reanalysis if necessary.
• Routine and Screening Procedures: The method can be adapted for rapid screening or more thorough analyses, depending on laboratory protocols and case demands.
• Quality Control: Laboratories can establish and document robust quality assurance processes, ensuring reliability and reproducibility in forensic results.

Related Standards

Several related ASTM standards complement or provide alternative approaches to separating ignitable liquid residues:

• ASTM E1386: Practice for Separation of Ignitable Liquid Residues from Fire Debris by Solvent Extraction
• ASTM E1388: Practice for Static Headspace Sampling of Vapors from Fire Debris Samples
• ASTM E1413: Practice for Dynamic Headspace Concentration onto Adsorbent Tubes
• ASTM E2154: Practice for Separation and Concentration by Passive Headspace with Solid Phase Microextraction (SPME)
• ASTM E1618: Test Method for Ignitable Liquid Residues in Extracts from Fire Debris Samples by GC-MS
• ASTM E1459 & E1492: Guides for evidence labeling, documentation, and handling
• ASTM E2451: Practice for Preserving Ignitable Liquids and Their Extracts

Practical Value

Adhering to ASTM E1412-19 ensures reproducible, sensitive, and contamination-controlled extraction of ignitable liquids from fire debris, enabling forensic scientists and investigators to obtain defensible analytical results. This standard is recognized internationally and aligns with established principles for developing trustworthy forensic protocols, as recommended by the World Trade Organization’s Technical Barriers to Trade Committee. By implementing this practice, laboratories contribute to justice processes and support the accurate determination of fire causes, arson detection, and the safeguarding of public safety.

Keywords: ASTM E1412-19, ignitable liquid residue, fire debris, passive headspace concentration, activated charcoal, forensic science, fire investigation, GC-MS, quality assurance, evidence preservation, ASTM standards

Standards Content (Sample)

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.
Designation: E1412 − 19 An American National Standard
Standard Practice for
Separation of Ignitable Liquid Residues from Fire Debris
Samples by Passive Headspace Concentration with
Activated Charcoal
This standard is issued under the fixed designation E1412; 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 2. Referenced Documents
2.1 ASTM Standards:
1.1 This practice describes the procedure for separation of
small quantities of ignitable liquid residues from samples of E1386 Practice for Separation of Ignitable Liquid Residues
fire debris using an adsorbent material to extract the residue from Fire Debris Samples by Solvent Extraction
E1388 Practice for Static Headspace Sampling of Vapors
from the static headspace above the sample, then eluting the
adsorbent with a solvent. from Fire Debris Samples
E1413 Practice for Separation of Ignitable Liquid Residues
1.2 Whilethispracticeissuitableforsuccessfullyextracting
from Fire Debris Samples by Dynamic Headspace Con-
ignitable liquid residues over the entire range of concentration,
centration onto an Adsorbent Tube
theheadspaceconcentrationmethodsarebestusedwhenahigh
E1459 Guide for Physical Evidence Labeling and Related
level of sensitivity is required due to a very low concentration
Documentation
of ignitable liquid residues in the sample.
E1492 Practice for Receiving, Documenting, Storing, and
1.2.1 Unlike other methods of separation and concentration,
Retrieving Evidence in a Forensic Science Laboratory
this practice is essentially nondestructive.
E1618 TestMethodforIgnitableLiquidResiduesinExtracts
1.3 Alternate separation and concentration procedures are
from Fire Debris Samples by Gas Chromatography-Mass
listed in the referenced documents (see Practices E1386,
Spectrometry
E1388, E1413, and E2154).
E2154 Practice for Separation and Concentration of Ignit-
able Liquid Residues from Fire Debris Samples by Pas-
1.4 This practice does not replace knowledge, skill, ability,
sive Headspace Concentration with Solid Phase Microex-
experience, education, or training and should be used in
traction (SPME)
conjunction with professional judgment.
E2451 Practice for Preserving Ignitable Liquids and Ignit-
1.5 The values stated in SI units are to be regarded as
able Liquid Residue Extracts from Fire Debris Samples
standard. No other units of measurement are included in this
standard. 3. Summary of Practice
1.6 This standard does not purport to address all of the
3.1 Charcoal in some form of an adsorption package is
safety concerns, if any, associated with its use. It is the
placed in the sample container to adsorb ignitable liquid
responsibility of the user of this standard to establish appro-
residues. The container can be heated or left at ambient
priate safety, health, and environmental practices and deter-
temperature. The charcoal is removed and eluted with a
mine the applicability of regulatory limitations prior to use.
suitable elution solvent as listed in 6.3.
1.7 This international standard was developed in accor-
4. Significance and Use
dance with internationally recognized principles on standard-
4.1 This practice is useful for preparing extracts from fire
ization established in the Decision on Principles for the
debris for later analysis by gas chromatography mass spec-
Development of International Standards, Guides and Recom-
trometry.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
4.2 This is a very sensitive separation procedure, capable of
isolating quantities smaller than ⁄10 µL of ignitable liquid
residue from a sample.
This practice is under the jurisdiction of ASTM Committee E30 on Forensic
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 15, 2019. Published December 2019. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1991. Last previous edition approved in 2016 as E1412 – 16. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E1412-19. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1412 − 19
5. Apparatus 7. Sample Preparation/Adsorption Procedure
5.1 Heating System—An oven, or a heating mantle to fit the 7.1 Observe the appropriate procedures for handling and
evidence container (or a hot plate). documentation of all submitted samples as described in Prac-
5.1.1 An oven is recommended to achieve a constant tice E1492.
temperature throughout the system. 7.1.1 Open and examine the fire debris sample in order to
determine that it is consistent with its description.
5.2 Temperature Measuring Device—A thermometer or
7.1.1.1 Resolve any discrepancies between the submitting
thermocouple capable of measuring temperatures in the range
agency’s description of the evidence and the analyst’s obser-
of 40 to 100°C.
vation prior to the completion of the report.
5.3 Adsorption Package.
7.2 Place an adsorbent package in the evidence container
5.3.1 Commercial charcoal adsorption packages are avail-
according to laboratory protocols and reseal the container.
able from several companies. These packages, in the form of
Suspend the adsorbent package above the sample whenever
polymer strips or small charcoal canisters or “C-bags,” are
possible.
used to adsorb organic vapors.
5.3.1.1 Theminimumrecommendedpolymerstripsizeis10 7.3 Heat the container to a temperature of 50 to 80°C, for 2
mm by 10 mm, or 100 mm . to 24 h. The longer times or higher temperatures, or both, are
5.3.2 Non-Commercial Adsorption Packages. required for the adsorption of higher boiling point compounds
5.3.2.1 C-Bags—Prepare C-bags by encapsulating 0.2 g of or for the adsorption of very small quantities of volatile
activated charcoal within a folded sheet of high strength, light hydrocarbons. The adsorption temperature and duration can
3, 5
weight, high porosity tissue paper, such as that commonly used vary based on the sample.
for making tea bags. 7.3.1 When other evidentiary considerations arise (such as
5.3.3 Storage of Adsorption Packages—To prevent document or latent print examinations) it may be appropriate to
contamination, store all adsorption packages away from any conduct the adsorption at ambient temperature (approximately
sources of organic vapors prior to and after sampling. 20°C) for extended periods (24 h or longer) to minimize
damage.
6. Reagents and Materials
7.3.2 Room temperature adsorption could also be appropri-
ate to detect low molecular weight compounds.
6.1 Purity of Reagents—Reagent grade or better chemicals
7.3.3 The optimum adsorption time for maximum sensitiv-
shall be used in all tests. Unless otherwise indicated, it is
ity will depend on the adsorption package and temperature
intended that all reagents conform to the specifications of the
selected.Temperatures lower than 60°C could be insufficient to
Committee on Analytical Reagents of the American Chemical
volatilize compounds heavier than C16.
Society where such specifications are available. Other grades
7.3.4 Temperatures in excess of 80°C could result in dis-
can be used, provided it is first ascertained that the reagent is
proportionate recovery of higher molecular weight compounds
of sufficiently high purity to permit its use without lessening
with the displacement of lower molecular weight compounds.
the accuracy of the determination.
7.3.5 The optimum adsorption time for representative sam-
6.2 Adsorption Package:
pling or maximum sensitivity, or both, wi
...

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: E1412 − 16 E1412 − 19
Standard Practice for
Separation of Ignitable Liquid Residues from Fire Debris
Samples by Passive Headspace Concentration Withwith
Activated Charcoal
This standard is issued under the fixed designation E1412; 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 samples of fire
debris using an adsorbent material to extract the residue from the static headspace above the sample, then eluting the adsorbent
with a solvent.
1.2 While 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 of
ignitable liquid residues in the sample.
1.2.1 Unlike other methods of separation and concentration, this practice is essentially nondestructive.
1.3 Alternate separation and concentration procedures are listed in the referenced documents (see Practices E1386, E1388,
E1413, and E2154).
1.4 This practice does not replace knowledge, skill, ability, experience, education, or training and should be used in conjunction
with professional judgment.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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.
1.7 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
E1413 Practice for Separation of Ignitable Liquid Residues from Fire Debris Samples by Dynamic Headspace Concentration
onto an Adsorbent Tube
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
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
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 Jan. 15, 2016Nov. 15, 2019. Published February 2016December 2019. Originally approved in 1991. Last previous edition approved in 20122016
as E1412 – 12.E1412 – 16. DOI: 10.1520/E1412-16.10.1520/E1412-19.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’sstandard’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
E1412 − 19
3. Summary of Practice
3.1 Charcoal in some form of an adsorption package is placed in the sample container to adsorb ignitable liquid residues. The
container maycan be heated or left at ambient temperature. The charcoal is removed and eluted with a suitable elution solvent as
listed in 6.3.
4. Significance and Use
4.1 This practice is useful for preparing extracts from fire debris for later analysis by gas chromatography mass spectrometry.
4.2 This is a very sensitive separation procedure, capable of isolating quantities smaller than ⁄10 μL of ignitable liquid residue
from a sample.
5. Apparatus
5.1 Heating System—An oven, or a heating mantle to fit the evidence container (or a hot plate).
5.1.1 An oven is recommended to achieve a constant temperature throughout the system.
5.2 Temperature Measuring Device—A thermometer or thermocouple capable of measuring temperatures in the range of 40 to
100°C.
5.3 Adsorption Package.
5.3.1 Commercial charcoal adsorption packages are available from several companies. These packages, in the form of polymer
strips or small charcoal canisters or “C-bags,” are used to adsorb organic vapors.
5.3.1.1 The minimum recommended polymer strip size is 10 mm by 10 mm, or 100 mm .
5.3.2 Non-Commercial Adsorption Packages.
5.3.2.1 C-Bags—Prepare C-bags by encapsulating 0.2 g of activated charcoal within a folded sheet of high strength, light
weight, high porosity tissue paper, such as that commonly used for making tea bags.
5.3.3 Storage of Adsorption Packages—To prevent contamination, store all adsorption packages away from any sources of
organic vapors prior to and after sampling.
6. Reagents and Materials
6.1 Purity of Reagents—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 maycan be used, provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of the determination.
6.2 Adsorption Package:
6.2.1 C-Bags:
6.2.1.1 4 by 5 in. (approximate) high strength, light weight, high porosity filter paper.
6.2.1.2 Activated charcoal.
6.2.2 Commercial charcoal adsorption package.
6.2.3 Check charcoal media purity by, at a minimum, desorbing a representative unit using the same elution solvent as will be
used for questioned samples and analyzing in accordance with Test MethodWhen necessary, charcoal can be activated and cleaned
by heating in a 400°C oven for E1618.4 h, then cooled in a desiccator.
6.3 Elution Solvent—Suitable elution solvents are carbon disulfide, n –pentane, -pentane, or diethyl ether. Use of a heavier
solvent, such as toluene or tetrachloroethylene, is sometimes necessary when the compounds of interest have low molecular
weights.
6.3.1 Check solvent purity by evaporating to at least twice the extent used in the analysis and analyzing the evaporated solvent
in accordance with Test Method E1618.
6.3.1 Read and follow the safety precautions described in the safety data sheet (SDS) of the extraction solvent that is used.
7. Sample Preparation/Adsorption Procedure
7.1 Observe the appropriate procedures for handling and documentation of all submitted samples as described in Practice
E1492.
7.1.1 Open and 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 agency’s description of the evidence and the analyst’s observation
prior to the completion of the report.
Dietz, W. R., “Improved Charcoal Packaging for Accelerant Recovery by Passive Diffusion,” Journal of Forensic Sciences, Vol 35, 1991, pp. 111–121 (Unk).
Reagent Chemicals, American Chemical Society Specifications,ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference
Materials, 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.
E1412 − 19
7.2 Place an adsorbent package in the evidence container according to laboratory protocols and reseal the container. Suspend
the adsorbent package above the sample wheneve
...