ASTM E2997-16

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: E2997 − 16 An American National Standard
Standard Test Method for
Analysis of Biodiesel Products by Gas Chromatography-
Mass Spectrometry
This standard is issued under the fixed designation E2997; 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 E1386 Practice for Separation of Ignitable Liquid Residues
from Fire Debris Samples by Solvent Extraction
1.1 This test method covers the analysis and identification
E1412 Practice for Separation of Ignitable Liquid Residues
of the fatty acid methyl esters (FAMEs) and petroleum distil-
from Fire Debris Samples by Passive Headspace Concen-
late components of biodiesel products.
tration with Activated Charcoal
1.2 This test method is suitable for identifying the compo-
E1413 Practice for Separation of Ignitable Liquid Residues
nents of biodiesel products in extracts of debris samples or in
from Fire Debris Samples by Dynamic Headspace Con-
liquid samples.
centration onto an Adsorbent Tube
1.3 The identification of a specific source of the FAMEs or
E1492 Practice for Receiving, Documenting, Storing, and
the proportion of the blend of biodiesel requires additional Retrieving Evidence in a Forensic Science Laboratory
analysis and is beyond the scope of this test method.
E1618 TestMethodforIgnitableLiquidResiduesinExtracts
from Fire Debris Samples by Gas Chromatography-Mass
1.4 This test method cannot replace the requisite
Spectrometry
knowledge, skills, or abilities acquired through appropriate
E2154 Practice for Separation and Concentration of Ignit-
education, training, and experience and should be used in
able Liquid Residues from Fire Debris Samples by Pas-
conjunction with sound professional judgment.
sive Headspace Concentration with Solid Phase Microex-
1.5 The values stated in SI units are to be regarded as
traction (SPME)
standard. No other units of measurement are included in this
E2451 Practice for Preserving Ignitable Liquids and Ignit-
standard.
able Liquid Residue Extracts from Fire Debris Samples
1.6 This standard does not purport to address all of the
E2881 Test Method for Extraction and Derivatization of
safety concerns, if any, associated with its use. It is the
Vegetable Oils and Fats from Fire Debris and Liquid
responsibility of the user of this standard to establish appro-
Samples with Analysis by Gas Chromatography-Mass
priate safety, health, and environmental practices and deter-
Spectrometry
mine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accor-
3. Summary of Test Method
dance with internationally recognized principles on standard-
3.1 Traditional ignitable liquid analysis will be used to
ization established in the Decision on Principles for the
identify biodiesel products.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
3.2 The debris sample is extracted or an aliquot of a liquid
Barriers to Trade (TBT) Committee.
is extracted or diluted and analyzed by gas chromatography-
mass spectrometry (GC-MS).
2. Referenced Documents
3.3 If fatty acid methyl esters (FAMEs) are suspected,
2.1 ASTM Standards:
further solvent extraction and analysis on a FAME-specific
E620 Practice for Reporting Opinions of Scientific or Tech-
column may be required.
nical Experts
3.4 Specific chemical components (fatty acid methyl esters)
are identified by their retention times and mass spectra.
ThistestmethodisunderthejurisdictionofASTMCommitteeE30onForensic
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics.
Current edition approved March 1, 2016. Published April 2016. DOI: 10.1520/
4. Significance and Use
E2997-16.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.1 This test method specifically identifies fatty acid methyl
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
esters and petroleum distillates found in biodiesel products.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Derivatization is not necessary to identify FAMEs.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2997 − 16
4.1.1 This test method is useful when biodiesel products are 5.1.3 GC Oven—A column oven capable of reproducible
suspected as a fuel source in a fire or a fuel product case and temperature program operation in the range from 50 to 300°C.
the identification of the “bio” portion of the fuel is of interest.
5.2 Mass Spectrometer—Capable of acquiring mass spectra
4.1.2 The identification of biodiesel in samples from a fire
from m/z 40 to m/z 400 with unit resolution or better, with
scene can support the field investigator’s opinion regarding the
continuous data output.
origin and cause of the fire or provide investigative leads.
5.2.1 Sensitivity and Resolution—The system shall be ca-
4.1.3 Theidentificationofbiodieselinasampleoffuelfrom
pable of detecting each component of the reference or test
a dispensing container or fuel tank can support the field
mixture (see 6.6) and providing sufficient ion intensity data to
investigator’s findings in a fuel product tampering investiga-
identify each component, either by computer search of a mass
tion.
spectral library or by comparison with reference spectra.
4.2 FAMEs can be identified in debris samples using head-
5.3 Data Station—A computerized data station capable of
space extraction techniques and GC-MS.
storing time sequenced mass spectral data from sample runs.
4.2.1 Solvent extraction may be required to further identify
5.3.1 Data Handling—The data system shall be capable of
and characterize the FAME content in biodiesel.
performing, either through its operating system or by user
4.2.2 The presence of FAMEs and petroleum diesel is a
programming, various data handling functions, including input
strong indication of a biodiesel product, as FAMEs are not
and storage of sample data files, generation of extracted ion
naturally occurring.
profiles, searching data files for selected compounds, and
4.3 Biodieselproductscanbeidentifiedinliquidsamplesby
qualitative and semi-quantitative compound analysis.
GC-MS after appropriate solvent dilution or extraction.
5.3.2 Mass Spectral Libraries—The system shall be capable
4.4 Biodiesel is available in different blends, where B100 is
of retrieving a specified mass spectrum from a data file and
100 % biodiesel (typically 100 % transesterified vegetable oils
comparing it against a library of mass spectra available to the
or recycled restaurant greases) and B2 is 2 % biodiesel and 98
data system. This capability is considered an aid to the analyst,
% petroleum diesel, with variations in between.
who will use it in conjunction with chromatographic data and
4.5 This test method is a sensitive technique and can detect
known reference materials to identify unknown components.
quantities as small as 7 µL of biodiesel residue in an extract
5.4 Syringes—A syringe capable of introducing a sample
from a debris sample.
size in the range from 0.1 to 10.0 µL.
4.6 This test method can be hampered by coincident extrac-
5.5 Steam bath or heating device, for use in warming
tion of interfering compounds present in the debris samples.
sample extracts in containers used during evaporation steps.
4.7 Depending on the extraction method used, this could be
a destructive technique and whenever possible the entire
6. Reagents and Materials
sample should not be used for the procedure. Solvent extracted
6.1 Purity of Reagents—Reagent grade chemicals should be
portions of the sample are not suitable for resampling.
used in all tests. It is intended that all reagents conform to the
4.8 Alternate methods of extraction or analysis exist and
specifications of the Committee on Analytical Reagents of the
may be suitable for use in obtaining similar results and
American Chemical Society. Other grades may be used,
conclusions.
provided it is first ascertained that the reagent is of sufficiently
5. Apparatus
high purity to permit its use without lessening the accuracy of
the determination.
5.1 Gas Chromatograph—A chromatograph capable of us-
ing capillary columns and being interfaced to a mass spectrom-
6.2 Solvent—A suitable solvent, such as n-pentane, carbon
eter.
disulfide, or other solvent that will not interfere with the
5.1.1 Sample Inlet System—A sample inlet system that can
analysis.
be operated in either split or splitless mode with capillary
6.2.1 Solvent purity can be verified by evaporating to at
columns; the inlet system may use on-column technology.
least twice the extent used in the analysis and analyzing the
5.1.2 Column—A non-polar capillary, bonded phase, meth-
evaporated solvent in accordance with Test Method E1618.
ylsilicone or phenylmethylsilicone column or equivalent, or a
6.3 Filter apparatus, free of extractable hydrocarbons, oils,
polar capillary, bonded phase column, such as a cyanopropyl-
and fats.
based fatty acid specific column or equivalent, may be used to
determine the presence of fatty acids.
6.4 Evaporation accelerants, compressed dry nitrogen, fil-
5.1.2.1 A polar capillary, bonded phase column, such as a
tered air, or inert gas used in the concentration of solvent
cyanopropyl-based fatty acid specific column or equivalent
extracts.
shall be used to perform comparative analysis between speci-
6.5 Carrier gas, helium or hydrogen of purity 99.995 % or
mens of questioned neat liquid samples, debris extracts, or
higher.
both.
5.1.2.2 Any column length or temperature program condi-
tions may be used for the polar column provided that each
component of the reference mixture (see 6.6.2) is adequately
Reagent Chemicals, American Chemical Society Specifications, American
separated. Chemical Society, Washington, DC.
E2997 − 16
6.6 Reference and Test Mixtures: 8.4.2 Running solvent blanks between each specimen is
6.6.1 Refer to Test Method E1618, Section 6, for the recommended but not required if studies demonstrate that the
appropriate test mixture for the hydrocarbon portion of the cleaning procedure is adequate to prevent carryover.
analysis.
8.5 Maintain reference files of known biodiesel products
6.6.2 Refer to Test Method E2881, Section 6, for the
that have been prepared and analyzed in the same manner as
appropriate reference mixture for the “bio” portion of the
the questioned samples.
analysis.
8.6 Extract a fire debris sample using one or more tech-
6.6.3 Reference biodiesel products should be obtained for
niques as described in Practices E1386, E1412, E1413,or
comparison and identification purposes. Typical chromato-
E2154 to isolate ignitable liquid residues and FAME compo-
grams of B100 and B20 on a non-polar fire debris column are
nents for analysis.
shown in Fig. 1. Typical chromatograms of B100 and B20 on
a fatty acid specific polar column are shown in Fig. 2. 8.7 Warning—Extract a fire debris sample using headspace
techniques prior
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