ASTM E2999-17

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: E2999 − 17 An American National Standard
Standard Test Method for
Analysis of Organic Compounds in Smokeless Powder by
Gas Chromatography-Mass Spectrometry and Fourier
Transform Infrared Spectroscopy
This standard is issued under the fixed designation E2999; 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 mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.1 This test method describes the analysis of organic
components in smokeless powders by gas chromatography-
2. Referenced Documents
mass spectrometry (1-6) and Fourier transform infrared spec-
2.1 ASTM Standards:
troscopy.
E620 Practice for Reporting Opinions of Scientific or Tech-
1.2 This test method is suited for analyzing samples com-
nical Experts
prisedofvisiblegrains(wholeorpartial)ofsmokelesspowder.
E1492 Practice for Receiving, Documenting, Storing, and
1.3 Analysis of post-blast debris and items containing gun-
Retrieving Evidence in a Forensic Science Laboratory
shot residue when visible grains of smokeless powder are not E2998 Practice for Characterization and Classification of
present is beyond the scope of this test method.
Smokeless Powder
1.4 The values stated in SI units are to be regarded as
3. Terminology
standard. The values given in parentheses are mathematical
3.1 Definitions of Terms Specific to This Standard:
conversions to inch-pound units that are provided for informa-
3.1.1 double-base, n—propellant containing nitrocellulose
tion only and are not considered standard.
and nitroglycerin.
1.5 This test method involves handling of low explosives
3.1.2 grain, n—an individual particle of smokeless powder.
and potentially other energetic materials. It is strongly sug-
gested that an analyst be trained in the storage and safe 3.1.3 single-base, n—propellant containing nitrocellulose as
handling of energetic materials and be familiar with the the major energetic material.
properties and hazards of explosives.
3.1.4 smokeless powder, n—a propellant and low explosive
composed of nitrocellulose and other organic and inorganic
1.6 This test method cannot replace knowledge, skill, or
compounds.
ability acquired through appropriate education, training, and
experience and should be used in conjunction with sound
3.1.5 triple-base, n—propellant containing nitrocellulose,
professional judgment.
nitroglycerin, and nitroguanidine.
1.7 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 4.1 Anextractedspecimenofsmokelesspowderisanalyzed
priate safety, health and environmental practices and deter-
by gas chromatography-mass spectrometry (GC-MS) and Fou-
mine the applicability of regulatory limitations prior to use. rier transform infrared (FTIR) spectroscopy to identify organic
1.8 This international standard was developed in accor- components.
dance with internationally recognized principles on standard-
4.2 Post GC-MS data analysis generates extracted ion pro-
ization established in the Decision on Principles for the
files (mass chromatograms) characteristic of the organic com-
Development of International Standards, Guides and Recom-
ponents in smokeless powders. Specific chemical components
(target compounds) can be identified by their mass spectra and
retention times.
ThistestmethodisunderthejurisdictionofASTMCommitteeE30onForensic
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics.
Current edition approved Sept. 15, 2017. Published September 2017. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/E2999-17. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
The boldface numbers in parentheses refer to a list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2999 − 17
4.3 FTIR analysis is used in the identification of nitrocellu- 7. Chemicals, Reagents, and Materials
lose and nitroguanidine. An FTIR generates a spectrum con-
7.1 Purity of Reagents—Reagent grade chemicals or better
sisting of IR absorption bands that can be searched through a
should be used in all tests. Unless otherwise indicated, it is
reference spectral library for a library match to nitrocellulose
intended that all reagents conform to the specifications of the
or nitroguanidine or compared to known reference materials.
Committee on Analytical Reagents of the American Chemical
Society where such specifications are available. Other grades
5. Significance and Use
may be used, provided it is first ascertained that the reagent is
of sufficiently high purity to permit its use without lessening
5.1 This test method establishes a procedure for the analysis
the accuracy of the determination.
and identification of organic components of smokeless powder
by GC-MS and FTIR.
7.2 Solvents—Methylene chloride and acetone (ACS re-
agent grade or better).
5.2 FTIR is used in the analysis of nitrocellulose, which is
a major component of all smokeless powders, and nitroguani-
7.3 GC-MS Test Mixture—The test mixture should consist
dine in triple-base powders.
of nitroglycerin, diphenylamine, ethyl centralite, and 2,6-
dinitrotoluene. The final test solution is prepared by diluting
5.3 GC-MS is used in the analysis of other organic com-
the above mixture such that the concentration of each compo-
pounds in smokeless powders, such as energetics, stabilizers,
nent is no greater than 0.005 % weight/volume (0.05 mg/mL)
plasticizers, and deterrents.
in the chosen solvent (see 7.2). Additional compounds com-
5.4 ThistestmethodisusedconcurrentlywithE2998forthe
monlyfoundinsmokelesspowdersmayalsobeincludedinthe
analysisofsmokelesspowderswhenwholeorpartialgrainsare
test mixture, such as methyl centralite, 2,4-dinitrotoluene,
present.
2-nitrodiphenylamine, 4-nitrodiphenylamine, diethylphthalate,
and dibutylphthalate.
5.5 GC-MS and FTIR are two techniques used in the
7.3.1 Appropriate concentrations of individual reference
analysis of smokeless powders. Additional techniques are
materials or standards of these compounds may be used in
available that are acceptable for use in the analysis and
addition to or instead of a test mixture.
identification of organic components of smokeless powders,
such as liquid chromatography-mass spectrometry, capillary
7.4 Internal Standard—An appropriate internal standard
electrophoresis, and gas chromatography with flame ionization
(for example, undecane, decane) may be used in the extraction
detection.
solvent for GC-MS analysis.
7.5 Reference Smokeless Powders—Reference smokeless
6. Apparatus
powders can be obtained as bulk reloading powders from
6.1 Stereo Light Microscope, with an appropriate light commercial and retail sources or directly from the distributor
source. or manufacturer.
7.6 Polystyrene Film Standard.
6.2 Gas Chromatograph-Mass Spectrometer—A gas chro-
matograph (GC) capable of using capillary columns and being
7.7 FTIR Supplies—Salt plates, mortar and pestle, pellet
interfaced to a mass spectrometer (MS) operating in electron
press.
ionization (EI) mode.
7.8 GC Carrier Gas—Helium or hydrogen of purity 99.995
6.2.1 Sample Inlet System—A sample inlet system that can
% or higher.
be operated in either split or splitless mode with capillary
7.9 Glassware and Other Supplies—Disposable test tubes,
columns; the inlet system may use on-column technology.
pipettes, beakers, autosampler vials, weigh boats, weigh paper,
6.2.2 Column—Acapillary,bondedphase,methylsiliconeor
watch glasses.
phenylmethylsilicone column or equivalent. Any column
length or temperature program conditions may be used pro-
8. Equipment Calibration and Maintenance
vided that each component of the test mixture (see 7.3)is
8.1 GC-MS Calibration and Maintenance:
adequately separated.
8.1.1 Verify the consistent performance of the chromato-
6.2.3 GC Oven—A column oven capable of reproducible
graphic instrument by using blanks and known concentrations
temperature program operation in the range from 40 to 300°C.
of either a prepared test mixture, reference materials, or
6.2.4 Mass Spectrometer—Capable of acquiring mass spec-
standards (see 7.3). Optimize gas flows periodically.
tra from m/z 40 to m/z 400 with unit resolution or better, with
8.1.2 Tune and check calibration of the mass spectrometer.
continuous data output.
8.1.2.1 Tune the mass spectrometer using perfluorotribu-
6.2.4.1 Sensitivity—The system must be capable of detect-
tylamine(PFTBA),oranotherappropriatecalibrationstandard,
ing each component of the test mixture (see 7.3) and providing
sufficient ion intensity data to identify each component, either
by computer library search or by comparison with reference
Reagent Chemicals, American Chemical Society Specifications, American
spectra. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
6.2.5 Fourier Transform Infrared Spectrometer—An FTIR
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
capable of acquiring spectra in the mid-infrared region (wave-
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
-1
number range of 4000 to 650 cm ). MD.
E2999 − 17
TABLE 1 Suggested GC-MS Conditions
according to the instrument manufacturer’s specifications,
prior to use. This should be done at least every day that the GC column: 30 metre, DB-5 capillary column
Initial temp: 45°C
instrument is used or in accordance with the manufacturer’s
Initial hold time: 3 minutes
recommendations.
Ramp 1: 15°C/minute to 150°C
8.1.2.2 Maintain tuning documentation as a portion of the Ramp 2: 40°C/minute to 265°C
Final hold time: 7 minutes
quality control documentation.
Injector temperature: 190 to 220°C
8.1.3 Equipment Maintenance:
Mode: Electron Ionization (EI)
MS scan range: 41 to 400 m/z
8.1.3.1 Change septa and clean or replace injector liners on
Solvent delay: 3 minutes
a periodic basis to avoid sample contamination by carryover of
residual material from previous sample injections.
8.2 FTIR Calibration Check and Maintenance:
used in smokeless powder formulations. The injector can be
8.2.1 Verifytheconsistentperformanceoftheinstrumentby
operated in either split or splitless mode.
analyzing a polystyrene film standard or equivalent (standard
10.4 FTIR Conditions:
or reference material per manufacturer’s recommendation)
10.4.1 Table 2 describes basic FTIR parameters that can be
prior to use. This should be done at least every day that the
used for the analysis of nitrocellulose and nitroguanidine.
instrument is used. Compare the obtained spectrum to that
10.4.2 For double and triple-base powder specimens, the
from a previously verified polystyrene film standard (or
nitroglycerin should be extracted from the specimen grains
equivalent) to verify acceptable performance.
prior to FTIR analysis using an appropriate extraction tech-
8.2.2 Maintain calibration documentation as a portion of the
nique as described in E2998.
quality control documentation.
NOTE 1—Nitroglycerin and nitrocellulose have similar FTIR spectral
9. Sample Handling
features.
9.1 Observe the appropriate procedures for handling and
10.4.3 An FTIR analysis should include an analysis of a
docume
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