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ASTM E2999-17

(Test Method)

Standard Test Method for Analysis of Organic Compounds in Smokeless Powder by Gas Chromatography-Mass Spectrometry and Fourier Transform Infrared Spectroscopy

Standard Test Method for Analysis of Organic Compounds in Smokeless Powder by Gas Chromatography-Mass Spectrometry and Fourier Transform Infrared Spectroscopy

SIGNIFICANCE AND USE
5.1 This test method establishes a procedure for the analysis and identification of organic components of smokeless powder by GC-MS and FTIR.  
5.2 FTIR is used in the analysis of nitrocellulose, which is a major component of all smokeless powders, and nitroguanidine in triple-base powders.  
5.3 GC-MS is used in the analysis of other organic compounds in smokeless powders, such as energetics, stabilizers, plasticizers, and deterrents.  
5.4 This test method is used concurrently with E2998 for the analysis of smokeless powders when whole or partial grains are present.  
5.5 GC-MS and FTIR are two techniques used in the analysis of smokeless powders. Additional techniques are available that are acceptable for use in the analysis and identification of organic components of smokeless powders, such as liquid chromatography-mass spectrometry, capillary electrophoresis, and gas chromatography with flame ionization detection.
SCOPE
1.1 This test method describes the analysis of organic components in smokeless powders by gas chromatography-mass spectrometry (1-6)2 and Fourier transform infrared spectroscopy.  
1.2 This test method is suited for analyzing samples comprised of visible grains (whole or partial) of smokeless powder.  
1.3 Analysis of post-blast debris and items containing gunshot residue when visible grains of smokeless powder are not present is beyond the scope of this test method.  
1.4 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions to inch-pound units that are provided for information only and are not considered standard.  
1.5 This test method involves handling of low explosives and potentially other energetic materials. It is strongly suggested that an analyst be trained in the storage and safe handling of energetic materials and be familiar with the properties and hazards of explosives.  
1.6 This test method cannot replace knowledge, skill, or ability acquired through appropriate education, training, and experience and should be used in conjunction with sound professional judgment.  
1.7 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.  
1.8 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-Sep-2017
ICS
07.140 - Forensic science
Technical Committee
E30 - Forensic Sciences
Drafting Committee
E30.01 - Criminalistics
Current Stage
Ref Project

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ASTM E2999-17 - Standard Test Method for Analysis of Organic Compounds in Smokeless Powder by Gas Chromatography-Mass Spectrometry and Fourier Transform Infrared SpectroscopyASTM E2999-17 - Standard Test Method for Analysis of Organic Compounds in Smokeless Powder by Gas Chromatography-Mass Spectrometry and Fourier Transform Infrared Spectroscopy
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ASTM E2999-17 - Standard Test Method for Analysis of Organic Compounds in Smokeless Powder by Gas Chromatography-Mass Spectrometry and Fourier Transform Infrared Spectroscopy
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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
1
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
2
mass spectrometry (1-6) and Fourier transform infrared spec-
3
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.
1
ThistestmethodisunderthejurisdictionofASTMCommitteeE30onForensic
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics.
3
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
2
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
1

---------------------- Page: 1 ----------------------
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 tha
...

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1.1 Infrared (IR) spectroscopy is a valuable method of fiber polymer identification and comparison in forensic examinations. The use of IR microscopes, coupled with Fourier transform infrared (FTIR) spectrometers, has greatly simplified the IR analysis of single fibers, thus making the technique feasible for routine use in the forensic laboratory. This guide provides basic recommendations and information about IR spectrometers and accessories, with an emphasis on sampling techniques specific to fiber examinations. The particular method(s) employed by each examiner or laboratory will depend upon available equipment, examiner training, sample suitability, and sample size.  
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4.1 A microscopical hair examination is conducted to determine if the item is a hair; from a human; from a particular somatic region; characteristic of a broad geographically-assigned ancestral group; characteristic of a particular growth phase; damaged; symptomatic of disease, condition, or disorder; forcibly removed; chemically altered (for example, dyed or bleached); suitable for microscopical comparison; suitable for DNA analysis; and similar to or different from a known sample (4-9).  
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1.1 This guide covers procedures used by forensic laboratory personnel in the forensic examination of hair by microscopy, including microscopical comparisons and classification of hair samples.  
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5.1 The overarching goals of the forensic analysis of geological materials include (A) identification of an unknown material (see 11.3), (B) analysis of soils, sediments, or rocks to restrict their possible geographic origins as part of a provenance analysis (see 11.4), and (C) comparison of two or more samples to assess if they could have originated from the same source or to exclude a common source based on observation of exclusionary differences (see 11.5). XRD is only one analytical method that can be applied to the evidentiary samples in service of these distinct goals.  
5.2 Within the analytical scheme of geological materials, XRD analysis is used to: identify the crystalline components within a sample; identify the crystalline components separated from a mixture, typically clay-sized material (see 8.8), or a selected particle class for which additional analysis is needed (see 8.11); or compare two or more samples based on the identified crystalline phases or diffraction patterns (see 11.5).  
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1.1 This guide covers techniques and procedures for the use of powder X-ray diffraction (XRD) in the forensic analysis of geological materials (to include soils, rocks, sediments, and materials derived from them such as concrete), to enable non-consumptive identification of solid crystalline materials present as single components or multi-component mixtures.  
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4.3.2 Texture Elucidation—SEM images and elemental maps provide insight into the texture (for example, surface topography, distribution of inclusions).  
4.3.3 Element Identification—Determination of the elements detected in a sample layer.  
4.3.4 Relative Elemental Abundance Determination—An EDS spectrum permits the relative abundance of elements in samples to be compared.  
4.4 In the context of a forensic polymer comparison, the evaluation of SEM/EDS results are intended to provide insight into the following forensic tasks:  
4.4.1 Comparison of structure, texture, and elemental data.  
4.4.2 Support for results from other instruments (for example, the presence of calcium, oxygen, and carbon in the EDS spectrum obtained from discrete particles indicates the presence of calcium carbonate as observed in an infrared spectrum). Refer to Guides E2937 and E3085 for further details.  
4.4.3 Significance of results given the presence of certain elements, layer structures, or textures.
SCOPE
1.1 This guide covers recommended techniques and procedures intended for use by forensic laboratory personnel that perform SEM/EDS analyses on polymer samples.  
1.2 This guide describes various techniques and procedures used in the SEM/EDS analysis of polymers that include sample handling and preparation, instrument operating conditions, and spectral data collection, evaluation and interpretation.  
1.3 The theoretical aspects of many of the topics presented can be found in texts such as Scanning Electron Microscopy and X-ray Microanalysis (1).2  
1.4 This guide is intended to be applied within the scope of a broader analytical scheme (for example, Guides E1610, E3260) for the forensic analysis of a polymer sample. An SEM/EDS analysis can provide additional information regarding the potential relationships between the sources of polymeric materials.  
1.5 This guide is intended for use by competent forensic science practitioners with the requisite formal education, discipline-specific training (see Practices E2917, E3233, and E3234), and demonstrated proficiency to perform forensic casework.  
1.6 The values stated in SI units are to be regarded as standard. Other units of measurement are included in this standard where applicable as a result of common usage (for example, keV).  
1.7 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.  
1.8 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.

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  • Guide
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ASTM
ASTM E3296-22(Guide)
Standard Guide for Using Pyrolysis Gas Chromatography and Pyrolysis Gas Chromatography-Mass Spectrometry in Forensic Polymer Examinations

SIGNIFICANCE AND USE
4.1 This guide provides guidance in the selection of appropriate sample preparation methods and instrumental parameters for the analysis, comparison, or identification of various polymeric materials by PGC and PGC/MS.  
4.1.1 PGC/MS can differentiate between classes of fibers (for example, acrylic, polyester, nylon) and within classes of fibers (for example, acrylics) (1-3).5  
4.1.2 Paint binders are differentiated based upon the variety of monomers used in paint formulations which could be difficult to identify by other analytical techniques. In addition, some additives can be detected or identified.  
4.1.3 Differentiation can be achieved by the separation and identification of organic components in the adhesive portion of tapes (4, 5) and in the backings of electrical tapes (6).  
4.1.4 PGC/MS can provide additional discrimination for other types of polymers such as automotive lenses, automotive body fillers, cosmetics, plastics, and rubbers (7-9).  
4.2 Pyrolysis breaks a large molecule into many smaller molecules in a reproducible fashion through the breaking of bonds by means of the application of thermal energy. Analytical pyrolysis is used to provide chemical information on organic-containing solids that cannot be dissolved or otherwise introduced into a chromatographic system. It is also used to analyze and compare solvents bound in a solid material (such as tape adhesives) (10). When analyzed using a separation technique such as gas chromatography, the smaller molecules produced through the action of pyrolysis form a pattern of separated fragments. Mass and structural information indicative of the original molecule are also available when a mass spectral detector is used.  
4.3 Although a destructive method, and therefore often placed at the end of an analytical scheme, the pyrograms produced from different polymer compositions form characteristic patterns that are useful for both identification of polymer type and comparisons between samples (4, 6...
SCOPE
1.1 This guide covers information and recommendations for the selection and application of various PGC and PGC/MS procedures and methods in the forensic examination of polymeric materials (for example, fibers, paint, tape). PGC and PGC/MS methods are used for the identification and comparison of the organic components of these materials. Refer to Practice D3452 for further information on the preparation of the pyrolysis system for polymeric analyses.  
1.2 This guide is to be used in conjunction with a broader analytical scheme such as Guides E1610 or E3260, or the SWGMAT Forensic Fiber Examination Guidelines.  
1.3 This standard is intended for use by competent forensic science practitioners with the requisite formal education, discipline-specific training (see Practices E2917, E3233, E3234), and demonstrated proficiency to perform forensic casework.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 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.

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