ASTM E1588-16
(Guide)Standard Guide for Gunshot Residue Analysis by Scanning Electron Microscopy/Energy Dispersive X-Ray Spectrometry
Standard Guide for Gunshot Residue Analysis by Scanning Electron Microscopy/Energy Dispersive X-Ray Spectrometry
SIGNIFICANCE AND USE
5.1 This document will be of use to forensic laboratory personnel who are involved in the analysis of GSR samples by SEM/EDS (4).
5.2 SEM/EDS analysis of GSR is a non-destructive method that provides (5, 6) both morphological information and the elemental profiles of individual particles.
5.3 Particle analysis contrasts with bulk sample methods, such as atomic absorption spectrophotometry (AAS) (7), neutron activation analysis (NAA) (8), inductively coupled plasma atomic emission spectrometry (ICP-AES), and inductively coupled plasma mass spectrometry (ICP-MS), where the sampled material is dissolved or extracted prior to the determination of total element concentrations, thereby sacrificing morphological information and individual particle identification.
5.4 X-ray fluorescence spectrometry (XRF) is a technique that has been used to map the placement and distribution of GSR particles surrounding bullet holes in order to establish shooting distances (9). Unlike the solution-based bulk methods of analysis, XRF is non-destructive; however, XRF still does not provide morphological information and is incapable of individual GSR particle identification.
SCOPE
1.1 This guide covers the analysis of gunshot residue (GSR) by scanning electron microscopy/energy-dispersive X-ray spectrometry (SEM/EDS) by manual and automated methods. The analysis may be performed manually, with the operator manipulating the microscope controls and the EDS system software, or in an automated fashion, where some amount of the analysis is controlled by pre-set software functions.
1.2 Since software and hardware formats vary among commercial systems, guidelines will be offered in the most general terms possible. For proper terminology and operation, consult the SEM/EDS system manuals for each system.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: E1588 − 16
StandardGuide for
Gunshot Residue Analysis by Scanning Electron
1
Microscopy/Energy Dispersive X-Ray Spectrometry
This standard is issued under the fixed designation E1588; 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 3.1.2 minor, adj—element whose main peak height is be-
1 1
tween ⁄10 and ⁄3 of the peak height of the strongest peak in the
1.1 This guide covers the analysis of gunshot residue (GSR)
spectrum. Wallace 1984 (15)
by scanning electron microscopy/energy-dispersive X-ray
3.1.3 trace, adj—element whose main peak height is less
spectrometry (SEM/EDS) by manual and automated methods.
1
than ⁄10 of the peak height of the strongest peak in the
The analysis may be performed manually, with the operator
spectrum. Wallace 1984 (15)
manipulating the microscope controls and the EDS system
software, or in an automated fashion, where some amount of
4. Summary of Practice
the analysis is controlled by pre-set software functions.
4.1 From the total population of particles collected, those
1.2 Since software and hardware formats vary among com-
that are detected by SEM to be within the limits of certain
mercial systems, guidelines will be offered in the most general
parameters (for example, atomic number, size, or shape) are
terms possible. For proper terminology and operation, consult
analyzed by EDS (1-3). Typically, particles composed of high
the SEM/EDS system manuals for each system.
mean atomic number elements are detected by their SEM
1.3 The values stated in SI units are to be regarded as
backscattered electron signals and an EDS spectrum is ob-
standard. No other units of measurement are included in this
tained from each. The EDS spectrum is evaluated for constitu-
standard.
ent elements that may identify the particle as being consistent
1.4 This standard does not purport to address all of the
with or characteristic of GSR, or both.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Significance and Use
priate safety and health practices and determine the applica-
5.1 This document will be of use to forensic laboratory
bility of regulatory limitations prior to use.
personnel who are involved in the analysis of GSR samples by
SEM/EDS (4).
2. Referenced Documents
2
5.2 SEM/EDS analysis of GSR is a non-destructive method
2.1 ASTM Standards:
that provides (5, 6) both morphological information and the
E1492 Practice for Receiving, Documenting, Storing, and
elemental profiles of individual particles.
Retrieving Evidence in a Forensic Science Laboratory
5.3 Particle analysis contrasts with bulk sample methods,
3. Terminology
such as atomic absorption spectrophotometry (AAS) (7), neu-
3.1 Definitions of Terms Specific to This Standard:
tronactivationanalysis(NAA) (8),inductivelycoupledplasma
3.1.1 major, adj—element whose main peak height is atomic emission spectrometry (ICP-AES), and inductively
1
greater than ⁄3 of the peak height of the strongest peak in the
coupled plasma mass spectrometry (ICP-MS), where the
3
spectrum. Wallace 1984 (15) sampled material is dissolved or extracted prior to the deter-
mination of total element concentrations, thereby sacrificing
morphological information and individual particle identifica-
1
This guide is under the jurisdiction of ASTM Committee E30 on Forensic
tion.
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics.
Current edition approved March 1, 2016. Published March 2016. Originally
5.4 X-ray fluorescence spectrometry (XRF) is a technique
ɛ1
approved in 1994. Last previous version approved in 2010 as E1588 – 10 . DOI:
that has been used to map the placement and distribution of
10.1520/E1588-16.
2
GSR particles surrounding bullet holes in order to establish
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
shooting distances (9). Unlike the solution-based bulk methods
Standards volume information, refer to the standard’s Document Summary page on
of analysis, XRF is non-destructive; however, XRF still does
the ASTM website.
3
not provide morphological information and is incapable of
The boldface numbers in parentheses refer to a list of references at the end of
this standard. individual GSR particle identification.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E1588 − 16
6. Sample Preparation the manufactu
...
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.
´1
Designation: E1588 − 10 E1588 − 16
Standard Guide for
Gunshot Residue Analysis by Scanning Electron
1
Microscopy/Energy Dispersive X-Ray Spectrometry
This standard is issued under the fixed designation E1588; 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
ε NOTE—Sections 7.1.5.2 and 7.2.1.2 were editorially corrected in July 2010.
1. Scope
1.1 This guide covers the analysis of gunshot residue (GSR) by scanning electron microscopy/energy-dispersive X-ray
spectrometry (SEM/EDS) by manual and automated methods. The analysis may be performed manually, with the operator
manipulating the microscope controls and the EDS system software, or in an automated fashion, where some amount of the
analysis is controlled by pre-set software functions.
1.2 Since software and hardware formats vary among commercial systems, guidelines will be offered in the most general terms
possible. For proper terminology and operation, consult the SEM/EDS system manuals for each system.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
E1492 Practice for Receiving, Documenting, Storing, and Retrieving Evidence in a Forensic Science Laboratory
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
1
3.1.1 major, adj—element whose main peak height is greater than ⁄3 of the peak height of the strongest peak in the spectrum.
3
Wallace 1984 (15)
1 1
3.1.2 minor, adj—element whose main peak height is between ⁄10 and ⁄3 of the peak height of the strongest peak in the
spectrum. Wallace 1984 (15)
1
3.1.3 trace, adj—element whose main peak height is less than ⁄10 of the peak height of the strongest peak in the spectrum.
Wallace 1984 (15)
4. Summary of Practice
4.1 From the total population of particles collected, those that are detected by SEM to be within the limits of certain parameters
(for example, atomic number, size, or shape) are analyzed by EDS (1-3). Typically, particles composed of high mean atomic
number elements are detected by their SEM backscattered electron signals and an EDS spectrum is obtained from each. The EDS
spectrum is evaluated for constituent elements that may identify the particle as being consistent with or characteristic of GSR, or
both.
5. Significance and Use
5.1 This document will be of use to forensic laboratory personnel who are involved in the analysis of GSR samples by
SEM/EDS (4).
1
This guide 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 June 1, 2010March 1, 2016. Published June 2010March 20116. Originally approved in 1994. Last previous version approved in 20082010 as
ɛ1
E1588 – 08.E1588 – 10 . DOI: 10.1520/E1588-10E01.10.1520/E1588-16.
2
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.
3
The boldface numbers in parentheses refer to a list of references at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E1588 − 16
5.2 SEM/EDS analysis of GSR is a non-destructive method that provides (5, 6) both morphological information and the
elemental profiles of individual particles.
5.3 Particle analysis contrasts with bulk sample methods, such as atomic absorption spectrophotometry (AAS) (7), neutron
activation analysis (NAA) (8), inductively coupled plasma atomic emission spectrometry (ICP-AES), and inductively coupled
plasma mass spectrometry (ICP-MS), where the sampled material is dissolved or extracted prior to the determination of total
element concentrations, thereby sacrificing morphological information and individual particle identification.
5.4 X-ray fluore
...
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