ASTM E1588-16a
(Practice)Standard Practice for Gunshot Residue Analysis by Scanning Electron Microscopy/Energy Dispersive X-Ray Spectrometry
Standard Practice 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 (6).
5.2 SEM/EDS analysis of GSR is a non-destructive method that provides (7, 8) 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) (9), neutron activation analysis (NAA) (10), 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 (11). 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 practice covers the analysis of gunshot residue (GSR) by scanning electron microscopy/energy-dispersive X-ray spectrometry (SEM/EDS) using 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. This practice refers to the analysis of electron microscopy stubs and does not address sample collection (1).2
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 instrument.
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 practice offers a set of instructions for performing one or more specific operations. This practice cannot replace knowledge, skill, or ability acquired through appropriate education, training, and experience and should be used in conjunction with sound professional judgment.
1.5 This practice does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user when applying this practice to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: E1588 − 16a
Standard Practice 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 Retrieving Evidence in a Forensic Science Laboratory
1.1 This practice covers the analysis of gunshot residue
3. Terminology
(GSR) by scanning electron microscopy/energy-dispersive
3.1 Definitions of Terms Specific to This Standard:
X-ray spectrometry (SEM/EDS) using manual and automated
3.1.1 major, adj—element whose main peak height is
methods. The analysis may be performed manually, with the
1
greater than ⁄3 of the peak height of the strongest peak in the
operator manipulating the microscope controls and the EDS
spectrum.
system software, or in an automated fashion, where some
Wallace, 1984 (2)
amount of the analysis is controlled by pre-set software
functions. This practice refers to the analysis of electron
3.1.2 minor, adj—element whose main peak height is be-
2
1 1
microscopy stubs and does not address sample collection (1).
tween ⁄10 and ⁄3 of the peak height of the strongest peak in the
spectrum.
1.2 Since software and hardware formats vary among com-
Wallace, 1984 (2)
mercial systems, guidelines will be offered in the most general
terms possible. For proper terminology and operation, consult 3.1.3 trace, adj—element whose main peak height is less
1
the SEM/EDS system manuals for each instrument.
than ⁄10 of the peak height of the strongest peak in the
spectrum.
1.3 The values stated in SI units are to be regarded as
Wallace, 1984 (2)
standard. No other units of measurement are included in this
standard.
4. Summary of Practice
1.4 This practice offers a set of instructions for performing
4.1 From the total population of particles collected, those
one or more specific operations. This practice cannot replace
that are detected by SEM to be within the limits of certain
knowledge, skill, or ability acquired through appropriate
parameters (for example, atomic number, size, or shape) are
education, training, and experience and should be used in
analyzed by EDS (3-5). Typically, particles composed of high
conjunction with sound professional judgment.
mean atomic number elements are detected by their SEM
1.5 This practice does not purport to address all of the
backscattered electron signals and an EDS spectrum is ob-
safety concerns, if any, associated with its use. It is the
tained from each. The EDS spectrum is evaluated for constitu-
responsibility of the user when applying this practice to
ent elements that may identify the particle as being consistent
establish appropriate safety and health practices and deter-
with or characteristic of GSR, or both. See Section 9 for
mine the applicability of regulatory limitations prior to use.
discussion on classification of particles.
2. Referenced Documents
5. Significance and Use
3
2.1 ASTM Standards:
5.1 This document will be of use to forensic laboratory
E1492 Practice for Receiving, Documenting, Storing, and
personnel who are involved in the analysis of GSR samples by
SEM/EDS (6).
1
This practice is under the jurisdiction of ASTM Committee E30 on Forensic
5.2 SEM/EDS analysis of GSR is a non-destructive method
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics.
that provides (7, 8) both morphological information and the
CurrenteditionapprovedMay1,2016.PublishedJuly2016.Originallyapproved
in 1994. Last previous version approved in 2016 as E1588 – 16. DOI: 10.1520/
elemental profiles of individual particles.
E1588-16A.
2
5.3 Particle analysis contrasts with bulk sample methods,
The boldface numbers in parentheses refer to a list of references at the end of
this standard.
such as atomic absorption spectrophotometry (AAS) (9), neu-
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
tron activation analysis (NAA) (10), inductively coupled
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
plasma atomic emission spectrometry (ICP-AES), and induc-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. tively coupled plasma mass spectrometry (ICP-MS), where the
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E1588 − 16a
sampled material is dissolved or extracted prior to the deter- case is a matter for the analyst to decide but should be subject
mination of total e
...
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: E1588 − 16 E1588 − 16a
Standard GuidePractice 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
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 guidepractice 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 March 1, 2016May 1, 2016. Published March 2016July 2016. Originally approved in 1994. Last previous version approved in 20102016 as
ɛ1
E1588 – 10E1588 – 16. . DOI: 10.1520/E1588-16.10.1520/E1588-16A.
3
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.
2
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 − 16a
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 t
...
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