ASTM E1588-10
(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
This document will be of use to forensic laboratory personnel who are involved in the analysis of GSR samples by SEM/EDS (4).
SEM/EDS analysis of GSR is a non-destructive method that provides (5, 6) both morphological information and the elemental profiles of individual particles.
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.
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:E1588–10
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. Scope 3. Significance and Use
1.1 This guide covers the analysis of gunshot residue (GSR) 3.1 This document will be of use to forensic laboratory
by scanning electron microscopy/energy-dispersive X-ray personnel who are involved in the analysis of GSR samples by
spectrometry (SEM/EDS) by manual and automated methods. SEM/EDS (4).
The analysis may be performed manually, with the operator 3.2 SEM/EDS analysis of GSR is a non-destructive method
manipulating the microscope controls and the EDS system that provides (5, 6) both morphological information and the
software, or in an automated fashion, where some amount of elemental profiles of individual particles.
the analysis is controlled by pre-set software functions. 3.3 Particle analysis contrasts with bulk sample methods,
1.2 Since software and hardware formats vary among com- such as atomic absorption spectrophotometry (AAS) (7), neu-
mercial systems, guidelines will be offered in the most general tronactivationanalysis(NAA) (8),inductivelycoupledplasma
terms possible. For proper terminology and operation, consult atomic emission spectrometry (ICP-AES), and inductively
the SEM/EDS system manuals for each system. coupled plasma mass spectrometry (ICP-MS), where the
1.3 The values stated in SI units are to be regarded as sampled material is dissolved or extracted prior to the deter-
standard. No other units of measurement are included in this mination of total element concentrations, thereby sacrificing
standard. morphological information and individual particle identifica-
1.4 This standard does not purport to address all of the tion.
safety concerns, if any, associated with its use. It is the 3.4 X-ray fluorescence spectrometry (XRF) is a technique
responsibility of the user of this standard to establish appro- that has been used to map the placement and distribution of
priate safety and health practices and determine the applica- GSR particles surrounding bullet holes in order to establish
bility of regulatory limitations prior to use. shooting distances (9). Unlike the solution-based bulk methods
of analysis, XRF is non-destructive; however, XRF still does
2. Summary of Practice
not provide morphological information and is incapable of
2.1 From the total population of particles collected, those individual GSR particle identification.
that are detected by SEM to be within the limits of certain
4. Sample Preparation
parameters (for example, atomic number, size, or shape) are
2
analyzed by EDS (1-3). Typically, particles composed of high 4.1 Once the evidence seal is broken, care should be taken
mean atomic number elements are detected by their SEM so that no object touches the surface of the adhesive SEM/EDS
backscattered electron signals and an EDS spectrum is ob- sample collection stub and that the stub is not left uncovered
tained from each. The EDS spectrum is evaluated for constitu- any longer than is reasonable for transfer, mounting, or
ent elements that may identify the particle as being consistent labeling.
with or characteristic of GSR, or both. 4.2 Label the sample collection stub in such a manner that it
is distinguishable from other sample collection stubs without
compromising the sample; for example, label the bottom or
side of the stub.
1
This guide is under the jurisdiction of ASTM Committee E30 on Forensic
4.3 If a non-conductive adhesive was used in the sample
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics.
Current edition approved June 1, 2010. Published June 2010. Originally
collectionstub,thesamplewillneedtobecoatedtoincreaseits
approved in 1994. Last previous version approved in 2008 as E1588 – 08. DOI:
electrical conductivity, unless an environmental SEM or
10.1520/E1588-10.
2 variable-pressure/low-vacuum SEM is used for the analysis.
The boldface numbers in parentheses refer to a list of references at the end of
this standard. Carbon is a common choice of coating material, since it will
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
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E1588–10
not interfere with X-ray lines of interest. For high-vacuum 6.3.4 Automated systems will also include software capable
SEM, coat the sample sufficiently to eliminate charging of the of acqu
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:E1588–08 Designation:E1588–10
Standard Guide for
Gunshot Residue Analysis by Scanning Electron
1
Microscopy/Energy Dispersive X-rayX-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.
1.2Since software and hardware formats vary among commercial systems, guidelines will be offered in the most general terms
possible. The software manual for each system should be consulted for proper terminology and operation.
1.3
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. Summary of Practice
2.1 From the total population of particles collected, those that are determineddetected by SEM to be within the limits of certain
2
parameters (for example, atomic number, size, or shape) characteristic of or consistent with GSR 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 elemental profile spectrum is evaluated for constituent elements that may
identify the particle as being characteristic ofconsistent with or consistent with GSR. characteristic of GSR, or both.
3. Significance and Use
3.1 This document will be of use to forensic laboratory personnel who are involved in the analysis of GSR samples by
SEM/EDS (4).
3.2 SEM/EDS analysis of GSR is a non-destructive method that provides (5, 6) both morphological information and the
elemental profiles of individual particles. This
3.3 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. In addition, X-ray
3.4 X-ray fluorescence spectrometry (XRF) is a bulk analysis technique that has been used for to map the elemental analysis
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.
4. Sample Preparation
4.1 Once the evidence seal is broken, care should be taken so that no object touches the surface of the adhesive SEM/EDS
sample collection stub and that the stub is not left uncovered any longer than is reasonable for transfer, mounting, or labeling.
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.
e1
Current edition approved March 15, 2008. Published April 2008. Originally approved in 1994. Last previous version approved in 2007 as E1588–07 . DOI:
10.1520/E1588-08.
CurrenteditionapprovedJune1,2010.PublishedJune2010.Originallyapprovedin1994.Lastpreviousversionapprovedin2008asE1588 – 08.DOI:10.1520/E1588-10.
2
Krishnan, S. S., “Detection of Gunshot Residue: Present Status,” Forensic Science Handbook, Volume I, Prentice Hall, I
...
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