ASTM E1588-08

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.
SEM/EDS analysis of GSR is a non-destructive method that provides2 ,3 both morphological information and the elemental profiles of individual particles. This contrasts with bulk sample methods, such as atomic absorption spectrophotometry, neutron activation analysis, inductively coupled plasma atomic emission spectrometry, and inductively coupled plasma mass spectrometry, 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 fluorescence spectrometry (XRF) is a bulk analysis technique that has been used for the elemental analysis of GSR. Unlike the solution-based bulk methods of analysis, XRF is nondestructive; 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. The software manual for each system should be consulted for proper terminology and operation.  
1.3 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.

General Information

• Status: Historical
• Publication Date: 14-Mar-2008
• ICS: 11.020 - Medical sciences and health care facilities in general
• Technical Committee: E30 - Forensic Sciences
• Drafting Committee: E30.01 - Criminalistics

Relations

• Replaces: ASTM E1588-07e1 - Standard Guide for Gunshot Residue Analysis by Scanning Electron Microscopy/Energy Dispersive X-ray Spectrometry
• Effective Date: 15-Mar-2008
• Replaced By: ASTM E1588-10 - Standard Guide for Gunshot Residue Analysis by Scanning Electron Microscopy/ Energy Dispersive X-ray Spectrometry
• Effective Date: 01-Jun-2010
• Referred By: ASTM E1732-22 - Standard Terminology Relating to Forensic Science
• Effective Date: 15-Mar-2008
• Referred By: ASTM E3309-21 - Standard Guide for Reporting of Forensic Primer Gunshot Residue (pGSR) Analysis by Scanning Electron Microscopy/Energy Dispersive X-Ray Spectrometry (SEM/EDS)
• Effective Date: 15-Mar-2008

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information.
Designation:E1588–08
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 emental profiles of individual particles. This contrasts with
bulk sample methods, such as atomic absorption spectropho-
1.1 This guide covers the analysis of gunshot residue (GSR)
tometry, neutron activation analysis, inductively coupled
by scanning electron microscopy/energy-dispersive X-ray
plasma atomic emission spectrometry, and inductively coupled
spectrometry (SEM/EDS) by manual and automated methods.
plasma mass spectrometry, where the sampled material is
The analysis may be performed manually, with the operator
dissolved or extracted prior to the determination of total
manipulating the microscope controls and the EDS system
element concentrations, thereby sacrificing morphological in-
software, or in an automated fashion, where some amount of
formation and individual particle identification. In addition,
the analysis is controlled by pre-set software functions.
X-ray fluorescence spectrometry (XRF) is a bulk analysis
1.2 Since software and hardware formats vary among com-
techniquethathasbeenusedfortheelementalanalysisofGSR.
mercial systems, guidelines will be offered in the most general
Unlike the solution-based bulk methods of analysis, XRF is
termspossible.Thesoftwaremanualforeachsystemshouldbe
nondestructive; however, XRF still does not provide morpho-
consulted for proper terminology and operation.
logical information and is incapable of individual GSR particle
1.3 This standard does not purport to address all of the
identification.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Sample Preparation
priate safety and health practices and determine the applica-
4.1 Once the evidence seal is broken, care should be taken
bility of regulatory limitations prior to use.
so that no object touches the surface of the adhesive SEM/EDS
2. Summary of Practice sample collection stub and that the stub is not left uncovered
any longer than is reasonable for transfer, mounting, or
2.1 From the total population of particles collected, those
labeling.
that are determined by SEM to be within the limits of certain
4.2 Label the sample collection stub in such a manner that it
parameters (for example, atomic number, size, or shape)
is distinguishable from other sample collection stubs without
characteristic of or consistent with GSR are analyzed by EDS.
compromising the sample; that is, label the bottom or side of
Typically, particles composed of high mean atomic number
the stub.
elements are detected by their SEM backscattered electron
4.3 If a non-conductive adhesive was used in the sample
signals and an EDS spectrum is obtained from each. The EDS
collectionstub,thesamplewillneedtobecoatedtoincreaseits
elementalprofileisevaluatedforconstituentelementsthatmay
electrical conductivity, unless an environmental SEM or low
identifytheparticleasbeingcharacteristicoforconsistentwith
pressure/low vacuum - SEM is used for the analysis. Carbon is
GSR.
a common choice of coating material, since it will not be
3. Significance and Use detected with a beryllium window EDS detector and, thus, will
not interfere with X-ray lines of interest. Furthermore, with
3.1 This document will be of use to forensic laboratory
EDSsystemscapableofdetectingcarbon,itisstillignoreddue
personnel who are involved in the analysis of GSR samples by
tothehighsignalintensityfromthecarbonintheadhesive.For
SEM/EDS.
high vacuum SEM, a carbon film thickness of between 5 and
3.2 SEM/EDS analysis of GSR is a non-destructive method
,
2 3
50 nm is typical, with less conductive samples requiring a
that provides both morphological information and the el-
thicker coat. If the carbon coating thickness is not measured,
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 March 15, 2008. Published April 2008. Originally
e1
approved in 1994. Last previous version approved in 2007 as E1588 – 07 . DOI:
3
10.1520/E1588-08. Wolten, G. M., Nesbitt, R. S., Calloway, A. R., Loper, G. L., and Jones, P. F.,
2
Krishnan, S. S., “Detection of Gunshot Residue: Present Status,” Forensic “Final Report on ParticleAnalysis for Gunshot Residue Detection,” Report ATR-77
Science Handbook, Volume I, Prentice Hall, Inc., Englewood Clif
...

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.
e1
Designation:E1588–07 Designation:E1588–08
Standard Guide for
Gunshot Residue Analysis by Scanning Electron
1
Microscopy/ Energy Dispersive X-ray Spectrometry
This standard is issued under the fixed designation E 1588; 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 (e) indicates an editorial change since the last revision or reapproval.
1
e NOTE—Editorial corrections were made in August 2007.
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. The software manual for each system should be consulted for proper terminology and operation.
1.3 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
2.1 ASTM Standard:
E876Practice for Use of Statistics in the Evaluation of Spectrometric Data
3.Summary of Practice
3.1From2.1 From the total population of particles collected, those that are determined by SEM to be within the limits of certain
parameters (e.g., atomic number, size, or shape) characteristic of or consistent with GSR are analyzed by EDS.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 is evaluated for constituent elements that may identify the particle as being
characteristic of or consistent with GSR.
4.3. Significance and Use
4.1This3.1 This document will be of use to forensic laboratory personnel who are involved in the analysis of GSR samples by
SEM/EDS.
,
2 3
43.2 SEM/EDS analysis of GSR is a non-destructive method that provides both morphological information and the elemental
profiles of individual particles. This contrasts with bulk sample methods, such as atomic absorption spectrophotometry, neutron
activation analysis, inductively coupled plasma atomic emission spectrometry, and inductively coupled plasma mass spectrometry,
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 fluorescence spectrometry (XRF) is a bulk
analysis technique that has been used for the elemental analysis of GSR. Unlike the solution-based bulk methods of analysis, XRF
is nondestructive; however, XRF still does not provide morphological information and is incapable of individual GSR particle
identification.
5.4. Sample Preparation
5.14.1 Once the evidence seal is broken, care should be taken so that no object touches the surface of the adhesive SEM/EDS
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 Feb.March 15, 2007.2008. Published April 2007.2008. Originally approved in 1994. Last previous version approved in 20012007 as
e1
E1588–95(2001). E 1588 – 07 .
2
Krishnan, S. S., “Detection of Gunshot Residue: Present Status,” Forensic Science Handbook, Volume I, Prentice Hall, Inc., Englewood Cliffs, NJ, 1982.
3
Krishnan, S. S., “Detection of Gunshot Residue: Present Status,” Forensic Science Handbook, Volume I, Prentice Hall, Inc., Englewood Cliffs, NJ, 1982.
3
Wolten,G.M.,Nesbitt,R.S.,Calloway,A.R.,Loper,G.L.,andJones,P.F.,“FinalReportonParticleAnalysisforGunshotResidueDetection,” ReportATR-77 (7915)-3,
Aerospace Corporation, Segundo, CA, 1977.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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E1588–08
sample collection stub and that the stub is not left uncovered any longer than is reasonable for transfer, mounting, or labeli
...