ASTM E3294-22
(Guide)Standard Guide for Forensic Analysis of Geological Materials by Powder X-Ray Diffraction
Standard Guide for Forensic Analysis of Geological Materials by Powder X-Ray Diffraction
SIGNIFICANCE AND USE
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).
5.2.1 Non-destructive XRD analysis can be performed in situ on geological material adhering to a substrate (see 8.12.3).
5.2.2 The most common forensic applications of XRD to geological materials are (A) identification or confirmation of a selected phase or fraction of a sample (see 8.12), (B) identification of minerals in the clay-sized fractions of soils (see 8.8), and (C) identification of the phases of the hydrated cement component of concrete or mortar.
5.3 This guide is intended to be used with other methods of analysis (for example, polarized light microscopy, scanning electron microscopy, palynology) within a more comprehensive analytical scheme for the forensic analysis or comparison of geological materials.
5.3.1 Comprehensive criteria for forensic comparisons of geological material integrating multiple analytical methods and provenance estimations (see 11.4) are not included and are beyond the scope of this guide.
SCOPE
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.
1.2 This guide makes recommendations for the preparation of geological materials for powder XRD analysis with adaptations for samples of limited quantity, instrumental configuration to generate high-quality XRD data, identification of crystalline materials by comparison to published diffraction data, and forensic comparison of XRD patterns from two or more samples of geological materials to support criminal investigations.
1.3 Units—The values stated in SI units are to be regarded as standard. Other units are avoided, in general, but there is a long-standing tradition of expressing X-ray wavelengths and lattice spacing in units of Ångströms (Å). One Ångström = 10–10 meter (m) = 0.1 nanometer (nm).
1.4 This standard is intended for use by competent forensic science practitioners with the requisite formal education, discipline-specific training (see Practice E2917), and demonstrated proficiency to perform forensic casework.
1.5 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.
1.6 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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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: E3294 − 22 An American National Standard
Standard Guide for
Forensic Analysis of Geological Materials by Powder X-Ray
1
Diffraction
This standard is issued under the fixed designation E3294; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 Thisguidecoverstechniquesandproceduresfortheuse
C1365Test Method for Determination of the Proportion of
of powder X-ray diffraction (XRD) in the forensic analysis of
Phases in Portland Cement and Portland-Cement Clinker
geological materials (to include soils, rocks, sediments, and
Using X-Ray Powder Diffraction Analysis
materials derived from them such as concrete), to enable
D934Practices for Identification of Crystalline Compounds
non-consumptive identification of solid crystalline materials
in Water-Formed Deposits By X-Ray Diffraction (With-
present as single components or multi-component mixtures.
3
drawn 2022)
1.2 This guide makes recommendations for the preparation
E620Practice for Reporting Opinions of Scientific or Tech-
of geological materials for powder XRD analysis with adapta-
nical Experts
tions for samples of limited quantity, instrumental configura-
E1492Practice for Receiving, Documenting, Storing, and
tion to generate high-quality XRD data, identification of
Retrieving Evidence in a Forensic Science Laboratory
crystalline materials by comparison to published diffraction
E2917Practice for Forensic Science Practitioner Training,
data, and forensic comparison of XRD patterns from two or
Continuing Education, and Professional Development
more samples of geological materials to support criminal
Programs
investigations.
E3272Guide for Collection of Soils and Other Geological
1.3 Units—The values stated in SI units are to be regarded Evidence for Criminal Forensic Applications
as standard. Other units are avoided, in general, but there is a 4
2.2 ISO Standard:
long-standing tradition of expressing X-ray wavelengths and
ISO/IEC 17025:2017General Requirements for the Compe-
lattice spacing in units of Ångströms (Å). One Ångström =
tence of Testing and Calibration Laboratories
–10
10 meter (m) = 0.1 nanometer (nm).
1.4 This standard is intended for use by competent forensic 3. Terminology
science practitioners with the requisite formal education,
3.1 Definitions of Terms Specific to This Standard:
discipline-specific training (see Practice E2917), and demon-
3.1.1 Bragg equation or Bragg’s law, n—describes the
strated proficiency to perform forensic casework.
physical phenomenon of X-ray scattering from a crystallo-
1.5 This standard does not purport to address all of the graphic three-dimensional lattice plane as nλ=2dsinθ, in which
n is any integer, λ is the wavelength of the X-ray, d is the
safety concerns, if any, associated with its use. It is the
crystal plane separation, also known as d-spacing, and θ is the
responsibility of the user of this standard to establish appro-
angle between the crystal plane and the diffracted beam, also
priate safety, health, and environmental practices and deter-
known as the Bragg Angle.
mine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accor-
3.1.2 crystal, n—a homogeneous, solid body of a chemical
dance with internationally recognized principles on standard-
element or compound, having a regularly repeating atomic
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Barriers to Trade (TBT) Committee.
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 last approved version of this historical standard is referenced on
1
This guide is under the jurisdiction of ASTM Committee E30 on Forensic www.astm.org.
4
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics. Available from International Organization for Standardization (ISO), ISO
Current edition approved March 15, 2022. Published June 2022. DOI: 10.1520/ Central Secretariat, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva,
E3294-22. Switzerland, https://www.iso.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Consh
...
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: E3294 − 22 An American National Standard
Standard Guide for
Forensic Analysis of Geological Materials by Powder X-Ray
1
Diffraction
This standard is issued under the fixed designation E3294; 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 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This guide covers techniques and procedures for the use
C1365 Test Method for Determination of the Proportion of
of powder X-ray diffraction (XRD) in the forensic analysis of
Phases in Portland Cement and Portland-Cement Clinker
geological materials (to include soils, rocks, sediments, and
Using X-Ray Powder Diffraction Analysis
materials derived from them such as concrete), to enable
D934 Practices for Identification of Crystalline Compounds
non-consumptive identification of solid crystalline materials
in Water-Formed Deposits By X-Ray Diffraction (With-
present as single components or multi-component mixtures.
3
drawn 2022)
1.2 This guide makes recommendations for the preparation
E620 Practice for Reporting Opinions of Scientific or Tech-
of geological materials for powder XRD analysis with adapta-
nical Experts
tions for samples of limited quantity, instrumental configura-
E1492 Practice for Receiving, Documenting, Storing, and
tion to generate high-quality XRD data, identification of
Retrieving Evidence in a Forensic Science Laboratory
crystalline materials by comparison to published diffraction
E2917 Practice for Forensic Science Practitioner Training,
data, and forensic comparison of XRD patterns from two or
Continuing Education, and Professional Development
more samples of geological materials to support criminal
Programs
investigations.
E3272 Guide for Collection of Soils and Other Geological
1.3 Units—The values stated in SI units are to be regarded Evidence for Criminal Forensic Applications
4
as standard. Other units are avoided, in general, but there is a
2.2 ISO Standard:
long-standing tradition of expressing X-ray wavelengths and
ISO/IEC 17025:2017 General Requirements for the Compe-
lattice spacing in units of Ångströms (Å). One Ångström =
tence of Testing and Calibration Laboratories
–10
10 meter (m) = 0.1 nanometer (nm).
3. Terminology
1.4 This standard is intended for use by competent forensic
science practitioners with the requisite formal education,
3.1 Definitions of Terms Specific to This Standard:
discipline-specific training (see Practice E2917), and demon-
3.1.1 Bragg equation or Bragg’s law, n—describes the
strated proficiency to perform forensic casework.
physical phenomenon of X-ray scattering from a crystallo-
graphic three-dimensional lattice plane as nλ=2dsinθ, in which
1.5 This standard does not purport to address all of the
n is any integer, λ is the wavelength of the X-ray, d is the
safety concerns, if any, associated with its use. It is the
crystal plane separation, also known as d-spacing, and θ is the
responsibility of the user of this standard to establish appro-
angle between the crystal plane and the diffracted beam, also
priate safety, health, and environmental practices and deter-
known as the Bragg Angle.
mine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accor-
3.1.2 crystal, n—a homogeneous, solid body of a chemical
dance with internationally recognized principles on standard-
element or compound, having a regularly repeating atomic
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Barriers to Trade (TBT) Committee.
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 last approved version of this historical standard is referenced on
1
This guide is under the jurisdiction of ASTM Committee E30 on Forensic www.astm.org.
4
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics. Available from International Organization for Standardization (ISO), ISO
Current edition approved March 15, 2022. Published June 2022. DOI: 10.1520/ Central Secretariat, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva,
E3294-22. Switzerland, https://www.iso.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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E3294 − 22
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