ASTM E3294-23

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. Guidance for the analysis of forensic geological materials can be found in Refs (2-4).  
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 ...
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.

General Information

• Status: Published
• Publication Date: 31-Oct-2023
• ICS: 07.140 - Forensic science
• ICS: 71.040.50 - Physicochemical methods of analysis
• ICS: 91.100.15 - Mineral materials and products
• Technical Committee: E30 - Forensic Sciences
• Drafting Committee: E30.01 - Criminalistics

Relations

• Replaces: ASTM E3294-22 - Standard Guide for Forensic Analysis of Geological Materials by Powder X-Ray Diffraction
• Effective Date: 01-Nov-2023

Standards Content (Sample)

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 − 23 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
1.1 This guide covers techniques and procedures for the use 2.1 ASTM Standards:
of powder X-ray diffraction (XRD) in the forensic analysis of C1365 Test Method for Determination of the Proportion of
geological materials (to include soils, rocks, sediments, and Phases in Portland Cement and Portland-Cement Clinker
materials derived from them such as concrete), to enable Using X-Ray Powder Diffraction Analysis
non-consumptive identification of solid crystalline materials D934 Practices for Identification of Crystalline Compounds
present as single components or multi-component mixtures. in Water-Formed Deposits By X-Ray Diffraction
E620 Practice for Reporting Opinions of Scientific or Tech-
1.2 This guide makes recommendations for the preparation
nical Experts
of geological materials for powder XRD analysis with adapta-
E1492 Practice for Receiving, Documenting, Storing, and
tions for samples of limited quantity, instrumental configura-
Retrieving Evidence in a Forensic Science Laboratory
tion to generate high-quality XRD data, identification of
E2917 Practice for Forensic Science Practitioner Training,
crystalline materials by comparison to published diffraction
Continuing Education, and Professional Development
data, and forensic comparison of XRD patterns from two or
Programs
more samples of geological materials to support criminal
E3272 Guide for Collection of Soils and Other Geological
investigations.
Evidence for Criminal Forensic Applications
1.3 Units—The values stated in SI units are to be regarded
3
2.2 ISO Standard:
as standard. Other units are avoided, in general, but there is a
ISO/IEC 17025:2017 General Requirements for the Compe-
long-standing tradition of expressing X-ray wavelengths and
tence of Testing and Calibration Laboratories
lattice spacing in units of Ångströms (Å). One Ångström =
–10
10 meter (m) = 0.1 nanometer (nm).
3. Terminology
1.4 This standard is intended for use by competent forensic
3.1 Definitions of Terms Specific to This Standard:
science practitioners with the requisite formal education,
3.1.1 Bragg equation or Bragg’s law, n—describes the
discipline-specific training (see Practice E2917), and demon-
physical phenomenon of X-ray scattering from a crystallo-
strated proficiency to perform forensic casework.
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.
3.1.2 crystal, n—a homogeneous, solid body of a chemical
1.6 This international standard was developed in accor-
element or compound, having a regularly repeating atomic
dance with internationally recognized principles on standard-
arrangement that can be outwardly expressed by plane faces
4
ization established in the Decision on Principles for the
(adapted from Ref (1)).
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
2
Barriers to Trade (TBT) Committee.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
1 3
This guide is under the jurisdiction of ASTM Committee E30 on Forensic Available from International Organization for Standardization (ISO), ISO
Sciences and is the direct responsibility of Subcommittee E30.01 on Criminalistics. Central Secretariat, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva,
Current edition approved Nov. 1, 2023. Published November 2023. Originally Switzerland, https://www.iso.org.
4
approved in 2022. Last previous edition approved in 2022 as E3294 – 22. DOI: The boldface nu
...

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: E3294 − 22 E3294 − 23 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
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
–10
long-standing tradition of expressing X-ray wavelengths and lattice spacing in units of Ångströms (Å). One Ångström = 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.
2. Referenced Documents
2
2.1 ASTM Standards:
C1365 Test Method for Determination of the Proportion of Phases in Portland Cement and Portland-Cement Clinker Using
X-Ray Powder Diffraction Analysis
D934 Practices for Identification of Crystalline Compounds in Water-Formed Deposits By X-Ray Diffraction
E620 Practice for Reporting Opinions of Scientific or Technical Experts
E1492 Practice for Receiving, Documenting, Storing, and Retrieving Evidence in a Forensic Science Laboratory
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, 2022Nov. 1, 2023. Published June 2022November 2023. Originally approved in 2022. Last previous edition approved in 2022 as
E3294DOI: 10.1520/E3294-22. – 22. DOI: 10.1520/E3294-23.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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E3294 − 23
E2917 Practice for Forensic Science Practitioner Training, Continuing Education, and Professional Development Programs
E3272 Guide for Collection of Soils and Other Geological Evidence for Criminal Forensic Applications
3
2.2 ISO Standard:
ISO/IEC 17025:2017 General Requirements for the Competence of Testing and Calibration Laboratories
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 Bragg equation or Bragg’s law, n—describes the physical phenomenon of X-ray scattering from a crystallographic
three-dimensional lattice plane as nλ=2dsinθ, in which n is any integer, λ is the wavelength of the X-ray, d is the crystal plane
separation, also known as d-spacing, and θ is the angle between the crystal plane and the diffracted beam, also known as the Bragg
Angle.
3.1.2 crystal, n—a homogeneous, solid b
...