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 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.
