Combining grazing incidence X-rays and micro-diffraction for qualitative phase identification in forensic powdered micro-samples

Autor: I. Queralt, J. Gárate-Lagos, P. Sáez-Martínez, F. Torres-Roquer, U. Salazar-Kuri, S. Camargo
Přispěvatelé: Ministerio de Ciencia e Innovación (España)
Jazyk: angličtina
Rok vydání: 2021
Předmět:
Zdroj: Digital.CSIC. Repositorio Institucional del CSIC
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Popis: Capillary diffraction or microdiffraction are standard techniques for characterizing small samples when only a few milligrams are available. On the other hand, we have typical grazing incidence diffraction or different variations of grazing incidence (GI) diffraction used, such as in-plane grazing incidence (IP-GI) or GI using a micro focusing source, to study thin films. However, when few powder micrograms are available, the characterization task is complicated. In the present work, few micrograms of typical forensic samples are analyzed using standard Bragg-Brentano, X-ray powder diffraction geometry, and grazing incidence X-ray micro-diffraction (GIµXRD). Samples include soils, cosmetic eyeshadows, two different pyrotechnic materials, and a highly explosive mixture contained at primer cup of ammunition. The analysis was carried out from 1 to 5 degrees of the incident parallel beam with a shaking sample. Depending on the fixed incident angle, different small regions of the diffraction patterns showed an improvement in the intensity of the peaks with respect to the conventional Bragg-Brentano configuration. However, 3–5 degrees of the fixed incident beam showed the best results. This new data acquisition technique, based on the combination of two known diffraction methods, could be a powerful tool for studying samples outside of forensic sciences such as nanomaterials, medicine, or any other field where the sample quantity is extremely small, also, without the need to transport evidence and travel to external facilities with higher analytical performance such as synchrotron radiation installations or other large experimental facilities.
The authors are grateful for the constructive criticism of two anonymous reviewers who contributed to the improvement of the quality of the work carried out. Authors acknowledge to the International Atomic Energy Agency (IAEA) for the financial support of this work, project CHI-0017. We also acknowledge the financial support of the CONACyT project A1-S-10011. IDAEA-CSIC is a Centre of Excellence Severo Ochoa (Spanish Ministry of Science and Innovation, Project CEX2018-000794-S).
Databáze: OpenAIRE